CN110129598B - Preparation method of quasicrystal reinforced aluminum matrix composite - Google Patents

Preparation method of quasicrystal reinforced aluminum matrix composite Download PDF

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CN110129598B
CN110129598B CN201910480764.8A CN201910480764A CN110129598B CN 110129598 B CN110129598 B CN 110129598B CN 201910480764 A CN201910480764 A CN 201910480764A CN 110129598 B CN110129598 B CN 110129598B
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quasicrystal
smelting
furnace
argon
vacuum
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CN110129598A (en
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赵宇宏
田晋忠
袁野
陈利文
田晓林
侯华
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Binzhou Beihai Rieger New Metal Materials Co.,Ltd.
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North University of China
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

The invention relates to a preparation method of a quasicrystal reinforced aluminum matrix composite, aiming at the conditions of low mechanical property strength and poor toughness of the aluminum matrix composite, quasicrystal particles are added into the aluminum matrix composite, and the quasicrystal reinforced aluminum matrix composite is prepared by smelting and casting, so that the strength and the hardness of the composite are improved.

Description

Preparation method of quasicrystal reinforced aluminum matrix composite
Technical Field
The invention relates to a preparation method of a quasicrystal reinforced aluminum matrix composite, and belongs to the field of composite preparation.
Background
The quasi-crystalline diffraction pattern has quintic, octal, eleven and twelve rotational symmetries, amorphous rotational symmetry and long periodic translation sequence; the quasicrystal has low electrical conductivity and thermal conductivity, special optical property, low surface energy and friction coefficient, oxidation resistance, biocompatibility and high hardness, but the low-temperature brittleness of the quasicrystal determines that the quasicrystal is difficult to be used as a structural part; in order to take advantage of its excellent properties, quasicrystals may be used as reinforcement, i.e., a second phase reinforcement mechanism is employed; on one hand, the quasicrystal can fully play the excellent performance of the quasicrystal as a reinforcement, and the mechanical performance of the composite material is improved; on the other hand, the aluminum-based quasicrystal and the aluminum alloy contain a large amount of aluminum, so that the problem of interface wettability between the reinforcing body particles and the matrix can be solved; AlNiCo is a ten-times single-phase porous structure, and Mn atoms have high hardness and wear resistance, so that a part of Co atoms are replaced by Mn atoms on the basis of AlNiCo quasicrystal, and AlNiCoMn quasicrystal can be designed.
The distribution and content of the quasicrystal in the matrix determine the overall performance of the composite material, at present, the research of the quasicrystal reinforced aluminum matrix composite material mainly adopts a powder metallurgy method, the preparation method has higher cost, is not suitable for mass production, and has poorer strength and toughness of the material; in order to enable the quasicrystal particles to be better compounded with the matrix material, an electromagnetic stirring mode is adopted; on one hand, all reactants can be fully mixed by electromagnetic stirring, the mixing is more uniform, and the temperature of the mixed materials is more uniform; on the other hand, the electromagnetic stirring can prevent the growth of dendrites, thereby obtaining a better as-cast microstructure; because the concentration of elements contained in the quasi-crystal particles and the matrix is different, the quasi-crystal phase structure is unstable due to component change caused by atomic diffusion; in order to better utilize the excellent performance of the quasicrystal, the technology of oxidizing the quasicrystal particles at high temperature to generate a thin oxide film on the quasicrystal surface so as to reduce the diffusion between the reinforcement and the matrix is also in scientific research.
Disclosure of Invention
Object of the Invention
Aiming at the defects of the background technology, the invention fully utilizes the excellent performance of quaternary system quasicrystal, takes cast aluminum alloy as a substrate and AlNiCoMn quasicrystal as reinforcement particles, forms an oxide film on the surface of the quasicrystal by oxidizing the quasicrystal at high temperature, and reduces the mutual diffusion between the quasicrystal and the substrate in the process of preparing the composite material; the quasicrystal reinforced aluminum matrix composite material with excellent performance is prepared by a method combining casting and electromagnetic smelting.
Technical scheme
The chemical substance materials used by the invention are aluminum, nickel, cobalt, manganese, aluminum alloy, absolute ethyl alcohol and argon, and the combined preparation dosage is as follows: g, ml, cm3As a unit of measure
Figure BDA0002083559060000021
The preparation method comprises the following steps:
(1) pretreatment of quasicrystalline materials
Firstly, 200g plus or minus 0.01g of aluminum block, 80g plus or minus 0.01g of nickel block, 60g plus or minus 0.01g of cobalt particles and 28g plus or minus 0.01g of manganese sheets are crushed into mixed particles;
secondly, ball milling, namely placing the granular quasicrystal component into a ball mill for ball milling for 30min to form quasicrystal mixed granules;
thirdly, cleaning, namely putting the quasicrystal mixed particles into an ultrasonic cleaning instrument, adding 1000mL of absolute ethyl alcohol, cleaning, and drying in the air;
drying, namely putting the dried quasicrystal mixed particles into a vacuum drying oven, wherein the drying temperature is 180 ℃, the vacuum degree is 2Pa, and the drying time is 60 min;
fifthly, high-temperature oxidation, namely placing the dried quasicrystal particles in a heat treatment furnace for high-temperature oxidation at 800 ℃ for 12 hours;
(2) aluminum alloy cutting block
Placing 3000g +/-0.01 g of aluminum alloy on a steel flat plate, and mechanically cutting into blocks with the block size of less than or equal to 80mm multiplied by 80 mm;
(3) smelting preparation of quasi-crystal reinforced aluminum-based composite material
Smelting of the quasicrystal reinforced aluminum matrix composite is carried out in a vacuum smelting furnace, and is completed under the protection of argon in the processes of heating, stirring and adding quasicrystal particles;
cleaning a smelting crucible, cleaning the smelting crucible by using a metal shovel and a metal brush, and cleaning the smelting crucible by using absolute ethyl alcohol to ensure that the smelting crucible is clean;
placing the raw materials, and placing the cut aluminum alloy at the bottom of a smelting crucible;
placing the quasicrystal particles, and uniformly placing the dried quasicrystal particles on the upper part of the aluminum alloy block in the crucible;
closing the vacuum smelting furnace, starting a vacuum pump, and extracting air in the furnace to enable the pressure in the furnace to reach 2 Pa;
introducing argon, opening a gas pressing valve and a bottom blowing motor, and introducing argon into the vacuum smelting furnace at an argon input speed of 200cm3Min, keeping the atmospheric pressure in the furnace at 1 atmosphere;
heating, starting a heater of an electromagnetic induction smelting furnace, heating at the temperature of 750 +/-2 ℃, heating for 120min, and fully melting the raw materials; when the raw materials are completely melted, reducing the heating temperature to 650 +/-2 ℃, and preserving the heat for 10 min;
electromagnetic stirring, starting a control switch of an electromagnetic stirring device, setting electromagnetic stirring parameters, wherein the stirring frequency is 35Hz, and stirring for 10min at constant temperature;
(4) pouring and stopping heating; stopping argon conveying; opening the furnace door, and taking out the smelting crucible; preparing a prefabricated casting mold, and aligning the solution to a mold pouring gate for casting;
(5) cooling, namely embedding a die for casting molten liquid into fine sand, cooling and cooling to 25 ℃;
(6) opening the mold, opening the cooled mold, and taking out the casting;
(7) cleaning, namely placing the casting on a steel block flat plate, and cleaning the surface of the casting by using a tool to smooth the surface of the casting; polishing the surface of the casting by using fine sand paper to clean the casting; cleaning with anhydrous ethanol to clean;
(8) detection, analysis, characterization
Detecting, analyzing and characterizing the prepared quasicrystal reinforced aluminum matrix composite;
analyzing the microstructure and structure of the composite material by a metallographic microscope;
analyzing the mechanical property of the quasi-crystal reinforced aluminum-based composite material by using a universal drawing machine;
measuring the hardness of the reinforced aluminum-based composite material by using a Vickers hardness tester;
observing the microstructure appearance of the composite material by using a scanning electron microscope, and carrying out phase analysis by using an energy spectrometer;
analyzing the phase composition of the composite material by using an X-ray diffractometer;
and (4) conclusion: the quasicrystal reinforced aluminum-based composite material is in a rectangular block shape, the hardness reaches 145Hv, the tensile strength reaches 366Mpa, and the tensile strength and the hardness are respectively improved by 61.11 percent and 42.5 percent relative to a matrix.
Advantageous effects
Compared with the background technology, the invention has obvious advancement, aiming at the conditions of low mechanical property strength and poor toughness of the aluminum-based composite material, the quasicrystal particles are added into the aluminum-based composite material and are prepared into the quasicrystal reinforced aluminum-based composite material through smelting and casting so as to improve the strength and the hardness of the composite material.
Drawings
FIG. 1 is a diagram showing the melting state of a quasicrystal reinforced aluminum matrix composite
FIG. 2 is a metallographic structure diagram of a quasicrystal-reinforced aluminum matrix composite
FIG. 3 is a scanning electron microscope microscopic morphology diagram of the quasicrystal reinforced aluminum matrix composite material
FIG. 4 is a diagram of energy spectrum analysis of the micro-morphology of the quasicrystal-reinforced aluminum matrix composite
FIG. 5 is an X-ray diffraction pattern of a quasicrystal-reinforced aluminum-based composite material
As shown in the figures, the list of reference numbers is as follows:
1. vacuum melting furnace, 2, furnace chamber, 3, electromagnetic stirring device, 4, fixing plate, 5, heater, 6, melting crucible, 7, melting alloy, 8, quasicrystal particles, 9, argon, 10, gas outlet valve, 11, exhaust pipe, 12, electromagnetic stirring regulator, 13, fault reset button, 14, electric cabinet, 15, electronic display screen, 16, melting furnace ascending button, 17, power supply stop button, 18, electromagnetic stirring start button, 19, first cable, 20, vent, 21, workbench, 22, vent pipe, 23, bottom blowing motor, 24, electromagnetic stirring stop button, 25, current and voltage display screen, 26, emergency stop button, 27, vacuum pipe, 28, vacuum pump, 29, heating indicator lamp, 30, argon switch valve, 31, argon bottle, 32, heating switch, 33, power master switch, 34, melting furnace descending button, 35, power supply start button, 36. second cable, 37, power cabinet.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
FIG. 1 shows a melting state diagram of a quasicrystal reinforced aluminum matrix composite, which is operated in sequence according to the ratio of the parts to be correctly positioned and connected.
The amount of the chemical substances used for the preparation and smelting is determined according to a preset range, and the chemical substances are measured in grams, milliliters and centimeters3Is a unit of measurement.
The vacuum smelting furnace 1 is vertical, a furnace chamber 2 is arranged in the vacuum smelting furnace 1, and a workbench 21 is arranged below the furnace chamber; the electromagnetic stirring device 3 is arranged on two sides of the upper part of the workbench 21 and is fixed on the fixing plate 4; a heater 5 is arranged outside the melting crucible 6, molten melting alloy 7 and added quasicrystal particles 8 are arranged inside the melting crucible 6, and the whole process is carried out under the protection of argon 9; an air outlet valve 10 and an exhaust pipe 11 are arranged at the upper right corner of the smelting furnace chamber 2;
an electromagnetic stirring electric cabinet 14 is arranged on the right side of the vacuum smelting furnace 1, an electromagnetic stirring regulator 12 is arranged below an electronic display screen 15, and a fault reset button 13, a smelting furnace ascending button 16, a power supply stop button 17, an electromagnetic stirring start button 18 and an electromagnetic stirring stop button 24 are arranged below the electromagnetic stirring regulator 12; the electric cabinet 14 is connected with the vacuum smelting furnace 1 through a first cable 19 and a second cable 36;
a power supply cabinet 37 is arranged at the left side of the vacuum smelting furnace 1, and an emergency stop knob 26, a heating indicator lamp 29, a heating switch 32, a power main switch 33, a smelting furnace descending button 34 and a power supply starting button 35 are arranged below the current and voltage display screen 25; a vacuum pipe 27 and a vacuum pump 28 are arranged above the workbench 21; argon is connected with the vacuum smelting furnace 1 through a vent 20, a vent pipe 22 and a bottom blowing motor 23; on the left side of the power cabinet 37 are an argon switch valve 30 and an argon bottle 31.
FIG. 2 shows a metallographic structure of a quasicrystal-reinforced aluminum matrix composite, in which a black phase is a quasicrystal phase, a dark gray phase is a eutectic Si phase, and a light gray phase is an α -Al phase.
FIG. 3 shows a scanning electron microscope microscopic morphology of the quasicrystal-reinforced aluminum matrix composite, in which white quasicrystal phase is uniformly distributed in the matrix.
FIG. 4 is a diagram of energy spectrum analysis of the micro-morphology of the quasicrystal-enhanced aluminum matrix composite, in which it can be seen that the elements are uniformly distributed in the aluminum matrix.
FIG. 5 shows an X-ray diffraction pattern of a quasicrystal-reinforced aluminum-based composite material, in which α -Al is an aluminum-silicon alloy, eutectic Si is primary silicon, and a quasicrystal phase is Al72Ni13Co10Mn5

Claims (2)

1. A preparation method of a quasicrystal reinforced aluminum matrix composite material is characterized by comprising the following steps:
the chemical substance materials used are aluminum, nickel, cobalt, manganese, aluminum alloy, absolute ethyl alcohol and argon, and the combined preparation dosage is as follows: g, ml, cm3As a unit of measure
Aluminum: al block 200g + -0.01 g
Nickel: ni block 80 g. + -. 0.01g
Cobalt: co particles 60 g. + -. 0.01g
Manganese: 28 g. + -. 0.01g Mn flakes
Aluminum alloy: 3000g plus or minus 0.01g of ZL101A block
Anhydrous ethanol: c2H5OH 2000mL±50 mL
Argon gas 600000cm3±100cm3
The preparation method comprises the following steps:
(1) pretreatment of quasicrystalline materials
Firstly, 200g plus or minus 0.01g of aluminum block, 80g plus or minus 0.01g of nickel block, 60g plus or minus 0.01g of cobalt particles and 28g plus or minus 0.01g of manganese sheets are crushed into mixed particles;
secondly, ball milling, namely placing the granular quasicrystal component into a ball mill for ball milling for 30min to form quasicrystal mixed granules;
thirdly, cleaning, namely putting the quasicrystal mixed particles into an ultrasonic cleaning instrument, adding 1000mL of absolute ethyl alcohol, cleaning, and drying in the air;
drying, namely putting the dried quasicrystal mixed particles into a vacuum drying oven, wherein the drying temperature is 180 ℃, the vacuum degree is 2Pa, and the drying time is 60 min;
fifthly, high-temperature oxidation, namely placing the dried quasicrystal particles in a heat treatment furnace for high-temperature oxidation at 800 ℃ for 12 hours;
(2) aluminum alloy cutting block
Placing 3000g +/-0.01 g of aluminum alloy on a steel flat plate, and mechanically cutting into blocks with the block size of less than or equal to 80mm multiplied by 80 mm;
(3) smelting preparation of quasi-crystal reinforced aluminum-based composite material
Smelting of the quasicrystal reinforced aluminum matrix composite is carried out in a vacuum smelting furnace, and is completed under the protection of argon in the processes of heating, stirring and adding quasicrystal particles;
cleaning a smelting crucible, cleaning the smelting crucible by using a metal shovel and a metal brush, and cleaning the smelting crucible by using absolute ethyl alcohol to ensure that the smelting crucible is clean;
placing the raw materials, and placing the cut aluminum alloy at the bottom of a smelting crucible;
placing the quasicrystal particles, and uniformly placing the dried quasicrystal particles on the upper part of the aluminum alloy block in the crucible;
closing the vacuum smelting furnace, starting a vacuum pump, and extracting air in the furnace to enable the pressure in the furnace to reach 2 Pa;
introducing argon, opening a gas pressing valve and a bottom blowing motor, and introducing argon into the vacuum smelting furnace at an argon input speed of 200cm3Min, keeping the atmospheric pressure in the furnace at 1 atmosphere;
heating, starting a heater of an electromagnetic induction smelting furnace, heating at the temperature of 750 +/-2 ℃, heating for 120min, and fully melting the raw materials;
when the raw materials are completely melted, reducing the heating temperature to 650 +/-2 ℃, and preserving the heat for 10 min;
electromagnetic stirring, starting a control switch of an electromagnetic stirring device, setting electromagnetic stirring parameters, wherein the stirring frequency is 35Hz, and stirring for 10min at constant temperature;
(4) pouring and stopping heating; stopping argon conveying;
opening the furnace door, and taking out the smelting crucible;
preparing a prefabricated casting mold, and aligning the molten liquid to a mold pouring gate for casting;
(5) cooling, namely embedding a die for casting molten liquid into fine sand, cooling and cooling to 25 ℃;
(6) opening the mold, opening the cooled mold, and taking out the casting;
(7) cleaning, namely placing the casting on a steel block flat plate, and cleaning the surface of the casting by using a tool to smooth the surface of the casting;
polishing the surface of the casting by using fine sand paper to clean the casting;
cleaning with anhydrous ethanol to clean;
(8) detection, analysis, characterization
Detecting, analyzing and characterizing the prepared quasicrystal reinforced aluminum matrix composite;
analyzing the microstructure and structure of the composite material by a metallographic microscope;
measuring the hardness of the reinforced aluminum-based composite material by using a Vickers hardness tester;
observing the microstructure appearance of the composite material by using a scanning electron microscope, and carrying out phase analysis by using an energy spectrometer;
analyzing the phase composition of the composite material by using an X-ray diffractometer;
and (4) conclusion: the quasicrystal reinforced aluminum-based composite material is in a rectangular block shape, the hardness reaches 145Hv, the tensile strength reaches 366MP a, and the tensile strength and the hardness are respectively improved by 61.11 percent and 42.5 percent relative to a matrix.
2. The method for preparing a quasicrystal reinforced aluminum matrix composite material according to claim 1, wherein:
the vacuum smelting furnace (1) is vertical, a furnace chamber (2) is arranged inside the vacuum smelting furnace (1), and a workbench (21) is arranged below the furnace chamber; the electromagnetic stirring device (3) is arranged on two sides of the upper part of the workbench (21) and is fixed on the fixing plate (4); a heater (5) is arranged outside the smelting crucible (6), molten smelting alloy (7) and added quasicrystal particles (8) are arranged inside the smelting crucible (6), and the whole process is carried out under the protection of argon (9); an air outlet valve (10) and an exhaust pipe (11) are arranged at the upper right corner of the smelting furnace chamber (2);
an electromagnetic stirring electric control box (14) is arranged on the right side of the vacuum smelting furnace (1), an electromagnetic stirring regulator (12) is arranged below an electronic display screen (15), and a fault reset button (13), a smelting furnace ascending button (16), a power supply stop button (17), an electromagnetic stirring start button (18) and an electromagnetic stirring stop button (24) are arranged below the electromagnetic stirring regulator (12); the electric cabinet (14) is connected with the vacuum smelting furnace (1) through a first cable (19) and a second cable (36);
a power supply cabinet (37) is arranged on the left side of the vacuum smelting furnace (1), and an emergency stop knob (26), a heating indicator lamp (29), a heating switch (32), a power main switch (33), a smelting furnace descending button (34) and a power starting button (35) are arranged below a current and voltage display screen (25); a vacuum pipe (27) and a vacuum pump (28) are arranged above the workbench (21); argon is connected with the vacuum smelting furnace (1) through a vent (20), a vent pipe (22) and a bottom blowing motor (23); an argon switch valve (30) and an argon bottle (31) are arranged on the left side of the power supply cabinet (37).
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CN114111335B (en) * 2021-11-25 2023-09-15 北京中辰至刚科技有限公司 Double-cavity double-crucible exchange suspension smelting furnace

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300905A (en) * 2017-12-30 2018-07-20 安徽玉成光华铝业有限公司 A kind of automotive wheel dedicated aluminium alloy material that impact resistance is strong
CN109825729A (en) * 2019-03-07 2019-05-31 中北大学 A kind of preparation method of quasi-crystalline substance reinforced aluminum matrix composites
CN109881036A (en) * 2019-04-23 2019-06-14 河北工业大学 A kind of preparation method being electromagnetically shielded foamed aluminium composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300905A (en) * 2017-12-30 2018-07-20 安徽玉成光华铝业有限公司 A kind of automotive wheel dedicated aluminium alloy material that impact resistance is strong
CN109825729A (en) * 2019-03-07 2019-05-31 中北大学 A kind of preparation method of quasi-crystalline substance reinforced aluminum matrix composites
CN109881036A (en) * 2019-04-23 2019-06-14 河北工业大学 A kind of preparation method being electromagnetically shielded foamed aluminium composite material

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