CN116716507A - Nanoscale TiB 2p 6201 porcelain rigid aluminum alloy, ultralow-temperature smelting synthesis method and application thereof - Google Patents

Nanoscale TiB 2p 6201 porcelain rigid aluminum alloy, ultralow-temperature smelting synthesis method and application thereof Download PDF

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CN116716507A
CN116716507A CN202310678103.2A CN202310678103A CN116716507A CN 116716507 A CN116716507 A CN 116716507A CN 202310678103 A CN202310678103 A CN 202310678103A CN 116716507 A CN116716507 A CN 116716507A
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tib
aluminum alloy
porcelain
temperature
alloy
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陈宗宁
郝志刚
郭恩宇
康慧君
王同敏
赵凯
卢一平
接金川
张宇博
曹志强
李廷举
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Dalian University of Technology
Ningbo Research Institute of Dalian University of Technology
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Dalian University of Technology
Ningbo Research Institute of Dalian University of Technology
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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
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
    • 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
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
    • 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/047—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/023—Alloys based on aluminium

Abstract

The invention provides a nano TiB 2p The preparation method of the 6201 porcelain aluminum alloy comprises the following steps: and (3) preparing a precursor by casting: al (Al)-10Ti and Al-3B intermediate alloy is heated and melted, mechanical stirring is combined with ultrasonic melt treatment to accelerate the reaction, and the reaction temperature is kept between 660 and 670 ℃ to synthesize nano-scale particles at low temperature; remelting and diluting; homogenizing; hot rolling; solution treatment; rolling at room temperature; preparing nano TiB after artificial aging treatment 2p 6201 porcelain steel aluminum alloy. The aluminum alloy has excellent mechanical property and conductivity, and compared with the traditional aluminum material for power transmission, the aluminum alloy for power transmission introduces nano TiB 2 The ceramic particles are synthesized at low temperature by adopting a fusion casting method, are tightly combined with the traditional preparation flow of the aluminum material for power transmission, are easy to popularize, have low cost and can be produced in large scale.

Description

Nanoscale TiB 2p 6201 porcelain rigid aluminum alloy, ultralow-temperature smelting synthesis method and application thereof
Technical Field
The invention relates to a new material technology, in particular to a nano TiB 2p 6201 porcelain aluminum alloy, and its ultra-low temperature smelting synthesis method and use.
Background
The large-scale preparation of the nano-scale particle reinforced metal matrix composite material has great research significance and application value. The size effect of the reinforcing phase in the particle-reinforced metal matrix composite is the most critical factor in determining the mechanical properties of the composite, and the finer the particles, the higher the strength. How to reduce the particle size of the particles during their preparation has become a great importance in further improving their strength.
In situ generation of TiB by fluoride salt reaction method 2 The ceramic particle reinforced aluminum matrix composite is tightly combined with the traditional aluminum alloy casting process, has wide application, and has great potential in the application field of transmission wires. TiB (TiB) 2 The introduction of ceramic particles not only can refine grains and improve strength and elongation, but also can improve the rigidity of the lead, thereby reducing sag and improving safety. Because of the low content of ceramic particles added (0.5-2 wt.%), this material is called a ceramic-steel-aluminium alloy.
Preparation of TiB in porcelain aluminum alloy by fluoride salt reaction method 2 The particle size of the ceramic particles is in the range of several hundred nanometers to several micrometers. From the nucleation growth of the crystals, the higher the temperature during the in-situ generation and growth of the ceramic particles, the faster the atomic diffusion speed, resulting in a larger particle size of the final particles. The thermodynamic condition of the reaction system is higher, the reaction temperature is generally 800-900 ℃, the reaction temperature is further reduced to cause incomplete, insufficient and even impossible reaction, the reaction itself belongs to thermit reaction, a large amount of heat is released, and the reaction temperature is inevitably increased. Therefore, how to put forward a new idea to reduce the reaction temperature and obtain the nano TiB 2 The ceramic particle reinforced phase has become the key to preparing high performance ceramic steel aluminum alloys.
Disclosure of Invention
The invention aims at solving the problem that the thermodynamic condition of a reaction system for preparing porcelain aluminum alloy by a traditional fluoride salt reaction method is high, and provides a nano-scale TiB 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain aluminum alloy is based on a master alloy reaction method, can further reduce the size of a particle reinforced phase, and has the advantages of low smelting temperature, simple process and low cost, and the prepared porcelain aluminum alloy has excellent mechanical property and conductivity.
In order to achieve the aim, the invention adopts the technical proposal thatThe method comprises the following steps: nanoscale TiB 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain aluminum alloy comprises the following steps:
step (1) raw material preparation: 1) Al-10Ti intermediate alloy (Al-10% Ti, mass fraction, the invention% is mass percent unless otherwise specified), wherein Ti element exists in the form of trace solid solution atoms and mainly comprises Al 3 The Ti intermetallic compound exists; 2) Al-3B master alloy (Al-3% B) in which B element is AlB 2 The ceramic particles are in the form; 3) Al-10Mg master alloy (Al-10% Mg); 4) Al-12Si master alloy (Al-12% Si); 5) Industrial pure aluminum (purity)>99.7％)；
And (2) preparing a precursor by casting: 1) The Al-10Ti intermediate alloy and the Al-3B intermediate alloy are proportioned according to the stoichiometric ratio of B/Ti of 2.0-2.1; 2) Simultaneously placing the two intermediate alloys into a graphite clay crucible, heating in a well-type smelting resistance furnace to 710-720 ℃, and immediately cooling the melt to 670-680 ℃; 3) Mechanical stirring (the rotating speed is 600-800 r/min, the same applies below) is applied for 5-10 min, and the temperature of a melt is 660-670 ℃; 4) Ultrasonic melt treatment (with the frequency of 20kHz, the power of 400-500W and the same applies below) is applied for 8-10 min, and the melt temperature is 660-670 ℃; 5) Mechanical stirring is applied for 15-20 min, and the temperature of a melt is 660-670 ℃; 6) Preserving heat for 20min at 660-670 ℃; 7) Applying ultrasonic melt treatment for 8-10 min, wherein the temperature of the melt is 660-670 ℃; 8) Mechanical stirring is applied for 15-20 min, and the temperature of a melt is 660-670 ℃; 9) Introducing high-purity argon gas to refine the melt for 3-5 min;10 Skimming; 11 Pouring to obtain Al-nTiB 2 A precursor;
and (3) remelting and diluting: 1) The Al-nTiB is subjected to 2 Precursor, al-10Mg master alloy, al-12Si master alloy and industrial pure aluminum according to 9-10: 5.2 to 6.2:4.8 to 5: 78.8-81, and simultaneously placing the materials into a graphite clay crucible for heating to 710-720 ℃ and stirring to fully mix the materials; 2) Preserving heat for 5-10 min; 3) Refining high-purity argon for 3-5 min; 4) Treating the ultrasonic melt for 3-5 min; 5) Pouring to obtain nano TiB 2p 6201 porcelain steel aluminum alloy ingot casting;
and (4) homogenizing: the nano TiB 2p 6201 porcelain steel aluminum alloy cast ingotPreserving heat in a muffle furnace at 540-570 ℃ for 12-24 h, cooling to 250-300 ℃ along with the furnace, and air-cooling to avoid coarsening of precipitated phases;
and (5) hot rolling: preheating the homogenized cast ingot to 450-470 ℃, preserving heat for 30-60 min, adopting a double-roll mill to carry out hot rolling, wherein the total rolling reduction is 20-30%, the rolling reduction of each pass is 3-5%, and the roller speed is 100-150 r/min;
and (6) solution treatment: putting the hot rolled plate into a muffle furnace for solid solution treatment, wherein the solid solution temperature is 550-570 ℃, the heat preservation time is 30-60 min, and the water quenching is carried out at room temperature;
and (7) rolling at room temperature: adopting a double-roller mill to roll the solid solution product at room temperature, wherein the total rolling reduction is 75-80%, the rolling reduction of each pass is 3-4%, and the roller speed is 50-100 r/min;
and (8) aging: and (3) adopting an ageing furnace to perform artificial ageing treatment, wherein the temperature is 160-170 ℃ and the time is 3-5 h.
Further, al-nTiB prepared in the step (2) 2 TiB in precursor 2 The ceramic particles are present in an amount of 4.5 to 5.5%, preferably 5%.
Further, the nano-scale TiB prepared in the step (3) 2p TiB in/6201 porcelain steel aluminum alloy cast ingot 2 The ceramic particles content is 0.45-0.55%, preferably 0.5%.
Further, the nano-scale TiB prepared in the step (3) 2p Mg in the 6201 porcelain aluminum alloy ingot is 0.6-0.9%, si is 0.5-0.9%, fe content of impurities is less than 0.2%, and the content of each impurity is less than 0.1%.
Further, all raw materials in the step (2) and the step (3) are dried in a drying box for 30-60 min before smelting, and the drying temperature is 200-220 ℃.
Further, in the step (6), the heat preservation temperature and the heat preservation time of the solution treatment are strictly controlled, so that the recrystallization coarsening of crystal grains in the hot rolled structure is prevented.
Another object of the invention also discloses a nano-scale TiB 2p The 6201 porcelain steel aluminum alloy is prepared by adopting the method.
Further, the nano-scale TiB 2p The 6201 porcelain steel aluminum alloy comprises the following components in parts by weight:
TiB 2 0.45～0.55％；
Mg 0.6～0.9％；
Si 0.5～0.9％；
the Fe content of impurities is lower than 0.2%;
each other impurity content was less than 0.1%;
the balance being Al.
Further, preferably the nanoscale TiB 2p The 6201 porcelain steel aluminum alloy comprises the following components in parts by weight:
TiB 2 0.5％；
Mg 0.6％；
Si 0.6％；
the Fe content of impurities is lower than 0.2%;
each other impurity content was less than 0.1%;
the balance being Al.
Further, the nano-scale TiB 2p The ceramic-steel aluminum alloy particles of the 6201 are 10-100 nanometers.
Another object of the invention also discloses a nano-scale TiB 2p Application of the 6201 porcelain aluminum alloy in the field of high-strength high-conductivity transmission aluminum materials.
Further, the nano-scale TiB 2p The tensile strength of the 6201 porcelain aluminum alloy is 375-380 MPa, the elongation after fracture is 6.8-7.1%, and the conductivity is 56.2-56.4% IACS; for example nano-scale TiB 2p TiB in 6201 porcelain rigid aluminum alloy 2 When the content of the ceramic particles is 0.5%, the tensile strength reaches 380MPa, the elongation after fracture is 6.8%, and the conductivity reaches 56.3% IACS.
The nano TiB of the invention 2p The 6201 porcelain aluminum alloy, the ultralow-temperature smelting synthesis method and the application thereof have the following advantages compared with the prior art:
1. the method adopts the casting method to prepare the porcelain aluminum alloy, is tightly combined with the preparation flow of the traditional power transmission aluminum material, is easy to popularize, has low cost and can be produced in large scale.
2. Compared with a fluoride salt reaction method, the ultra-low temperature smelting synthetic method of the invention has 1) the product has only a strengthening phase and a matrix, and no other reaction products; 2) The reaction is carried out in the whole melt, and the fluoride salt reaction method is carried out only at the molten salt/melt interface; 3) The reaction of the invention can be carried out at ultralow temperature (660-670 ℃), and the reaction does not release a large amount of heat.
3. Al-nTiB prepared by the method of the invention 2 Obtaining a large amount of nano TiB in the precursor 2 Ceramic particles with a minimum particle size as low as tens of nanometers. The nano TiB prepared by the invention 2p The grain diameter of the majority of the grains of the 6201 porcelain aluminum alloy is 10-100 nanometers.
4. The nano TiB prepared by the method of the invention 2p The 6201 porcelain aluminum alloy has excellent mechanical property and conductivity, such as TiB 2 When the content of the ceramic particles is only 0.5%, the tensile strength reaches 380MPa, the elongation after fracture is 6.8%, and the conductivity reaches 56.3% IACS.
In the invention, P represents particles, particle, n represents nano, nano and mu represents micro.
Drawings
FIG. 1 is an Al-nTiB prepared in example 1 2 The morphology and the size of ceramic particles in the precursor, wherein the graph (a) is a scanning electron microscope image of the 3D morphology of the particles after the deep corrosion, the graph (b) is an enlarged image of the graph (a), and the graph (c) is a transmission electron microscope image of the morphology of the particles.
FIG. 2 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Engineering stress-engineering strain curve of the 6201 porcelain steel aluminum alloy.
FIG. 3 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Conductivity of the 6201 porcelain aluminum alloy.
FIG. 4 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Scanning electron microscope image of the fracture morphology of 6201 porcelain aluminum alloy.
Detailed Description
The invention is further illustrated by the following examples:
comparative example 1
The comparative example discloses a preparation method of 6201 aluminum alloy for power transmission aluminum materials, which comprises the following steps:
step (1) raw material preparation
1) Industrial pure aluminum (purity > 99.7%) with mass fraction 88.8%; 2) Al-10Mg intermediate alloy with mass fraction of 6.2%; 3) Al-12Si intermediate alloy with mass fraction of 5%; 4) The raw materials are dried for 30min by adopting a drying box before smelting, and the temperature is 200 ℃; 5) The prepared 6201 aluminum alloy comprises 0.6% of Mg,0.6% of Si, the content of Fe is lower than 0.2%, and the content of each other impurity is lower than 0.1%.
Smelting in step (2)
1) Simultaneously placing the Al-10Mg intermediate alloy, the Al-12Si intermediate alloy and the industrial pure aluminum into a graphite clay crucible, heating to 720 ℃, and stirring to fully mix the materials; 2) Preserving heat for 10min; 3) Refining high-purity argon for 5min; 4) Treating the ultrasonic melt for 3min; 5) And pouring to prepare the 6201 aluminum alloy cast ingot.
Step (3) homogenization treatment
The 6201 aluminum alloy ingot is insulated for 12 hours at 560 ℃ in a muffle furnace, cooled to 300 ℃ along with the furnace, and air-cooled to avoid coarsening of precipitated phases.
Step (4) hot rolling
Preheating the homogenized cast ingot to 460 ℃, preserving heat for 60min, and adopting a double-roll mill to carry out hot rolling, wherein the total reduction is 30%, the reduction of each pass is 5%, and the roll speed is 150r/min;
step (5) solution treatment
And (3) putting the hot rolled plate into a muffle furnace for solid solution treatment, wherein the solid solution temperature is 560 ℃, the heat preservation time is 30min, and the water quenching is carried out at room temperature.
Step (6) room temperature rolling
The solid solution sample is rolled at room temperature by a double-roller mill, the total rolling reduction is 78.6 percent, the rolling reduction of each pass is 3.6 percent, and the roller speed is 50r/min.
Step (7) aging
And (3) adopting an aging furnace to perform artificial aging treatment, wherein the temperature is 170 ℃ and the time is 4 hours.
Comparative example 2:
the comparative example discloses a method for synthesizing micron-sized TiB by using a fluorite reaction method 2p The preparation method of the 6201 porcelain rigid aluminum alloy for the power transmission aluminum material comprises the following steps:
step (1) raw material preparation: 1) Al- μTiB produced in industrial ton level 2 Precursor (containing micron-sized TiB) 2 Granular aluminum material), wherein the contents of Ti element and B element are respectively 4.01 percent and 1.75 percent, and the mass fraction of the added Ti element and B element is 8.3 percent; 2) Al-10Mg intermediate alloy with mass fraction of 6.2%; 3) Al-12Si intermediate alloy with mass fraction of 5%; 4) Industrial pure aluminum (purity)>99.7 percent of the total mass fraction of the alloy is 80.5 percent; 5) The raw materials are dried for 30min by adopting a drying box before smelting, and the temperature is 200 ℃; 6) For preparing micron-sized TiB 2p The grain content of the 6201 porcelain rigid aluminum alloy is 0.5%, other components are 0.6% of Mg,0.6% of Si, the Fe impurity content is less than 0.2%, and the impurity content of each other is less than 0.1%.
Smelting: 1) Al-6% μTiB 2 Simultaneously placing the precursor, the Al-10Mg intermediate alloy, the Al-12Si intermediate alloy and the industrial pure aluminum into a graphite clay crucible, heating to 720 ℃, and stirring to fully mix the materials; 2) Preserving heat for 10min; 3) Refining high-purity argon for 5min; 4) Treating the ultrasonic melt for 3min; 5) Pouring to obtain TiB 2μp 6201 porcelain steel aluminum alloy ingot casting.
And (3) homogenizing: tiB (TiB) 2μp The/6201 porcelain aluminum alloy ingot is insulated for 12 hours at 560 ℃ in a muffle furnace, cooled to 300 ℃ along with the furnace, and air-cooled to avoid coarsening of precipitated phases.
And (4) hot rolling: preheating the homogenized cast ingot to 460 ℃, preserving heat for 60min, and adopting a double-roll mill to carry out hot rolling, wherein the total reduction is 30%, the reduction of each pass is 5%, and the roll speed is 150r/min.
And (5) solution treatment: and (3) putting the hot rolled plate into a muffle furnace for solid solution treatment, wherein the solid solution temperature is 560 ℃, the heat preservation time is 30min, and the water quenching is carried out at room temperature.
And (6) rolling at room temperature: the solid solution sample is rolled at room temperature by a double-roller mill, the total rolling reduction is 78.6 percent, the rolling reduction of each pass is 3.6 percent, and the roller speed is 50r/min.
Step (7) aging
And (3) adopting an aging furnace to perform artificial aging treatment, wherein the temperature is 170 ℃ and the time is 4 hours.
Example 1
The embodiment discloses a method for synthesizing nano TiB by ultra-low temperature smelting 2p The preparation method of the 6201 porcelain steel aluminum alloy comprises the following steps:
step (1) raw material preparation
1) Al-10Ti intermediate alloy, wherein Ti element is mainly Al 3 The Ti intermetallic compound exists; 2) Al-3B master alloy in which B element is AlB 2 The ceramic particles are in the form; 3) Al-10Mg intermediate alloy; 4) Al-12Si master alloy; 5) Industrial pure aluminum (purity)>99.7%); 6) The raw materials are dried for 30min by adopting a drying box before smelting, and the temperature is 200 ℃.
Step (2) preparation of precursor by casting
1) Al-10Ti master alloy, al-3B master alloy and industrial pure aluminum were mixed according to 34.2:51.8:14, simultaneously placing the mixture into a graphite clay crucible, heating the mixture to 720 ℃ in a well-type smelting resistance furnace, and immediately cooling the melt to 680 ℃; 3) Mechanical stirring (with the rotating speed of 700r/min, the same applies below) is applied for 10min, and the temperature of a melt is 660 ℃; 4) Applying ultrasonic melt treatment (frequency 20kHz, power 400W, the same applies below) for 10min, and melt temperature 660 ℃; 5) Mechanical stirring is applied for 20min, and the temperature of a melt is 660 ℃; 6) Preserving heat at 660 ℃ for 20min; 7) Applying ultrasonic melt treatment for 10min, wherein the melt temperature is 660 ℃; 8) Mechanical stirring is applied for 20min, and the temperature of a melt is 660 ℃; 9) Refining the melt for 5min by introducing high-purity argon; 10 Skimming; 11 Casting to obtain Al-5% nTiB 2 Precursor ingot casting.
Step (3) remelting dilution
1) Al-nTiB 2 Precursor, al-10Mg master alloy, al-12Si master alloy and industrial pure aluminum according to the following weight ratio of 10:6.2:5:78.8, simultaneously placing the materials into a graphite clay crucible, heating to 720 ℃, and stirring to fully mix the materials; 2) Preserving heat for 10min; 3) Refining high-purity argon for 5min; 4) Treating the ultrasonic melt for 3min; 5) Pouring to obtain TiB 2np 6201 porcelain steel aluminum alloy ingot casting.
Step (4) homogenization treatment
TiB 2np The/6201 porcelain aluminum alloy ingot is insulated for 12 hours at 560 ℃ in a muffle furnace, cooled to 300 ℃ along with the furnace, and air-cooled to avoid coarsening of precipitated phases.
Step (5) hot rolling
Preheating the homogenized cast ingot to 460 ℃, preserving heat for 60min, and adopting a double-roll mill to carry out hot rolling, wherein the total reduction is 30%, the reduction of each pass is 5%, and the roll speed is 150r/min.
Step (6) solution treatment
And (3) putting the hot rolled plate into a muffle furnace for solid solution treatment, wherein the solid solution temperature is 560 ℃, the heat preservation time is 30min, and the water quenching is carried out at room temperature.
Step (7) room temperature rolling
The solid solution sample is rolled at room temperature by a double-roller mill, the total rolling reduction is 78.6 percent, the rolling reduction of each pass is 3.6 percent, and the roller speed is 50r/min.
Step (8) aging
And (3) adopting an aging furnace to perform artificial aging treatment, wherein the temperature is 170 ℃ and the time is 4 hours.
The nano TiB prepared in the embodiment 2p The/6201 porcelain rigid aluminum alloy can be used as a high-strength high-conductivity transmission aluminum material.
By combining comparative example 1, comparative example 2 and example 1, the synthesized nano-scale TiB thereof 2 Morphology and size of the particles, 6201 aluminum alloy, tiB 2μp 6201 porcelain rigid aluminum alloy and TiB 2np The mechanical property, the conductivity and the stretching fracture morphology of the 6201 porcelain rigid aluminum alloy are shown in figures 1 to 4:
FIG. 1 is an Al-nTiB prepared in example 1 2 The morphology and the size of ceramic particles in the precursor, wherein the graph (a) is a scanning electron microscope image of the 3D morphology of the particles after the deep corrosion, the graph (b) is an enlarged image of the graph (a), and the graph (c) is a transmission electron microscope image of the morphology of the particles. From the figure, it can be seen that the hexagonal prism plate-shaped TiB which is more mature except for hundreds of nanometers 2 The ceramic particles are externally attached with a huge amount of nano TiB 2 And (3) particles. From transmission electron microscope imagesIt can be seen that the nano-sized particles also take the shape of regular hexagons, which vary in size from tens to hundreds of nanometers, and that many finer particles can be observed. On the whole, ultra-low temperature smelting and synthesizing nano TiB 2 The particles have a larger size range of tens to hundreds of nanometers, and the number of the tens of nanometer particles is huge, so that the particles play a key strengthening role in the porcelain aluminum alloy.
FIG. 2 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Engineering stress-engineering strain curve of the 6201 porcelain steel aluminum alloy. From the graph, the tensile strength of the 6201 aluminum alloy is the lowest and is only 325MPa, the tensile strength is improved to 334.8MPa after 0.5% of micron-sized particles are introduced, the improvement effect is not obvious, and the tensile strength is improved to 380.1MPa after 0.5% of nanometer-sized particles are introduced, the improvement effect is obvious, and the improvement of the strength brought by the refined particles is huge. In terms of elongation after break, the elongation after break of the 6201 aluminum alloy is 7.8%, and the strength of the introduced 0.5% micron-sized particles is not reduced but is increased to 9.6%, because the micron-sized particles serve as fine grains when heterogeneous core particles, thereby increasing the elongation. The elongation after breaking is reduced by introducing 0.5% of nano-sized particles, but the uniform elongation is increased, which means that the nano-sized particles can achieve a synergistic increase in the strength and plasticity.
FIG. 3 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Conductivity of the 6201 porcelain aluminum alloy. As can be seen from the graph, the electrical conductivity of the 6201 aluminum alloy is only 49.5% IACS, the electrical conductivity is only slightly improved after 0.5% of micron-sized particles are introduced, but the electrical conductivity is greatly improved after 0.5% of nanometer-sized particles are introduced, because the dimensions of the nanometer-sized particles and the precipitated phases are nearly the same order of magnitude, the huge number of nanometer-sized particles introduce a large number of particle/matrix phase interfaces, and meanwhile, during the heat treatment and deformation process, a large number of CTE dislocation and geometric necessary dislocation are generated around the particles due to the difference of the elastic modulus of two phases, and the dislocation and the phase interfaces become the flux of rapid diffusion of solid solution elementsThe precipitation process is further promoted, so that solid solution atoms are precipitated as much as possible, and the damage to the conductivity is reduced.
FIG. 4 is a schematic diagram of the 6201 aluminum alloy, tiB, prepared in comparative example 1, comparative example 2 and example 1 2μp 6201 porcelain rigid aluminum alloy and TiB 2np Scanning electron microscope image of the fracture morphology of 6201 porcelain aluminum alloy. From the graph, it can be seen that the fracture behavior of the 6201 aluminum alloy and the two porcelain aluminum alloys both belong to plastic fracture, and a large number of plastic fracture ductile fosters are generated. Except that the ductile fossa of the 6201 aluminum alloy is large in size, while the fracture ductile fossa of the porcelain aluminum alloy is very fine and deep, wherein TiB 2np Not only the/6201 porcelain rigid aluminum alloy exists and TiB 2μp The same micron-sized ductile fossa of the 6201 porcelain aluminum-steel alloy also has a large number of nanometer-sized ductile fossa, because the introduction of the nanometer-sized particles leads to the generation of a large number of small-angle grain boundaries on the substrate, and the size of the subgrain is very small, thereby generating a remarkable strengthening effect on the substrate, while TiB 2μp The ductile fossa of the/6201 porcelain aluminum alloy is deeper, which is also the reason for the higher elongation.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (10)

1. Nanoscale TiB 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain aluminum alloy is characterized by comprising the following steps of:
step (1) raw material preparation: 1) Al-10Ti master alloy; 2) Al-3B intermediate alloy; 3) Al-10Mg intermediate alloy; 4) Al-12Si master alloy; 5) Industrial pure aluminum;
and (2) preparing a precursor by casting: 1) The Al-10Ti intermediate alloy and the Al-3B intermediate alloy are processed according to the stoichiometric ratio of B/Ti of 2.0-2.1Proportioning; 2) Simultaneously placing the two intermediate alloys into a graphite clay crucible, heating in a well-type smelting resistance furnace to 710-720 ℃, and immediately cooling the melt to 670-680 ℃; 3) Mechanical stirring is applied for 5-10 min, and the temperature of a melt is 660-670 ℃; 4) Applying ultrasonic melt treatment for 8-10 min, wherein the temperature of the melt is 660-670 ℃; 5) Mechanical stirring is applied for 15-20 min, and the temperature of a melt is 660-670 ℃; 6) Preserving heat for 20min at 660-670 ℃; 7) Applying ultrasonic melt treatment for 8-10 min, wherein the temperature of the melt is 660-670 ℃; 8) Mechanical stirring is applied for 15-20 min, and the temperature of a melt is 660-670 ℃; 9) Introducing high-purity argon gas to refine the melt for 3-5 min;10 Skimming; 11 Pouring to obtain Al-nTiB 2 A precursor;
and (3) remelting and diluting: 1) The Al-nTiB is subjected to 2 Precursor, al-10Mg master alloy, al-12Si master alloy and industrial pure aluminum according to 9-10: 5.2 to 6.2:4.8 to 5: 78.8-81, and simultaneously placing the materials into a graphite clay crucible for heating to 710-720 ℃ and stirring to fully mix the materials; 2) Preserving heat for 5-10 min; 3) Refining high-purity argon for 3-5 min; 4) Treating the ultrasonic melt for 3-5 min; 5) Pouring to obtain nano TiB 2p 6201 porcelain steel aluminum alloy ingot casting;
homogenizing;
step (5) hot rolling;
step (6) solid solution treatment;
step (7) rolling at room temperature;
and (8) aging.
2. The nanoscale TiB of claim 1 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain rigid aluminum alloy is characterized in that the Al-nTiB prepared in the step (2) 2 TiB in precursor 2 The content of the ceramic particles is 4.5-5.5%.
3. The nanoscale TiB of claim 1 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain rigid aluminum alloy is characterized in that the nano TiB prepared in the step (3) 2p TiB in/6201 porcelain steel aluminum alloy cast ingot 2 The content of the ceramic particles is 0.45-0.55%.
4. The nanoscale TiB of claim 1 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain rigid aluminum alloy is characterized in that the nano TiB prepared in the step (3) 2p Mg in the 6201 porcelain aluminum alloy ingot is 0.6-0.9%, si is 0.5-0.9%, fe content of impurities is less than 0.2%, and the content of each impurity is less than 0.1%.
5. The nanoscale TiB of claim 1 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain aluminum alloy is characterized in that all raw materials in the step (2) and the step (3) are dried in a drying box for 30-60 min before smelting, and the drying temperature is 200-220 ℃.
6. The nanoscale TiB of claim 1 2p The ultra-low temperature smelting synthesis method of the 6201 porcelain aluminum alloy is characterized in that the homogenization treatment of the step (4) is as follows: the ceramic-steel aluminum alloy ingot is kept at 540-570 ℃ for 12-24 hours in a muffle furnace, cooled to 250-300 ℃ along with the furnace, and air-cooled to avoid coarsening of precipitated phases;
and/or, step (5) hot rolling: preheating the homogenized cast ingot to 450-470 ℃, preserving heat for 30-60 min, adopting a double-roll mill to carry out hot rolling, wherein the total rolling reduction is 20-30%, the rolling reduction of each pass is 3-5%, and the roller speed is 100-150 r/min;
and/or, step (6) of solid solution treatment: putting the hot rolled plate into a muffle furnace for solid solution treatment, wherein the solid solution temperature is 550-570 ℃, the heat preservation time is 30-60 min, and the water quenching is carried out at room temperature;
and/or, step (7) room temperature rolling: adopting a double-roller mill to roll the solid solution product at room temperature, wherein the total rolling reduction is 75-80%, the rolling reduction of each pass is 3-4%, and the roller speed is 50-100 r/min;
and/or, step (8) aging: and (3) adopting an ageing furnace to perform artificial ageing treatment, wherein the temperature is 160-170 ℃ and the time is 3-5 h.
7. Nanoscale TiB 2p 6201 porcelain aluminium alloy, characterized in that it is used according to any one of claims 1 to 6The method is used for preparing the product.
8. The nanoscale TiB of claim 7 2p The 6201 porcelain rigid aluminum alloy is characterized in that the nano TiB 2p The 6201 porcelain steel aluminum alloy comprises the following components in parts by weight:
TiB 2 0.45～0.55％；
Mg 0.6～0.9％；
Si 0.5～0.9％；
the Fe content of impurities is lower than 0.2%; each other impurity content was less than 0.1%;
the balance being Al.
9. The nanoscale TiB of claim 7 2p The 6201 porcelain rigid aluminum alloy is characterized in that the nano TiB 2p The tensile strength of the/6201 porcelain aluminum alloy is 375-380 MPa, the elongation after fracture is 6.8-7.1%, and the conductivity is 56.2-56.4% IACS.
10. A nano-sized TiB as claimed in any one of claims 7 to 9 2p Application of the 6201 porcelain aluminum alloy in the field of high-strength high-conductivity transmission aluminum materials.
CN202310678103.2A 2023-06-09 2023-06-09 Nanoscale TiB 2p 6201 porcelain rigid aluminum alloy, ultralow-temperature smelting synthesis method and application thereof Pending CN116716507A (en)

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