CN107385291B - A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and its preparation process - Google Patents

A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and its preparation process Download PDF

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CN107385291B
CN107385291B CN201710480732.9A CN201710480732A CN107385291B CN 107385291 B CN107385291 B CN 107385291B CN 201710480732 A CN201710480732 A CN 201710480732A CN 107385291 B CN107385291 B CN 107385291B
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aluminium
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CN107385291A (en
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尹登峰
程仁策
余鑫祥
祝贞凤
李铸铁
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Yantai Nanshan University
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    • 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
    • C22C21/10—Alloys based on aluminium with zinc as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making alloys
    • C22C1/02—Making alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making alloys
    • C22C1/02—Making alloys by melting
    • C22C1/03—Making alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making alloys
    • C22C1/06—Making 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
    • 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
    • C22F1/053—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 zinc as the next major constituent

Abstract

This patent discloses a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and its preparation processes, micro Ce and Ti is added on base alloy component base, and the feature processes such as the annealing of preparation process combination two-step homogenization and double_stage guide processing, make 20% or more the Fracture Toughness raising of alloy aluminum, zinc, magnesium, copper, zirconium, cerium (AlZnMgCuZrCeTi) alloy ratio base alloy (AlZnMgCuZr) of the present invention.

Description

A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and its preparation process
Technical field
The present invention relates to alloy production preparation method, specifically a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and Its preparation process.
Background technique
7000 be the superhard series alloys of Al-Zn-Mg-Cu be heat-treatable strengthened type alloy, has that density is small, intensity High, the advantages that processing performance is good, it is widely used in aerospace civilian industry, is one of primary structural material of aerospace, It is also used widely in communications and transportation and other Ministry of Industry simultaneously.As the development people of aerospace industry gradually recognize Fracture toughness oneself become the bottleneck further applied of limitation high strength alumin ium alloy.With the hair of linear elasticity and fracture toughness mechanics The application of exhibition and fail safety design principle in actual operation, people are tough to structural material especially high strength alumin ium alloy fracture Property importance understanding it is clearer, how to further increase 7000 be Al-Zn-Mg-Cu alloy fracture toughness become aluminium The target that alloy research worker pursues jointly.
Summary of the invention
Invention is to design a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy and its preparation process, on basis Micro Ce and Ti, and the features such as the annealing of preparation process combination two-step homogenization and double_stage guide processing are added on the basis of alloying component Technique, making invention alloy ratio 7000 is the fracture toughness (K of Al-Zn-Mg-Cu-Zr base alloy1C) significantly improve, K1CValue improves 20% or more.The main contents of invention are as follows:
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy, which is characterized in that the alloy described by weight percentage by Following components composition: zinc 5.4-6.5%, magnesium 1.7-2.7%, copper 1.5-2.5%, zirconium 0.07-0.15%, cerium 0.05-0.18%, titanium 0.08-0.16%, other content of impurities are no more than 0.1 %, and single impurity component content is no more than 0.05%, remaining is Al.
Further, the impurity is one or more of iron, silicon, manganese, ytterbium.
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy preparation technology, which is characterized in that alloy preparation technology packet Include following below scheme: ingredient, melting casting, Homogenization Treatments, hot rolling, cold rolling, double_stage guide processing, quenching, ageing treatment, specifically Operating procedure is as follows:
1) ingredient: raw materials are as follows: rafifinal (99.95%), pure magnesium (99.99%), aluminum bronze intermediate alloy (0.12%) aluminium-copper content accounting 50%, content of impurities are lower than, aluminium cerium intermediate alloy (aluminium-cerium content accounting 10%), aluminium zirconium Intermediate alloy (aluminium-zirconium content accounting 3%)；
2) melting is cast: being applied clay graphite paint with graphite crucible or high-purity magnesium oxide brick and is done hearth inner lining material melting conjunction Gold, fusion process add always coverture, charging sequence are as follows: industrial rafifinal -- aluminum bronze intermediate alloy -- aluminium zirconium hardener -- aluminium Cerium intermediate alloy, casts until completely melted, after carrying out first time outlet with carbon trichloride or argon gas, adds technical pure Magnesium carries out second of outlet with carbon trichloride or argon gas after being completely melt；
3) Homogenization Treatments: the ingot casting that step 2 is produced carries out Homogenization Treatments in salt bath furnace or argon gas protection stove, tool Body technology are as follows: will first be doomed 420 DEG C heat preservation 14-16 hours, then be heated to 465 DEG C of heat preservations 15-16 hours；
4) anneal before hot rolling preheating, cold rolling: concrete operations can carry out in air resistance furnace, wherein hot rolling preheating temperature For 430 DEG C ~ 440 DEG C heat preservation 3-4 hours, before cold rolling annealing temperature be 420 DEG C ~ 430 DEG C heat preservation 2-3 hours；
5) solution treatment: concrete operations carry out in salt bath furnace or argon gas protection stove, and double_stage guide treatment process is 280 DEG C/2h+475 DEG C/1h, and in room temperature quenching-in water；
6) ageing treatment: quenched alloy material is subjected to ageing treatment in two hours, ageing treatment is general permanent It is carried out in warm resistance furnace, technique are as follows: 120 DEG C/20 ~ 26h.
Further, the coverture in the step 2 closes sodium aluminate by sodium chloride, potassium chloride and hexafluoro and constitutes, by matter Amount is than being sodium chloride: potassium chloride: hexafluoro closes sodium aluminate=4:4:2.
Further, when step 1 ingredient, the scaling loss amount of magnesium is supplemented, scaling loss amount is the 2.0-4.0% of gross mass.
Further, the smelting temperature of the step 2 is about 760 ~ 780 DEG C, and cast temperature is about 690 ~ 720 DEG C.
The beneficial effects of the present invention are: with registered various 7000 be Al-Zn-Mg-Cu-Zr main alloying component range not Together, and contain RE elements of Ce and transition element Ti.Alloy aluminum of the present invention, zinc, magnesium, copper, zirconium, cerium (AlZnMgCuZrCeTi) Fracture Toughness of alloy ratio base alloy (AlZnMgCuZr) improves 20% or more.
Specific embodiment
Presently in connection with specific embodiment, the present invention is described in further detail.
Embodiment 1
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy, which is characterized in that the alloy described by weight percentage by Following components composition: zinc 5.92%, magnesium 2.35%, copper 2.15%, zirconium 0.13%, cerium 0.07%, titanium 0.11%, iron 0.045%, silicon 0.042%, remaining is Al.
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy preparation technology, which is characterized in that alloy preparation technology packet Include following below scheme: ingredient, melting casting, Homogenization Treatments, hot rolling, cold rolling, double_stage guide processing, quenching, ageing treatment, specifically Operating procedure is as follows:
1) ingredient: raw materials are as follows: rafifinal (99.95%), pure magnesium (99.99%), aluminum bronze intermediate alloy (0.12%) aluminium-copper content accounting 50%, content of impurities are lower than, aluminium cerium intermediate alloy (aluminium-cerium content accounting 10%), aluminium zirconium Intermediate alloy (aluminium-zirconium content accounting 3%)；
2) melting is cast: doing hearth inner lining material molten alloy with graphite crucible, fusion process adds always coverture, charging Sequentially are as follows: industrial rafifinal -- aluminum bronze intermediate alloy -- aluminium zirconium hardener -- aluminium cerium intermediate alloy, carries out until completely melted Casting, after carrying out first time outlet with carbon trichloride or argon gas, adds pure magnesium, and carbon trichloride or argon are used after being completely melt Gas carries out second of outlet；
3) Homogenization Treatments: the ingot casting that step 2 is produced carries out Homogenization Treatments in salt bath furnace or argon gas protection stove, tool Body technology are as follows: will first be doomed to keep the temperature 14 hours at 420 DEG C, then be heated to 465 DEG C and keep the temperature 15 hours；Two-step homogenization processing The first order 14-16 hours purposes of 420 DEG C of heat preservations of lower temperature be conducive to microalloy constituent element Ce and Ti formed secondary precipitation Disperse phase (Al8Cu4Ce, TiAl3) particle；The second level in heat preservation 15-16 hours of 465 DEG C of higher temperature be in order to make alloy at Divide full and uniform.
4) anneal before hot rolling preheating, cold rolling: concrete operations can carry out in air resistance furnace, wherein hot rolling preheating temperature 3 hours are kept the temperature for 430 DEG C, annealing temperature is 420 DEG C of heat preservations 2 hours before cold rolling；
5) solution treatment: concrete operations carry out in salt bath furnace or argon gas protection stove, and double_stage guide treatment process is 280 DEG C/2h+475 DEG C/1h, and in room temperature quenching-in water；The double_stage guide first order kept the temperature at 280 DEG C of lower temperature be within 2 hours in order to Cold deformation alloy is allowed to occur to reply release deformation and energy storage, in addition disperse phase (Al8Cu4Ce, TiAl3) particle hinders the work of recrystallization With, alloy will be made not occur as far as possible in 475 DEG C of higher temperature solution treatment, 1 hour alloy substrate or recrystallize less, and 475 DEG C of higher temperature solid solutions, 1 hour main purpose is to make alloy obtain degree of supersaturation as high as possible.
6) ageing treatment: quenched alloy material is subjected to ageing treatment in two hours, ageing treatment is general permanent It is carried out in warm resistance furnace, technique are as follows: 120 DEG C/20h.
Preferably, the coverture in step 2 closes sodium aluminate by sodium chloride, potassium chloride and hexafluoro and constitutes, and is in mass ratio Sodium chloride: potassium chloride: hexafluoro closes sodium aluminate=4:4:2.
Preferably, when step 1 ingredient, the scaling loss amount of magnesium is supplemented, scaling loss amount is the 2.0% of gross mass.
Preferably, the smelting temperature of step 2 is about 760 DEG C, and cast temperature is about 690 DEG C.
Embodiment 2
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy, which is characterized in that the alloy described by weight percentage by Following components composition: zinc 6.23%, magnesium 1.95%, copper 1.98%, zirconium 0.09%, cerium 0.12%, titanium 0.12%, iron 0.046%, silicon 0.041%, remaining is Al.
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy preparation technology, which is characterized in that alloy preparation technology packet Include following below scheme: ingredient, melting casting, Homogenization Treatments, hot rolling, cold rolling, double_stage guide processing, quenching, ageing treatment, specifically Operating procedure is as follows:
1) ingredient: raw materials are as follows: rafifinal (99.95%), pure magnesium (99.99%), aluminum bronze intermediate alloy (0.12%) aluminium-copper content accounting 50%, content of impurities are lower than, aluminium cerium intermediate alloy (aluminium-cerium content accounting 10%), aluminium zirconium Intermediate alloy (aluminium-zirconium content accounting 3%)；
2) melting is cast: doing hearth inner lining material molten alloy with graphite crucible, fusion process adds always coverture, charging Sequentially are as follows: industrial rafifinal -- aluminum bronze intermediate alloy -- aluminium zirconium hardener -- aluminium cerium intermediate alloy, carries out until completely melted Casting, after carrying out first time outlet with carbon trichloride or argon gas, adds pure magnesium, and carbon trichloride or argon are used after being completely melt Gas carries out second of outlet；
3) Homogenization Treatments: the ingot casting that step 2 is produced carries out Homogenization Treatments in salt bath furnace or argon gas protection stove, tool Body technology are as follows: will first be doomed to keep the temperature 15 hours at 420 DEG C, then be heated to 465 DEG C and keep the temperature 15 hours；
4) anneal before hot rolling preheating, cold rolling: concrete operations can carry out in air resistance furnace, wherein hot rolling preheating temperature 3 hours are kept the temperature for 435 DEG C, annealing temperature is 425 DEG C of heat preservations 2 hours before cold rolling；
5) solution treatment: concrete operations carry out in salt bath furnace or argon gas protection stove, and double_stage guide treatment process is 280 DEG C/2h+475 DEG C/1h, and in room temperature quenching-in water；
6) ageing treatment: quenched alloy material is subjected to ageing treatment in two hours, ageing treatment is general permanent It is carried out in warm resistance furnace, technique are as follows: 120 DEG C/22h.
Preferably, the coverture in step 2 closes sodium aluminate by sodium chloride, potassium chloride and hexafluoro and constitutes, and is in mass ratio Sodium chloride: potassium chloride: hexafluoro closes sodium aluminate=4:4:2.
Preferably, when step 1 ingredient, the scaling loss amount of magnesium is supplemented, scaling loss amount is the 3.0% of gross mass.
Preferably, the smelting temperature of step 2 is about 770 DEG C, and cast temperature is about 700 DEG C.
Embodiment 3
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy, which is characterized in that the alloy described by weight percentage by Following components composition: zinc 6.12%, magnesium 2.23%, copper 2.35%, zirconium 0.11%, cerium 0.12%, titanium 0.11%, iron 0.043%, silicon 0.049%, remaining is Al.
A kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy preparation technology, which is characterized in that alloy preparation technology packet Include following below scheme: ingredient, melting casting, Homogenization Treatments, hot rolling, cold rolling, double_stage guide processing, quenching, ageing treatment, specifically Operating procedure is as follows:
1) ingredient: raw materials are as follows: rafifinal (99.95%), pure magnesium (99.99%), aluminum bronze intermediate alloy (0.12%) aluminium-copper content accounting 50%, content of impurities are lower than, aluminium cerium intermediate alloy (aluminium-cerium content accounting 10%), aluminium zirconium Intermediate alloy (aluminium-zirconium content accounting 3%)；
2) melting is cast: doing hearth inner lining material molten alloy with graphite crucible, fusion process adds always coverture, charging Sequentially are as follows: industrial rafifinal -- aluminum bronze intermediate alloy -- aluminium zirconium hardener -- aluminium cerium intermediate alloy, carries out until completely melted Casting, after carrying out first time outlet with carbon trichloride or argon gas, adds pure magnesium, and carbon trichloride or argon are used after being completely melt Gas carries out second of outlet；
3) Homogenization Treatments: the ingot casting that step 2 is produced carries out Homogenization Treatments in salt bath furnace or argon gas protection stove, tool Body technology are as follows: will first be doomed to keep the temperature 16 hours at 420 DEG C, then be heated to 465 DEG C and keep the temperature 16 hours；
4) anneal before hot rolling preheating, cold rolling: concrete operations can carry out in air resistance furnace, wherein hot rolling preheating temperature 3 hours are kept the temperature for 440 DEG C, annealing temperature is 430 DEG C of heat preservations 2 hours before cold rolling；
5) solution treatment: concrete operations carry out in salt bath furnace or argon gas protection stove, and double_stage guide treatment process is 280 DEG C/2h+475 DEG C/1h, and in room temperature quenching-in water；
6) ageing treatment: quenched alloy material is subjected to ageing treatment in two hours, ageing treatment is general permanent It is carried out in warm resistance furnace, technique are as follows: 120 DEG C/26h.
Further, the coverture in the step 2 closes sodium aluminate by sodium chloride, potassium chloride and hexafluoro and constitutes, by matter Amount is than being sodium chloride: potassium chloride: hexafluoro closes sodium aluminate=4:4:2.
Further, when step 1 ingredient, the scaling loss amount of magnesium is supplemented, scaling loss amount is the 4.0% of gross mass.
Further, the smelting temperature of the step 2 is about 780 DEG C, and cast temperature is about 720 DEG C.
Alloying component weight percent (unit wt%) in each embodiment of table 1.:
By standard GB/T/6497-14 regulations, slab sampling is along plate thickness direction from surface to middle heart septum 5 plate with a thickness of 2.5mm is uniformly taken, the tensile sample to (L-T) and long laterally (T-L), then vertical plate thickness are rolled in processing Degree direction takes the plate of 2.5 mm thickness, processes tensile sample of the hyphen to (S-L), draftability is carried out on almighty test machine It can test.
2. embodiment of table and base alloy fracture toughness (K1C) test table:
As can be seen from Table 2 with the difference of alloying ingredient Ingredients Weight in embodiment 1,2,3, the fracture shown Toughness difference, the processing in above-mentioned 3 embodiment, which is rolled, to be all larger than to (L-T) fracture toughness equal to 42MPam1/2, long lateral (T-L) fracture toughness is all larger than equal to 35MPam1/2, hyphen is all larger than 27MPam to the fracture toughness of (S-L)1/2, respectively The fracture toughness that aspect is shown is superior to base alloy Fracture Toughness.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.

Claims (5)

1. a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy manufacturing methods, which is characterized in that
The alloy described by weight percentage is composed of the following components:
Zinc 5.4-6.5%, magnesium 1.7-2.7%, copper 1.5-2.5%, zirconium 0.07-0.15%, cerium 0.05-0.18%, titanium 0.08-0.16%, Other content of impurities are no more than 0.1 %, and single impurity component content is no more than 0.05%, remaining is Al；
Alloy preparation technology includes following below scheme: ingredient, melting casting, Homogenization Treatments, hot rolling, cold rolling, double_stage guide processing, Quenching, ageing treatment, specific steps are as follows:
1) ingredient: raw materials are as follows: rafifinal contains 99.95% aluminium, and pure magnesium contains 99.99% magnesium, aluminium Copper intermediate alloy, aluminium-copper content accounting 50%, content of impurities is lower than 0.12%, aluminium cerium intermediate alloy, aluminium-cerium content Accounting 10%, aluminium zirconium hardener, aluminium-zirconium content accounting 3%；
2) melting is cast: clay graphite paint is applied with graphite crucible or high-purity magnesium oxide brick and does hearth inner lining material molten alloy, Fusion process adds always coverture, charging sequence are as follows: industrial rafifinal -- aluminum bronze intermediate alloy -- aluminium zirconium hardener -- aluminium cerium Intermediate alloy is cast until completely melted, after carrying out first time outlet with carbon trichloride or argon gas, adds technical pure Magnesium carries out second of outlet with carbon trichloride or argon gas after being completely melt；
3) Homogenization Treatments: the ingot casting that step 2 is produced carries out Homogenization Treatments, specific work in salt bath furnace or argon gas protection stove Skill are as follows: will first be doomed 420 DEG C heat preservation 14-16 hours, then be heated to 465 DEG C of heat preservations 15-16 hours；
4) anneal before hot rolling preheating, cold rolling: concrete operations can carry out in air resistance furnace, wherein hot rolling preheating temperature is 430 DEG C ~ 440 DEG C heat preservation 3-4 hours, before cold rolling annealing temperature be 420 DEG C ~ 430 DEG C heat preservation 2-3 hours；
5) solution treatment: concrete operations carry out in salt bath furnace or argon gas protection stove, and double_stage guide treatment process is 280 DEG C/2h+ 475 DEG C/1h, and in room temperature quenching-in water；
6) ageing treatment: quenched alloy material is subjected to ageing treatment in two hours, ageing treatment is in general constant temperature electricity It is carried out in resistance furnace, technique are as follows: 120 DEG C/20 ~ 26h.
2. a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy manufacturing methods according to claim 1, feature exist In the impurity is one or more of iron, silicon, manganese, ytterbium.
3. a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy manufacturing methods according to claim 1, feature exist In it is sodium chloride: chlorine that the coverture in the step 2 closes sodium aluminate by sodium chloride, potassium chloride and hexafluoro and constitutes in mass ratio Change potassium: hexafluoro closes sodium aluminate=4:4:2.
4. a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy manufacturing methods according to claim 3, feature exist When, step 1 ingredient, the scaling loss amount of magnesium is supplemented, scaling loss amount is the 2.0-4.0% of gross mass.
5. a kind of high-performance Al-Zn-Mg-Cu-Zr-Ce-Ti alloy manufacturing methods according to claim 3, feature exist In the smelting temperature of the step 2 is 760 ~ 780 DEG C, and cast temperature is 690 ~ 720 DEG C.
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