CN107447140B - A kind of high strength alumin ium alloy and preparation method thereof haveing excellent performance - Google Patents

A kind of high strength alumin ium alloy and preparation method thereof haveing excellent performance Download PDF

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CN107447140B
CN107447140B CN201710615086.2A CN201710615086A CN107447140B CN 107447140 B CN107447140 B CN 107447140B CN 201710615086 A CN201710615086 A CN 201710615086A CN 107447140 B CN107447140 B CN 107447140B
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CN107447140A (en
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庞兴志
杨剑冰
湛永钟
胡治流
李逸泰
许征兵
赵艳君
杨文超
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Guangxi University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/10Alloys based on aluminium with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making 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 alloys
    • C22C1/02Making alloys by melting
    • C22C1/03Making alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/053Changing 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

The invention discloses a kind of high strength alumin ium alloys and preparation method thereof haveing excellent performance, Ho and Zr element is added simultaneously toward Al-Zn-Mg-Cu high strength aluminum alloy, pass through the processing steps such as the processing of ingredient, melting, casting and homogenizing annealing and solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance, its chemical component forms by weight percentage: 6%Zn, 2.5%Mg, 1.6%Cu, 0.5%Ho, 0.1~0.3%Zr, remaining is Al.Since the catharsis of Ho is combined with the Grain refinement of Zr, Al-Zn-Mg-Cu alloy tissue is set to obtain significant refinement, and impurity is reduced, crystal boundary is purified;After homogenizing annealing processing and solution treatment, the tensile strength of alloy is effectively improved, alloy comprehensive mechanical property is significantly improved.

Description

A kind of high strength alumin ium alloy and preparation method thereof haveing excellent performance
Technical field
The present invention relates to metallic composite preparation technical field, in particular to a kind of high strength alumin ium alloy haveing excellent performance and Preparation method.
Background technique
Al-Zn-Mg-Cu high strength aluminum alloy is due to easily molded processing and with high specific strength, excellent physics and change Performance is learned, and is widely used in aircraft, in naval vessel naval vessels.But with Aeronautics and Astronautics, the fast development of sea-freight, people couple More stringent requirements are proposed for Al-Zn-Mg-Cu high strength aluminum alloy, and therefore, acquisition high specific strength, high specific stiffness, high fracture are tough Property, low crack growth rate, it is antifatigue, corrosion-resistant and inexpensive the advantages that Al-Zn-Mg-Cu system ultra-high-strength aluminum alloy have become For one of the hot spot of countries in the world developing material.It can by the way that microelement is added into Al-Zn-Mg-Cu high strength aluminum alloy The performance of material is improved to a certain extent, but by rare earth Ho and Zr are added jointly research, its performance does not see report both at home and abroad Road.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of Al-Zn-Mg-Cu-Ho- haveing excellent performance Zr high strength alumin ium alloy.
The technical solution of the present invention is as follows: a kind of high strength alumin ium alloy haveing excellent performance, the high strength alumin ium alloy is Al-Zn-Mg- Cu-Ho-Zr alloy, the alloy composition form by weight percentage: 6%Zn, 2.5%Mg, 1.6%Cu, 0.5%Ho, 0.1~ 0.3%Zr, remaining is Al.
A kind of preparation method for the high strength alumin ium alloy haveing excellent performance, comprising the following steps:
(1) with commercial-purity aluminium (99.99%), pure zinc (99.99%), pure magnesium (99.99%), fine copper (99.99%), Al-10%Ho Intermediate alloy and Al-10%Zr intermediate alloy are raw material, and above-mentioned raw materials are cut into small pieces respectively using cutting machine, and is beaten with sand paper Mill with partial impurities such as the oxidation film, the greasy dirts that remove raw material surface, and preheats at 150~200 DEG C, removal raw material surface Water;
(2) preheated technical pure aluminium block is placed in graphite-clay crucible first and be put into crucible open type resistance furnace, adjusted Section furnace temperature is increased to 770~780 DEG C, after the fusing of technical pure aluminium block adjusting furnace temperature to 750~760 DEG C when fine copper block is added, and It is stirred with stirring rod, stands 15~20min;When adjusting furnace temperature is to 730 DEG C~740 DEG C, Al-10%Zr intermediate alloy is added, It stirs and stands 10~15min;It is subsequently added into the stirring of Al-10%Ho intermediate alloy, blow-on is skimmed after standing 10~15min, is added Pure spelter stands 10~15min;It is eventually adding pure MAG block, stirring is opened after standing 10~15min after pure MAG block fuses into molten aluminum Furnace is skimmed, and refining agent 15g is added later and refines degasification, stands 15~20min after mixing evenly, and blow-on checks whether liquid level has furnace The impurity such as slag after taking off clean liquid level, control furnace temperature at 720 DEG C~730 DEG C;
(3) it will pour and cast from 200~220 DEG C of preheated metal grinding tools through the melted alloy liquid of step (2), it is cooling Demoulding, is prepared into Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot;
(4) Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot is placed in chamber type electric resistance furnace, first carries out homogenizing annealing processing With rear carry out solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance.
Further, every when a kind of alloy raw material is added carrying out melting, 15g, which is uniformly all sprinkled, on the alloy molten solution surface covers Lid agent, the coverture are NaCl:KCl=1:1.
Further, the refining agent in the step (2) is C2Cl6
Further, the temperature of the Homogenization Treatments in the step (4) be 460 DEG C, soaking time be for 24 hours, furnace temperature Control errors are come out of the stove air-cooled at ± 2 DEG C when furnace temperature is reduced to 300 DEG C after keeping the temperature;The furnace temperature of the solution treatment is 470 DEG C, 1h is kept the temperature, the control errors of furnace temperature take out Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot at ± 2 DEG C, after soaking time and use Room temperature water quenching, quenching shift time are less than 5s.
The beneficial effects of the present invention are: after adding Ho, Zr simultaneously to Al-Zn-Mg-Cu alloy, due to the catharsis of Ho It is combined with the Grain refinement of Zr, alloy structure obtains significant refinement, and impurity is reduced, and crystal boundary is purified;Through uniform After annealing processing and solution treatment, the tensile strength of alloy is effectively improved, alloy comprehensive mechanical property is significantly improved.
Detailed description of the invention
Fig. 1 is the Al-Zn-Mg-Cu alloy micro-organization chart of different content Ho and Zr.
Fig. 2 is the Al-Zn-Mg-Cu-Ho-Zr alloy surface shape appearance figure of as cast condition and solid solution state in embodiment 2.
Fig. 3 is influence of the different content Ho and Zr to Al-Zn-Mg-Cu alloy tensile strength.
Appended drawing reference: A, Al-Zn-Mg-Cu alloy, B, Al-Zn-Mg-Cu-0.5%Ho alloy, C, Al-Zn-Mg-Cu- 0.5%Ho-0.2%Zr, a- as cast condition, b- are dissolved state.
Specific embodiment
Embodiment 1
A kind of preparation method for the high strength alumin ium alloy haveing excellent performance, comprising the following steps:
1. with commercial-purity aluminium (99.99%), pure zinc (99.99%), pure magnesium (99.99%), fine copper (99.99%), Al-10%Ho Intermediate alloy and Al-10%Zr intermediate alloy are raw material, and Al-6%Zn-2.5%Mg-1.6%Cu by weight percentage is prepared, rare earth Ho It is 0.5% that content, which is added, is separately added into 0.1%Zr on the basis of 0.5%Ho, is cut into above-mentioned raw materials respectively using cutting machine small Block, and being polished with sand paper with partial impurities such as the oxidation film, the greasy dirts that remove raw material surface, and is preheated at 150~200 DEG C, is gone Except the water on raw material surface;
2. preheated technical pure aluminium block is placed in graphite-clay crucible first and is put into crucible open type resistance furnace, adjust Furnace temperature is increased to 770~780 DEG C, after the fusing of technical pure aluminium block adjusting furnace temperature to 750~760 DEG C when fine copper block is added, be used in combination Stirring rod is stirred, and stands 15~20min;When adjusting furnace temperature is to 730 DEG C~740 DEG C, Al-10%Zr intermediate alloy is added, stirs It mixes and stands 10~15min;It is subsequently added into the stirring of Al-10%Ho intermediate alloy, blow-on is skimmed after standing 10~15min, is added pure Spelter stands 10~15min;It is eventually adding pure MAG block, stirring stands blow-on after 10~15min after pure MAG block fuses into molten aluminum It skims, refining agent (C is added later2Cl6) 15g refining degasification, 15~20min is stood after mixing evenly, and whether blow-on checks liquid level There are the impurity such as clinker, after taking off clean liquid level, controls furnace temperature at 720 DEG C~730 DEG C;It is every above a kind of alloy raw material is added to be melted When refining, 15g coverture is uniformly all sprinkled on the alloy molten solution surface, the coverture is NaCl:KCl=1:1;
3. it is cast from being poured through the melted alloy liquid of step 2 in 200~220 DEG C of preheated metal grinding tools, it is cooling de- Mould is prepared into Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot;
4. Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot is placed in chamber type electric resistance furnace, homogenizing annealing processing is first carried out With rear carry out solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance;Wherein, Homogenization Treatments Temperature is 460 DEG C, and soaking time is for 24 hours that the control errors of furnace temperature are at ± 2 DEG C, when furnace temperature is reduced to 300 DEG C after keeping the temperature It comes out of the stove air-cooled;The furnace temperature of the solution treatment is 470 DEG C, keeps the temperature 1h, at ± 2 DEG C, soaking time terminates the control errors of furnace temperature Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot room temperature water quenching is taken out afterwards, and quenching shift time is less than 5s.
Embodiment 2
A kind of preparation method for the high strength alumin ium alloy haveing excellent performance, comprising the following steps:
1. with commercial-purity aluminium (99.99%), pure zinc (99.99%), pure magnesium (99.99%), fine copper (99.99%), Al-10%Ho Intermediate alloy and Al-10%Zr intermediate alloy are raw material, and Al-6%Zn-2.5%Mg-1.6%Cu by weight percentage is prepared, rare earth Ho It is 0.5% that content, which is added, is separately added into 0.2%Zr on the basis of 0.5%Ho, is cut into above-mentioned raw materials respectively using cutting machine small Block, and being polished with sand paper with partial impurities such as the oxidation film, the greasy dirts that remove raw material surface, and is preheated at 150~200 DEG C, is gone Except the water on raw material surface;
2. preheated technical pure aluminium block is placed in graphite-clay crucible first and is put into crucible open type resistance furnace, adjust Furnace temperature is increased to 770~780 DEG C, after the fusing of technical pure aluminium block adjusting furnace temperature to 750~760 DEG C when fine copper block is added, be used in combination Stirring rod is stirred, and stands 15~20min;When adjusting furnace temperature is to 730 DEG C~740 DEG C, Al-10%Zr intermediate alloy is added, stirs It mixes and stands 10~15min;It is subsequently added into the stirring of Al-10%Ho intermediate alloy, blow-on is skimmed after standing 10~15min, is added pure Spelter stands 10~15min;It is eventually adding pure MAG block, stirring stands blow-on after 10~15min after pure MAG block fuses into molten aluminum It skims, refining agent (C is added later2Cl6) 15g refining degasification, 15~20min is stood after mixing evenly, and whether blow-on checks liquid level There are the impurity such as clinker, after taking off clean liquid level, controls furnace temperature at 720 DEG C~730 DEG C;It is every above a kind of alloy raw material is added to be melted When refining, 15g coverture is uniformly all sprinkled on the alloy molten solution surface, the coverture is NaCl:KCl=1:1;
3. it is cast from being poured through the melted alloy liquid of step 2 in 200~220 DEG C of preheated metal grinding tools, it is cooling de- Mould is prepared into Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot;
4. Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot is placed in chamber type electric resistance furnace, homogenizing annealing processing is first carried out With rear carry out solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance;Wherein, Homogenization Treatments Temperature is 460 DEG C, and soaking time is for 24 hours that the control errors of furnace temperature are at ± 2 DEG C, when furnace temperature is reduced to 300 DEG C after keeping the temperature It comes out of the stove air-cooled;The furnace temperature of the solution treatment is 470 DEG C, keeps the temperature 1h, at ± 2 DEG C, soaking time terminates the control errors of furnace temperature Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot room temperature water quenching is taken out afterwards, and quenching shift time is less than 5s.
Embodiment 3
A kind of preparation method for the high strength alumin ium alloy haveing excellent performance, comprising the following steps:
1. with commercial-purity aluminium (99.99%), pure zinc (99.99%), pure magnesium (99.99%), fine copper (99.99%), Al-10%Ho Intermediate alloy and Al-10%Zr intermediate alloy are raw material, and Al-6%Zn-2.5%Mg-1.6%Cu by weight percentage is prepared, rare earth Ho It is 0.5% that content, which is added, is separately added into 0.3%Zr on the basis of 0.5%Ho, is cut into above-mentioned raw materials respectively using cutting machine small Block, and being polished with sand paper with partial impurities such as the oxidation film, the greasy dirts that remove raw material surface, and is preheated at 150~200 DEG C, is gone Except the water on raw material surface;
2. preheated technical pure aluminium block is placed in graphite-clay crucible first and is put into crucible open type resistance furnace, adjust Furnace temperature is increased to 770~780 DEG C, after the fusing of technical pure aluminium block adjusting furnace temperature to 750~760 DEG C when fine copper block is added, be used in combination Stirring rod is stirred, and stands 15~20min;When adjusting furnace temperature is to 730 DEG C~740 DEG C, Al-10%Zr intermediate alloy is added, stirs It mixes and stands 10~15min;It is subsequently added into the stirring of Al-10%Ho intermediate alloy, blow-on is skimmed after standing 10~15min, is added pure Spelter stands 10~15min;It is eventually adding pure MAG block, stirring stands blow-on after 10~15min after pure MAG block fuses into molten aluminum It skims, refining agent (C is added later2Cl6) 15g refining degasification, 15~20min is stood after mixing evenly, and whether blow-on checks liquid level There are the impurity such as clinker, after taking off clean liquid level, controls furnace temperature at 720 DEG C~730 DEG C;It is every above a kind of alloy raw material is added to be melted When refining, 15g coverture is uniformly all sprinkled on the alloy molten solution surface, the coverture is NaCl:KCl=1:1;
3. it is cast from being poured through the melted alloy liquid of step 2 in 200~220 DEG C of preheated metal grinding tools, it is cooling de- Mould is prepared into Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot;
4. Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot is placed in chamber type electric resistance furnace, homogenizing annealing processing is first carried out With rear carry out solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance;Wherein, Homogenization Treatments Temperature is 460 DEG C, and soaking time is for 24 hours that the control errors of furnace temperature are at ± 2 DEG C, when furnace temperature is reduced to 300 DEG C after keeping the temperature It comes out of the stove air-cooled;The furnace temperature of the solution treatment is 470 DEG C, keeps the temperature 1h, at ± 2 DEG C, soaking time terminates the control errors of furnace temperature Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot room temperature water quenching is taken out afterwards, and quenching shift time is less than 5s.
Beneficial effect in order to further illustrate the present invention prepares control group A l-Zn-Mg-Cu alloy and Al-Zn- respectively Mg-Cu-Ho alloy;Using the grain size and pattern of alloy lower after metallography microscope sem observation as cast condition and solution treatment, use Model Phenom ProX scanning electron microscopic observation tissue and fracture surface of sample pattern, using Instron8801 universal material testing The tensile strength of machine measurement alloy.
As shown in Figure 1, the Al-Zn-Mg-Cu alloy tissue crystal grain for not adding rare earth Ho and Zr is largely column crystal Grain, and it is coarseer to be present in the cocrystalization compound between crystal grain and crystal boundary.And after being added to 0.5% rare earth Ho, Crystal grain in Al-Zn-Mg-Cu-Ho alloy has obtained certain refinement, and the cocrystalization compound being present between crystal boundary and crystal grain is thin Change particularly evident, crystal boundary is completely clear;On the basis of 0.5% rare earth Ho is added, it is added to the Al-Zn-Mg- of 0.2%Zr element Cu-Ho-Zr alloy (embodiment 2) tissue crystal grain more refines, and the pattern of crystal grain more levels off to spherical shape.
As shown in Fig. 2, a part of Solid Solution of Second Phase Particles is in matrix, and another part is due to adding after solution treatment The Microalloying Effect for having entered rare earth Ho and Zr combines with Al, Cu, Zn etc. around crystal boundary and forms the phase that can be dissolved in matrix, So that the second phase oversize grain that part concentrates on crystal boundary has dissolved in matrix again, reduce the crystalline substance of Al-Zn-Mg-Cu alloy Boundary's segregation, improves tissue, optimizes performance.
As shown in figure 3, the tensile strength of alloy obtains after addition rare earth Ho for as cast condition Al-Zn-Mg-Cu alloy It is promoted.Meanwhile in the case where rare earth Ho content is constant, with the increase of Zr content, curve is in downward trend after first rising, When content is 0.2%Zr, tensile strength reaches maximum value (328MPa).This illustrates that Al-Zn-Mg-Cu alloy is moved back by homogenization After fire processing and solution treatment, the solute element in alloy has dissolved in matrix, meanwhile, the second phase particles of part segregation also incorporate Matrix makes matrix generate distortion of lattice, hinders dislocation motion, thus improve the intensity of alloy, and the addition of Ho and Zr The non-spontaneous nucleation of formation plays the role of refining crystal grain.When Ho content is constant, with the increase of Zr content, refinement is brilliant The effect of grain and solution strengthening is improved, so that the tensile strength of Al-Zn-Mg-Cu alloy be made more to be significantly improved.

Claims (2)

1. a kind of preparation method for the high strength alumin ium alloy haveing excellent performance, it is characterised in that: the high strength alumin ium alloy is Al-Zn-Mg- Cu-Ho-Zr alloy, the alloy composition form by weight percentage: 6%Zn, 2.5%Mg, 1.6%Cu, 0.5%Ho, 0.1~ 0.3%Zr, remaining is Al;
Preparation method, comprising the following steps:
(1) using commercial-purity aluminium, pure zinc, pure magnesium, fine copper, Al-10%Ho intermediate alloy and Al-10%Zr intermediate alloy as raw material, benefit Above-mentioned raw materials are cut into small pieces respectively with cutting machine, and are polished with sand paper, it is miscellaneous with the oxidation film, the greasy dirt part that remove raw material surface Matter, and preheated at 150~200 DEG C, remove the water on raw material surface;
(2) preheated technical pure aluminium block is placed in graphite-clay crucible first and be put into crucible open type resistance furnace, regulating stove Up to 770~780 DEG C of temperature rise, after the fusing of technical pure aluminium block adjusting furnace temperature to 750~760 DEG C when be added fine copper block, and with stirring It mixes stick to be stirred, stands 15~20min;When adjusting furnace temperature is to 730 DEG C~740 DEG C, Al-10%Zr intermediate alloy, stirring is added And stand 10~15min;It is subsequently added into the stirring of Al-10%Ho intermediate alloy, blow-on is skimmed after standing 10~15min, and pure zinc is added Block stands 10~15min;It is eventually adding pure MAG block, blow-on is taken off after stirring stands 10~15min after pure MAG block fuses into molten aluminum Refining agent 15g is added later and refines degasification, stands 15~20min after mixing evenly for slag, and blow-on checks whether liquid level has clinker miscellaneous Matter after taking off clean liquid level, controls furnace temperature at 720 DEG C~730 DEG C;
(3) it will pour and cast from 200~220 DEG C of preheated metal grinding tools through the melted alloy liquid of step (2), it is cooling de- Mould is prepared into Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot;
(4) Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot is placed in chamber type electric resistance furnace, first carries out homogenizing annealing processing with after Carry out solution treatment, the high strength alumin ium alloy that obtained Al-Zn-Mg-Cu-Ho-Zr is had excellent performance;
Above-mentioned steps are every when a kind of alloy raw material is added carrying out melting, all uniformly sprinkle 15g coverture on the alloy molten solution surface, The coverture is NaCl:KCl=1:1;
The temperature of Homogenization Treatments in the step (4) is 460 DEG C, and soaking time is for 24 hours that the control errors of furnace temperature are ± 2 DEG C, it comes out of the stove when furnace temperature is reduced to 300 DEG C after keeping the temperature air-cooled;The temperature of the solution treatment is 470 DEG C, keeps the temperature 1h, furnace The control errors of temperature take out Al-Zn-Mg-Cu-Ho-Zr alloy cast ingot room temperature water quenching at ± 2 DEG C after soaking time, Quenching shift time is less than 5s.
2. the preparation method for the high strength alumin ium alloy haveing excellent performance according to claim 1, it is characterised in that: the step (2) In refining agent be C2Cl6
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