WO2017215104A1 - 一种超高强度非快速凝固铝合金及其制备方法 - Google Patents

一种超高强度非快速凝固铝合金及其制备方法 Download PDF

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WO2017215104A1
WO2017215104A1 PCT/CN2016/094819 CN2016094819W WO2017215104A1 WO 2017215104 A1 WO2017215104 A1 WO 2017215104A1 CN 2016094819 W CN2016094819 W CN 2016094819W WO 2017215104 A1 WO2017215104 A1 WO 2017215104A1
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aluminum alloy
alloy
mass percentage
strength non
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许晓静
朱金鑫
丁清
吴瑶
孙良省
谈成
张香丽
赵建吉
杨帆
杜东辉
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Jiangsu 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 non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous 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 non-ferrous alloys
    • C22C1/02—Making non-ferrous 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
    • 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

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  • the invention belongs to the field of metal alloys, in particular to a 770MPa grade ultra high strength non-rapid solidified aluminum alloy and a preparation method thereof.
  • Aluminum alloy is a typical lightweight material with low density, high strength, good toughness, corrosion resistance, easy processing, easy recycling, low manufacturing cost, strong foundational industrial strength, good military-civilian integration, etc. Or the leap-forward improvement of a certain important single item performance has played a very strong supporting role for the development of advanced equipment in different periods. For a long time, the development of aluminum alloy with higher strength level and more balanced performance has been a very important research topic. It is related to a country's aerospace, weaponry, general industry, resource conservation, environmental protection and many other fields. The level of development has always been one of the most competitive areas of science and technology in the world.
  • Chinese patent CN101338391 discloses a rapid solidification block aluminum alloy with high strength and high ductility and a preparation method thereof, but the rapid solidification block aluminum alloy has high strength, but the preparation process is spray forming rapid solidification technology, and the cost is high. And this technology can only prepare millimeter-scale bulk aluminum alloy, which can hardly be applied to actual production.
  • Chinese patent CN102127665 discloses an Al-Zn-Mg-Cu-Sc-Zr-RE alloy which can be used as an ultra-high-strength cast aluminum alloy and a preparation method thereof, wherein RE is a rare metal element such as Er or Yb.
  • RE is a rare metal element such as Er or Yb.
  • the elements are rare earth metal elements, the price is relatively expensive, and the raw material cost is high.
  • the maximum tensile strength of the aluminum alloy prepared by this method can reach 605 MPa, and there is no substantial breakthrough compared with the international advanced level.
  • Chinese patent CN103993211 discloses a 720-750MPa ultra-high strength non-rapid solidified aluminum alloy and a preparation method thereof.
  • the strength of the aluminum alloy can reach 720-750 MPa, but the patent only gives the composition of the alloy, and the content of the main alloy element
  • the relationship between the two is not limited, and has certain limitations, and the alloy needs to be subjected to melt casting-homogenization annealing-hot extrusion-pre-reduction annealing-solution treatment-pre-deformation-aging treatment.
  • the process is relatively cumbersome, which is not conducive to industrial production, and some of these processes still have room for optimization.
  • the object of the present invention is to design a 770 MPa ultra-high strength non-rapid solidified aluminum alloy and a preparation method thereof by component design and preparation technology design.
  • a 770 MPa ultra-high strength non-rapid solidified aluminum alloy characterized by: aluminum alloy (Al), zinc (Zn), magnesium (Mg), copper (Cu), zirconium (Zr) and strontium (Sr)
  • Al aluminum alloy
  • Zn zinc
  • Mg magnesium
  • Cu copper
  • Zr zirconium
  • strontium strontium
  • the composition wherein the mass percentage of zinc (Zn) is 8.8 to 9.4%, the mass percentage of magnesium (Mg) is 2.75 to 2.85%, the mass percentage of copper (Cu) is 1.8 to 2.2%, and the mass of zirconium (Zr) The percentage is 0.25 to 0.55%, the mass percentage of strontium (Sr) is 0 to 0.025%, and the balance is aluminum, and only the ratio of the mass percentage of Zn and Mg in the alloying element is satisfied to satisfy 3 ⁇ Wt Zn / Wt Mg ⁇ 4, Wt Mg Mg percentage of quality to meet the 2% ⁇ Wt Mg ⁇
  • the invention discloses a preparation method of 770MPa grade ultra high strength non-rapid solidified aluminum alloy, which is characterized in that it comprises: melting casting - homogenization annealing - hot extrusion - solution treatment - aging treatment.
  • the casting is based on the composition design, weighing each raw material, wherein Cu, Zr, Sr three elements are added using Al-Cu, Al-Zr, Al-Sr intermediate alloy, Al, Zn, Mg are used Elemental, the specific order of smelting is to first weigh the well-prepared Al, Zn, Al-Cu, Al-Zr, Al-Sr in a melting furnace, the melting temperature is 900 ° C, after the five raw materials are melted with titanium The alloy rod is evenly stirred, allowed to stand for 3 min, and then de-evaporated by adding hexachloroethane and argon until no gas escapes.
  • the furnace temperature is lowered to 800 ° C, and then Mg is added.
  • Mg should be wrapped in aluminum foil.
  • press the titanium alloy container into the bottom of the liquid alloy let stand for 5 minutes, stir with titanium rod, then add hexachloroethane and argon. Refined degassing until no gas escapes, then raise the furnace temperature to 850 ° C, keep warm for 10 min, and finally cast into ingots.
  • the homogenization annealing is characterized in that the annealing mechanism is 420 ° C ⁇ 6 h + 440 ° C ⁇ 6 h + 460 ° C ⁇ 6 h + 465 ° C ⁇ 12 h, and the annealing end temperature is higher, so that the composition inside the alloy is more uniform.
  • the hot extrusion is characterized in that the process is to heat the alloy after homogenization annealing to 480 ° C and hold for 8 hours, and then perform extrusion with a compression ratio of 10:1, and the moderate extrusion ratio can be reduced.
  • the generation of internal defects in the alloy is characterized in that the process is to heat the alloy after homogenization annealing to 480 ° C and hold for 8 hours, and then perform extrusion with a compression ratio of 10:1, and the moderate extrusion ratio can be reduced. The generation of internal defects in the alloy.
  • the solution treatment is characterized in that the solid solution mechanism is 450 ° C ⁇ 2 h + 460 ° C ⁇ 2 h + 470 ° C ⁇ 2 h after the room temperature water quenching, the water quenching transfer time does not exceed 10 s.
  • the aging treatment is characterized in that the process is T6 aging, and the aging mechanism is 121 ° C ⁇ 24 h.
  • An ultra-high strength non-rapid solidified aluminum alloy of 770 MPa grade can be obtained.
  • the present invention obtains a composition of a 770 MPa ultra-high strength non-rapidly solidified aluminum alloy and a preparation method thereof. Compared with the disclosed patent, the composition is clearly distinguished, and the composition interval is more precise, and the alloy is clearly given.
  • the relationship between the content of major alloying elements is more scientific and reasonable in process, especially smelting, homogenization annealing and hot extrusion Process, more scientific component design and process optimization together improve the strength of the aluminum alloy. Moreover, the process is obviously simplified as a whole, laying the foundation for industrialization.
  • each raw material is weighed, wherein Cu, Zr and Sr are added by using Al-Cu, Al-Zr and Al-Sr intermediate alloys, and Al, Zn and Mg are used as simple substances.
  • the specific sequence of smelting is to first weigh the well-prepared Al, Zn, Al-Cu, Al-Zr, Al-Sr in a melting furnace, and the melting temperature is 900 ° C. After the five raw materials are melted, the titanium alloy rod is used. Stir well, let stand for 3min, then add hexachloroethane and argon to refine the gas until no gas escapes.
  • Hot extrusion The alloy after homogenization annealing was heated to 480 ° C and held for 8 hours, and then extruded at a compression ratio of 10:1 to obtain an extruded bar.
  • Solution treatment The solution bar obtained in the previous step is solution treated, and the solution mechanism is 450 ° C ⁇ 2 h + 460 ° C ⁇ 2 h + 470 ° C ⁇ 2 h after heat preservation at room temperature, the water quenching transfer time is not More than 10s.
  • the aluminum alloy was obtained, and the tensile strength of the alloy was measured to be 770.1 MPa and the elongation was 8.2%.

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  • Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

一种770Mpa级超高强度非快速凝固铝合金，其中锌为8.8~9.4wt%，镁为2.75~2.85wt%，铜为1.8~2.2 wt%，锆为0.25~0.55 wt%，锶为0~0.025 wt%，余量为铝，并且合金元素中Zn和Mg的质量百分数的比值应满足3≤WtZn／WtMg≤４，Mg的质量百分数WtMg应满足2%≤WtMg≤3%。该合金通过熔铸—均匀退火—热挤压—固溶处理—时效处理制备获得。

Description

一种超高强度非快速凝固铝合金及其制备方法 技术领域
本发明属于金属合金领域，尤其涉及一种770MPa级超高强度非快速凝固铝合金及其制备方法。
背景技术
铝合金是典型的轻量化材料，具有密度低、强度高、韧性好、耐腐蚀、易加工、易回收、制造成本低、可依托的基础工业实力强、军民融合性好等特点，其综合性能或某一重要单项性能的跨越式提升，对于不同时期先进装备的发展，起到了非常有力的支撑作用。长期以来，研制强度级别更高、综合性能更加平衡优化的铝合金一直是一个非常重要的研究课题，它关系到一个国家的航空航天、武器装备、通用产业、资源节约、环境保护等诸多领域的发展水平，一直是国际上竞争最激烈的科学技术领域之一。
20世纪90年代中期，发达国家采用喷射成形快速凝固技术成功地开发出了750MPa强度级超强铝合金，其典型合金为RSA7034(Al-11Zn-2.3Mg-1Cu)，走在了世界前列。但是，喷射成形快速凝固技术制备难以制备大型锭坯铝合金，并且价格高昂，限制了其应用。
中国专利CN101338391公布了一种具有高强度高延韧性快速凝固块体铝合金及其制备方法，但是这种快速凝固块体铝合金虽然强度高，但是制备工艺为喷射成形快速凝固技术，成本很高，且这种技术只能制备毫米级的块体铝合金，基本上无法应用到实际生产中。
中国专利CN102127665公布了一种可作为超高强铸造铝合金使用的Al-Zn-Mg-Cu-Sc-Zr-RE合金及其制备方法，其中RE为Er或者Yb这两种稀有金属元素，这两种元素为稀土金属元素，价格相对昂贵，原料成本较高，同时这种方法制备的铝合金最高抗拉强度能达到605MPa，与国际先进水平相比没有实质性突破。
中国专利CN103993211公开了一种720-750MPa超高强非快速凝固铝合金及其制备方法，这种铝合金的强度能够达到720-750MPa，但是专利只给出了合金的成分，对主合金元素含量之间的关系并没有进行限定，具有一定的局限性，而且这种合金需经过熔铸-均质化退火-热挤压-预回复退火-固溶处理-预变形-时效处理，处理工艺多达七道，工艺相对繁琐，不利于工业化生产，而且其中有些工艺还存在优化的空间。
到目前为止，尚未有一种具有自主知识产权的770MPa级超高强度非快速凝固铝合金及其制备方法可供使用，这一定程度上制约了我国航空航天、武器装备等工业的发展。
发明内容
本发明的目的是通过成分设计和制备技术设计，发明一种770MPa级超高强度非快速凝固铝合金及其制备方法。
本发明的技术方案是：
一种770MPa级超高强度非快速凝固铝合金，其特征在于：本铝合金主要由铝(Al)、锌(Zn)、镁(Mg)、铜(Cu)、锆(Zr)和锶(Sr)组成，其中，锌(Zn)的质量百分比为8.8～9.4％，镁(Mg)的质量百分比为2.75～2.85％，铜(Cu)的质量百分比为1.8～2.2％，锆(Zr)的质量百分比为0.25～0.55％，锶(Sr)的质量百分比为0～0.025％，余量为铝，并且只有保证合金元素中Zn和Mg的质量百分数的比值满足3≤WtZn/WtMg≤4，Mg的质量百分数WtMg满足2％≤WtMg≤3％，才能使得合金中的主要ZnMg强化相取得最大的强化效果。
一种770MPa级超高强度非快速凝固铝合金的制备方法，其特征是它依次包括：熔铸—均质化退火—热挤压—固溶处理—时效处理。
所述的熔铸：其过程为根据成分设计，称量各原料，其中Cu、Zr、Sr三种元素的加入使用Al-Cu、Al-Zr、Al-Sr中间合金，Al、Zn、Mg均使用单质，熔炼的具体顺序是先将称量好的Al、Zn、Al-Cu、Al-Zr、Al-Sr置于熔炼炉中熔炼，熔炼温度为900℃，待这五种原料熔化后用钛合金棒搅拌均匀，静置3min，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，为了减少Mg在熔炼时的烧损，将炉温降至800℃，再加入Mg，且Mg要用铝箔包裹，为了防止Mg密度低，漂浮在其他液体合金上，用钛合金容器一直压入液体合金底部，静置保温5min后用钛合金棒搅拌，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，再将炉温升至850℃，保温10min，最后浇铸成锭。
所述的均质化退火：其特征是退火机制为420℃×6h+440℃×6h+460℃×6h+465℃×12h，退火终端温度较高，能使得合金内部的成分更加均匀。
所述的热挤压：其特征是其工艺为将均质化退火后的合金加热至480℃并保温8h后进行挤压比为10：1的挤压，这种适中的挤压比能减少合金内部缺陷的产生。
所述的固溶处理：其特征是固溶机制为450℃×2h+460℃×2h+470℃×2h保温后室温水淬，水淬转移时间不超过10s。
所述的时效处理：其特征是其工艺为T6时效，时效机制为121℃×24h。
即可获得770MPa级超高强度非快速凝固铝合金。
本发明的有益效果：
(1)本发明获得了一种770MPa级超高强度非快速凝固铝合金的成分及其制备方法相比于已经公开的专利，成分上区别明显，且成分区间更加精确，并且明确给出了合金中主要合金元素含量之间的关系，工艺上更加科学合理，尤其是熔炼，均质化退火和热挤压 工艺，更加科学的成分设计和工艺的优化共同提高了铝合金的强度。而且从整体上看工艺明显简化，为产业化打下基础。
(2)本发明获得的770MPa级超高强度非快速凝固铝合金的成分及其制备方法，合金强度高，同时延伸率仍能保持在7％以上，与现有的喷射成形快速凝固技术只能制造毫米级的块状铝合金相比，本技术能够生产制造更大的高强铝合金制品，更具有使用价值。
具体实施方式
下面结合具体实施例对本发明作进一步的说明。
实施例一
制备770MPa级超高强度非快速凝固铝合金Al-9.01Zn-2.79Mg-2.14Cu-0.52Zr-0.025Sr，WtZn/WtMg＝3.23，且WtMg＝2.79％，满足3≤WtZn/WtMg≤4，2％≤WtMg≤3％，其制备工艺如下：
(1)熔铸：根据上述成分设计，称量各原料，其中Cu、Zr、Sr三种元素的加入使用Al-Cu、Al-Zr、Al-Sr中间合金，Al、Zn、Mg均使用单质，熔炼的具体顺序是先将称量好的Al、Zn、Al-Cu、Al-Zr、Al-Sr置于熔炼炉中熔炼，熔炼温度为900℃，待这五种原料熔化后用钛合金棒搅拌均匀，静置3min，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，为了减少Mg在熔炼时的烧损，将炉温降至800℃，再加入Mg，且Mg要用铝箔包裹，为了防止Mg密度低，漂浮在其他液体合金上，用钛合金容器一直压入液体合金底部，静置保温5min后用钛合金棒搅拌，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，再将炉温升至850℃，保温10min，最后浇铸成锭。
(2)均质化退火：将上一步获得的铸锭进行均质化退火，退火机制为420℃×6h+440℃×6h+460℃×6h+465℃×12h。
(3)热挤压：将均质化退火后的合金加热至480℃并保温8h后进行挤压比为10：1的挤压，得到挤压棒材。
(4)固溶处理：将上一步获得的挤压棒材进行固溶处理，固溶机制为450℃×2h+460℃×2h+470℃×2h保温后室温水淬，水淬转移时间不超过10s。
(5)时效处理：将上一步得到的固溶处理后的棒材进行T6时效处理，时效机制为121℃×24h。
经过上述步骤即获得所述的铝合金，经过强度拉伸实验，测得本合金抗拉强度为770.1MPa，延伸率为8.2％。
实施例二
制备770MPa级超高强度非快速凝固铝合金Al-9.34Zn-2.84Mg-2.17Cu-0.29Zr-0.025 Sr，WtZn/WtMg＝3.29，且WtMg＝2.84％，满足3≤WtZn/WtMg≤4，2％≤WtMg≤3％，其制备工艺与实施例一相同，本实施例获得的铝合金，经过强度拉伸实验，测得最高抗拉强度为780.8MPa，延伸率为7％。
实施例三
制备770MPa级超高强度非快速凝固铝合金Al-8.89Zn-2.82Mg-1.85Cu-0.31Zr-0.025Sr，WtZn/WtMg＝3.15，且WtMg＝2.82％，满足3≤WtZn/WtMg≤4，2％≤WtMg≤3％，其制备工艺与实施例一相同，本实施例获得的铝合金，经过强度拉伸实验，测得抗拉强度为776.4MPa，延伸率为7.8％。
本领域的技术人员可以根据上述实例适当地调整各组份的配比并严格按上述步骤进行制造即可获得理想的770MPa级超高强度非快速凝固铝合金及其制备方法。
本发明未涉及部分均与现有技术相同或可采用现有技术加以实现。

Claims (4)

  1. 一种超高强度非快速凝固铝合金，所述铝合金的抗拉强度不低于770Mpa，同时延伸率仍能保持在7％以上，所述铝合金的成分由铝(Al)、锌(Zn)、镁(Mg)、铜(Cu)、锆(Zr)和锶(Sr)组成，其特征在于：锌(Zn)的质量百分比为8.8～9.4％，镁(Mg)的质量百分比为2.75～2.85％，铜(Cu)的质量百分比为1.8～2.2％，锆(Zr)的质量百分比为0.25～0.55％，锶(Sr)的质量百分比为0～0.025％，余量为铝，并且合金元素中Zn和Mg的质量百分数的比值应满足3≤WtZn/WtMg≤4，Mg的质量百分数WtMg应满足2％≤WtMg≤3％。
  2. 如权利要求1所述的一种超高强度非快速凝固铝合金的制备方法，步骤依次包括：熔铸—均质化退火—热挤压—固溶处理—时效处理，其特征是，
    所述的熔铸，其过程为：根据成分设计，称量各原料，其中Cu、Zr、Sr三种元素的加入使用Al-Cu、Al-Zr、Al-Sr中间合金，Al、Zn、Mg均使用单质，熔炼的具体顺序是先将称量好的Al、Zn、Al-Cu、Al-Zr、Al-Sr置于熔炼炉中熔炼，熔炼温度为900℃，待这五种原料熔化后用钛合金棒搅拌均匀，静置3min，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，为了减少Mg在熔炼时的烧损，将炉温降至800℃，再加入Mg，且Mg要用铝箔包裹，为了防止Mg密度低，漂浮在其他液体合金上，用钛合金容器将Mg一直压入液体合金底部，静置保温5min后用钛合金棒搅拌，再加入六氯乙烷和氩气精炼除气直至没有气体逸出，再将炉温升至850℃，保温10min，最后浇铸成锭；
    所述的均质化退火：退火机制为420℃×6h+440℃×6h+460℃×6h+465℃×12h；
    所述的热挤压，其工艺为：将均质化退火后的合金加热至480℃并保温8h后进行挤压比为10：1的挤压。
  3. 如权利要求2所述的一种超高强度非快速凝固铝合金的制备方法，其特征是：所述的固溶处理，固溶机制为450℃×2h+460℃×2h+470℃×2h保温后室温水淬，水淬转移时间不超过10s。
  4. 如权利要求2所述的一种超高强度非快速凝固铝合金的制备方法，其特征是：所述的时效处理，其特征是其工艺为T6时效，时效机制为121℃×24h；
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