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WO2013012352A1 - Alliages d'aluminium à très petits grains pour articles électrotechniques et procédés de fabrication correspondants (et variantes) - Google Patents

Alliages d'aluminium à très petits grains pour articles électrotechniques et procédés de fabrication correspondants (et variantes) Download PDF

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Publication number
WO2013012352A1
WO2013012352A1 PCT/RU2012/000005 RU2012000005W WO2013012352A1 WO 2013012352 A1 WO2013012352 A1 WO 2013012352A1 RU 2012000005 W RU2012000005 W RU 2012000005W WO 2013012352 A1 WO2013012352 A1 WO 2013012352A1
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WIPO (PCT)
Prior art keywords
grains
temperature
plastic deformation
deformation
carried out
Prior art date
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Ceased
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PCT/RU2012/000005
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English (en)
Russian (ru)
Inventor
Руслан Зуфарович ВАЛИЕВ
Максим Юрьевич МУРАШКИН
Елена Владимировна БОБРУК
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
FEDERAL'NOE GOSUDARSTVENNOE BYUDZHETNOE OBRAZOVATEL'NOE UCHREZHDENIE VYSSHEGO PROFESSIONAL'NOGO OBRAZOVANIYA "UFIMSKIJ GOSUDARSTVENNYJ AVIATSIONYJ TEKHNICHESKIJ UNIVERSITET" (FGBOU VPO "UGATU")
Original Assignee
FEDERAL'NOE GOSUDARSTVENNOE BYUDZHETNOE OBRAZOVATEL'NOE UCHREZHDENIE VYSSHEGO PROFESSIONAL'NOGO OBRAZOVANIYA "UFIMSKIJ GOSUDARSTVENNYJ AVIATSIONYJ TEKHNICHESKIJ UNIVERSITET" (FGBOU VPO "UGATU")
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Application filed by FEDERAL'NOE GOSUDARSTVENNOE BYUDZHETNOE OBRAZOVATEL'NOE UCHREZHDENIE VYSSHEGO PROFESSIONAL'NOGO OBRAZOVANIYA "UFIMSKIJ GOSUDARSTVENNYJ AVIATSIONYJ TEKHNICHESKIJ UNIVERSITET" (FGBOU VPO "UGATU") filed Critical FEDERAL'NOE GOSUDARSTVENNOE BYUDZHETNOE OBRAZOVATEL'NOE UCHREZHDENIE VYSSHEGO PROFESSIONAL'NOGO OBRAZOVANIYA "UFIMSKIJ GOSUDARSTVENNYJ AVIATSIONYJ TEKHNICHESKIJ UNIVERSITET" (FGBOU VPO "UGATU")
Publication of WO2013012352A1 publication Critical patent/WO2013012352A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22F1/05—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 of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions
    • 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
    • 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
    • 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

Definitions

  • the invention relates to the field of UFG aluminum alloys with increased mechanical strength and conductivity, intended for the manufacture of billets for electrical purposes, for example, wire rod of round and square cross section, wire, wire for overhead power lines, conductive tires and profiles, as well as a method for processing said alloys.
  • thermomechanical processing of an aluminum alloy Al-Mg-Si is described, including in series: quenching from a temperature of 621 ° C into water and cold rolling to a degree of deformation of 99.6%.
  • the alloy structure is characterized by large elongated, mainly non-crystallized grains with a transverse size of more than 50 microns.
  • the grains contain a developed cellular dislocation structure and nanoscale precipitates in the form of needles of reinforcing particles of Mg 2 Si metastable modification ⁇ "and ⁇ '.
  • the content of Mg and Si in the aluminum matrix is at least 0.2 and 0.3 am. %, respectively.
  • a drawback of the structure of aluminum alloys formed by the known TMT method is that it contains predominantly small-angle dislocation boundaries, and it contains nanosized particles of Mg 2 Si phases of only metastable modification.
  • Such a structural state and the method for its preparation do not provide sufficient strength and do not allow to achieve electrical conductivity in aluminum alloys close to that of technically pure aluminum.
  • a wire made of electrotechnical aluminum of the AE grade (99.5A1) shows a level of temporary resistance ( ⁇ ⁇ ) of 100 ... .150 MPa with a specific electrical resistance (p) of 0.0283 Ohm * mm / m (about 61% IACS)
  • the wire made of an ABE grade Al-Mg-Si alloy, obtained by the known TMT method has 280 ...
  • the technical result of the invention is to increase the mechanical strength and electrical conductivity of aluminum alloys of the Al-Mg-Si system by creating an ultrafine-grained (UFG) structure in them obtained by the proposed processing methods.
  • UFG ultrafine-grained
  • an aluminum alloy of the Al-Mg-Si system with an UFG structure, which is characterized by an average grain size of not more than 400 nm. No less than 60% of the grains have large-angle boundaries misoriented relative to neighboring grains by angles of 10 degrees or more.
  • the aluminum matrix of the UFG alloy is significantly depleted in the main alloying elements Mg and Si, the content of which does not exceed contains 0.06 and 0.09 am%, respectively, and contains nanoscale precipitates of particles of the strengthening phase Mg 2 Si of a stable modification ( ⁇ ) of globular shape uniformly distributed in the grain volume.
  • an aluminum alloy of the Al-Mg-Si system with an UFG structure, which is characterized by an average grain size in the range from 400 to 1000 nm. At least 60% of the grains have large-angle boundaries misoriented with respect to neighboring grains by angles of 10 degrees or more.
  • the aluminum matrix of the UFG alloy is significantly depleted in the main alloying elements Mg and Si, the content of which does not exceed 0.08 and 0.10 at.%, Respectively, and contains nanoscale precipitates of particles of the reinforcing phase Mg 2 Si of a stable modification ( ⁇ ) of a globular shape located in the boundary region of grains and metastable modification ( ⁇ ", ⁇ ') in the form of needles located in the central region of grains.
  • the technical result is also achieved by the method of producing an aluminum alloy with an UFG structure with a grain size of not more than 400 nm, including quenching from a temperature of 520 ... 565 ° C in water and plastic deformation, in which, unlike the prototype, plastic The deformation is carried out with the true accumulated deformation e> 8 at a temperature not exceeding 200 ° ⁇ by the method of intensive plastic deformation (IPD).
  • IPD intensive plastic deformation
  • the technical result is also achieved by the method of producing an aluminum alloy for electrical products with UFG structure with a grain size in the range from 400 to 1000 nm, including quenching from a temperature of 520 ... 565 ° C in water and plastic deformation, in which unlike the prototype, plastic deformation is carried out with a true accumulated deformation e> 4 at a temperature of no higher than 300 ° C using the IPD method and artificial aging at a temperature of 10 ... 180 ° C for 0.5 ... 24 hours.
  • the SPD is carried out by torsion (IPDK), equal channel angular pressing (ECAP), equal channel angular pressing in parallel channels (ECAP-PC) and equal channel angular pressing according to the Conform (ECAP-K) scheme.
  • artificial aging is carried out at a temperature of 10 ... 180 ° C for 0.5 ... 24 hours.
  • the proposed UMP structures and methods for their preparation provide a higher level of mechanical strength and electrical conductivity of aluminum alloys of the Al-Mg-Si system used in electrical products.
  • the regulated release in the UFG structure of the hardening nanoscale particles of phases stable ( ⁇ ) and, in particular, metastable modification ( ⁇ ", ⁇ '), also provides the hardening effect from the implementation of the dispersion hardening mechanism [I. Fridlyander Aluminum deformable structural alloys. M: Metallurgy, 1979-208].
  • the regulated release of nanosized particles leads to the depletion of the UFG of the aluminum matrix by the main alloying elements (Mg and Si), which ensures an increase in the electrical conductivity of alloys, since it is the alloying elements that are responsible for electron scattering [B. Livshits, Kraposhin BC, Lipetskiy Ya. L. Physical properties of metals and alloys. M.: Metallurgy, 1973-31 1 s; Aluminum and aluminum alloys in electrical products / L. A. Vorontsova, V. V. Maslov, I. B. Peshkov Publ. "Energy", Moscow 1971 - 224 s].
  • Mg and Si main alloying elements
  • FIG. 1 shows an UFG structure with a grain size of less than 400 nm
  • a is an electron microscopic photograph of the structure
  • b is a schematic representation of the structure
  • FIG. 2 UFG structure with a grain size of more than 400 nm
  • a is an electron microscopic photograph of a general view of the structure
  • b is an electron microscopic photograph of a grain
  • c is an electron microscopic photograph of a fragment of the central region of the grain
  • d is a schematic image of the structure).
  • FIG. Figure 1a shows that the structure consists of grains (1) with a size of less than 400 nm, and contains nanoscale precipitates of particles of the strengthening phase Mg 2 Si (2) of stable modification ( ⁇ ), which have a globular shape and are uniformly distributed in the volume of grains.
  • the structure consists of grains (3) with sizes greater than 400 nm
  • FIG. 2b it can be seen that in the boundary region of the grain there are precipitates of particles of the strengthening phase Mg 2 Si (2) of stable modification ( ⁇ ), which have a globular shape.
  • region (4) shown in enlarged view in Fig. 2c, containing nanoscale precipitates of particles of the hardening phase of the metastable modification ( ⁇ ', ⁇ ") in the form of a needle (5).
  • the invention is implemented as follows:
  • the initial billet of an Al – Mg – Si alloy with a standard chemical composition is used.
  • the billet is subjected to heat treatment-hardening, including heating the billet to a temperature of 520 ... 565 ° C, exposure under these temperature conditions is continued up to 2 hours and subsequent cooling in water at room temperature.
  • the hardened billet is subjected to SPD processing at a temperature not exceeding 200 ° C, with a true accumulated deformation of e> 8.
  • SPDK or ECAP or ECAP-PK or ECAP-K.
  • the microstructure is crushed in the bulk of the workpiece without changing its size. Due to the evolution of the structure during the SPD process under specified conditions, an UFG structure with an average grain size of not more than 400 nm is formed in aluminum alloys. At least 60% of the grains have large-angle boundaries misoriented with respect to neighboring grains by angles of 10 degrees or more.
  • DDS occurs in the aluminum matrix, as a result of which nanodimensional precipitates of particles of the hardening ⁇ phase (Mg 2 Si) of stable modification are formed in it, having a globular shape uniformly located in the grain volume.
  • the separation of ⁇ phase particles leads to a significant depletion of the aluminum matrix by the main alloying components (Mg and Si), which ensures an increase in the electrical conductivity of the material.
  • an initial billet of an alloy of the Al-Mg-Si system with a standard chemical composition is used.
  • the billet is subjected to heat treatment — quenching, which includes heating the billet to a temperature of 520 ... 565 ° C, holding it under given temperature conditions for up to 2 hours and then cooling it in room temperature water.
  • the hardened billet is subjected to SPD processing at a temperature not exceeding 300 ° C, with a true accumulated deformation of e> 4.
  • SPD processing can be carried out using the IPDK or ECAP or ECAP-PK or ECAP-K method.
  • the initial structure is transformed into a subgrain one with a clearly defined orientation with respect to the shear plane.
  • the transverse size of the formed subgrains is 600 nm, and the longitudinal size is 1200 nm, respectively.
  • the resulting structural state is characterized by a high density of lattice dislocations.
  • an UFG structure is formed in an aluminum alloy with a grain size in the range of 400 ... 1000 nm, of which more than 60% of the grains have large-angle boundaries, misoriented relative to neighboring grains by angles of 10 degrees or more .
  • DDS passes in the aluminum matrix, as a result of which nanoscale precipitates of particles of the strengthening phase (Mg 2 Si) of a stable modification ( ⁇ ) of globular shape are formed.
  • the formed ⁇ phase particles are predominantly located in regions adjacent to the grain boundaries.
  • the billet is subjected to artificial aging at a temperature of 10 ... 180 ° C with a holding time of 0.5 ... 24 hours.
  • Artificial aging according to the indicated regime leads to further evolution of the structure obtained after SPD, which consists in the formation in the central region of grains of nanoscale precipitates of particles of strengthening phases of Mg 2 Si metastable modification ( ⁇ ', ⁇ "), having the shape of a needle, which ensures additional increase in material strength.
  • the depletion of the aluminum matrix by the main alloying elements (Mg and Si) at the second stage of processing — during the DDS, and at the third stage of processing — during artificial aging ensures an increase in the electrical conductivity of the material.
  • a hot pressed rod of alloy 6060 of the Al – Mg – Si system with a standard chemical composition with a diameter of 20 mm was used as the initial billet. From this rod, a billet in the form of a disk with a diameter of 20 mm and a thickness of 1.5 mm was made by machining. This preparation was subjected to heat treatment — quenching, which included heating to a temperature of 540 ° C, holding at a given temperature for 1 hour, and subsequent cooling to room temperature in water. The time interval between the heat treatment operation and the IPD was no more than 1 hour.
  • the microstructure was analyzed by transmission electron microscopy (TEM) using a Jeol 2100 EX microscope.
  • XRD X-ray diffraction analysis
  • Table 1 presents the results of structural studies, mechanical tests and measurements of the electrical conductivity of the obtained samples. As a comparison, the results of studies of alloy samples subjected to the TMT method according to the prototype are given.
  • a hot-pressed rod of alloy ADZ 1 of the Al-Mg-Si system of standard chemical composition with a diameter of 12 mm and a length of 500 mm was used as the initial billet.
  • This billet was subjected to heat treatment — quenching, including heating to a temperature of 540 ° C, holding at a given temperature for 1 hour, and subsequent cooling to room temperature in water. The interval between the heat treatment operation and the IPD was no more than 1 hour.
  • the billet was subjected to ECAP-K processing to the true accumulated strain e – 4.8 under isothermal conditions at a temperature of 100 ° ⁇ .
  • the angle of conjugation of the channels in the instrument was P O degrees.
  • the workpiece was removed from the tool / tool, cooled in air to room temperature, and then subjected to drawing at room temperature with a total degree of deformation of 50%.
  • a bar with a diameter of 6 mm and a length of more than 1 m was obtained.
  • the billet was subjected to heat treatment — artificial aging at a temperature of 130 ° C and a holding time of 12 hours.
  • the microstructure was analyzed by transmission electron microscopy (TEM) using a Jeol 2100 EX microscope.
  • XRD X-ray diffraction analysis
  • the obtained UFG structure in the alloy preform (Fig. 2a), which was formed during the implementation of the proposed processing method, has an average grain size (3) of 600 nm.
  • Fig. 2b Inside the grain (Fig. 2b), there are visible precipitates of globular particles of the secondary reinforcing ⁇ phase (Mg 2 Si) (2) of stable modification with an average size of 20 nm located in the border region, and precipitates of particles of the reinforcing phases ( ⁇ ', ⁇ ") of metastable modification in the form of needles (5) (Fig. 2c) with a diameter of 2 nm and a length of up to 40 nm, located in the central region of grains (4) (Fig. 2b).
  • Table 2 presents the results of structural studies, mechanical tests, and measurements of the electrical resistivity of the obtained samples. As a comparison, the results of studies of alloy samples subjected to the TMT method according to the prototype are given.
  • the proposed invention allows the formation in the UFG aluminum alloys of a structure providing the material with enhanced mechanical strength and electrical conductivity.

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Abstract

L'invention concerne la production d'alliages d'aluminium et s'utilise dans des articles électrotechniques. Pour augmenter la résistance mécanique et la conductivité électrique on forme dans des alliages d'aluminium du système Al-Mg-Si deux types de structure à très faible granularité présentant une granularité de 400 à 1000 nm comprenant un trempage dans l'eau à une température de 520-565°С, une déformation plastique intensive avec un bilan de déformation authentique accumulée е>8 et une température de déformation inférieure ou égale à 200 °С dans un premier mode de réalisation е>4 et une température inférieure ou égale 300 °С dans un deuxième mode de réalisation; dans ce mode de réalisation, la déformation est suivie d'un vieillissement artificiel. Les alliages ont une structure dans laquelle au moins 60 % des grains ont des frontières en forme d'angle orientées différemment par rapport aux grains voisins à la hauteur d'une valeur de 10 degrés et plus, et qui est appauvrie en éléments d'alliage principaux Mg et Si sur une matrice d'aluminium; elle comportent des excrétions de la taille de quelques nanomètres de la phase de raffermissement Mg2Si de la modification (β), qui est répartie dans le volume des grains ou dans la modification (β) disposée dans la région frontière des grains et de modification (β", β') possédant une forme en aiguilles et disposée dans la partie centrale des grains.
PCT/RU2012/000005 2011-07-15 2012-01-13 Alliages d'aluminium à très petits grains pour articles électrotechniques et procédés de fabrication correspondants (et variantes) Ceased WO2013012352A1 (fr)

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RU2011129486 2011-07-15
RU2011129486/02A RU2478136C2 (ru) 2011-07-15 2011-07-15 Ультрамелкозернистые алюминиевые сплавы для электротехнических изделий и способы их получения (варианты)

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RU2534909C1 (ru) * 2013-10-17 2014-12-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" СПОСОБ ТЕРМОМЕХАНИЧЕСКОЙ ОБРАБОТКИ ДЛЯ ПОВЫШЕНИЯ ТЕХНОЛОГИЧЕСКОЙ ПЛАСТИЧНОСТИ ОБЪЕМНЫХ ПОЛУФАБРИКАТОВ ИЗ Al-Cu-Mg-Ag СПЛАВОВ
RU2616316C1 (ru) * 2015-11-06 2017-04-14 Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) Проводниковый ультрамелкозернистый алюминиевый сплав и способ его получения
RU2641211C1 (ru) * 2016-12-22 2018-01-16 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Нижегородский государственный университет им. Н.И. Лобачевского" Способ формирования высокопрочной и коррозионно-стойкой структуры алюминиево-магниевого сплава
RU2641212C1 (ru) * 2016-12-22 2018-01-16 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Нижегородский государственный университет им. Н.И. Лобачевского" Способ формирования мелкозернистой высокопрочной и коррозионно-стойкой структуры алюминиевого сплава
RU2667271C1 (ru) * 2017-11-23 2018-09-18 Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) Термостойкий проводниковый ультрамелкозернистый алюминиевый сплав и способ его получения
RU2749601C2 (ru) * 2019-12-13 2021-06-15 Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ)" Способы термомеханической обработки проводниковых сплавов системы Al-Mg-Si
CN112251691B (zh) * 2020-10-30 2022-03-08 郑州轻研合金科技有限公司 一种5a90铝锂合金超细晶板材的制备方法
CN115094277B (zh) * 2022-07-11 2023-01-24 上海交通大学 一种混晶结构铝合金及其制备方法和应用

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RU2105621C1 (ru) * 1993-11-10 1998-02-27 Валерий Николаевич Щерба Способ горячего экструдирования металла с активным действием сил трения и гидравлический экструзионный пресс для его осуществления
US7490752B2 (en) * 2003-05-20 2009-02-17 Alcan Rhenalu Manufacturing method for friction welded aluminum alloy parts
RU2284367C1 (ru) * 2005-01-27 2006-09-27 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") Способ изготовления изделий из алюминиевых деформируемых сплавов
RU73875U1 (ru) * 2007-12-28 2008-06-10 Институт проблем сверхпластичности металлов РАН Холодный катод

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