WO2008120497A1 - Alliage de magnésium résistant à la chaleur - Google Patents

Alliage de magnésium résistant à la chaleur Download PDF

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Publication number
WO2008120497A1
WO2008120497A1 PCT/JP2008/052085 JP2008052085W WO2008120497A1 WO 2008120497 A1 WO2008120497 A1 WO 2008120497A1 JP 2008052085 W JP2008052085 W JP 2008052085W WO 2008120497 A1 WO2008120497 A1 WO 2008120497A1
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Prior art keywords
magnesium alloy
crystal
heat
grain boundary
mass
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PCT/JP2008/052085
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English (en)
Japanese (ja)
Inventor
Tsukasa Sugie
Kyoichi Kinoshita
Motoharu Tanizawa
Manabu Miyoshi
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Kabushiki Kaisha Toyota Jidoshokki
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Application filed by Kabushiki Kaisha Toyota Jidoshokki filed Critical Kabushiki Kaisha Toyota Jidoshokki
Priority to US12/594,508 priority Critical patent/US20100116378A1/en
Priority to EP08710964A priority patent/EP2135965A4/fr
Priority to JP2009507427A priority patent/JPWO2008120497A1/ja
Publication of WO2008120497A1 publication Critical patent/WO2008120497A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent

Definitions

  • the present invention relates to a heat-resistant magnesium alloy that can withstand use under high temperature and high load.
  • Magnesium alloys which are lighter than aluminum alloys, are being widely used as sailing materials and vehicle materials from the viewpoint of weight reduction.
  • magnesium alloys are not sufficient in strength and heat resistance depending on the application, so further improvement in properties is required.
  • Japanese Laid-Open Patent Publication Nos. 2004-162090 and 2004-232060 disclose magnesium alloys containing appropriate amounts of calcium (Ca) and aluminum (A1).
  • the dislocation motion is stopped because the Ca 1 A 1 compound or Mg—Ca compound is crystallized or precipitated at the grain boundary of the Mg crystal grains of the magnesium alloy.
  • the magnesium alloy exhibits excellent heat resistance with little creep deformation even at high temperatures.
  • the magnesium alloy described above strengthens the magnesium alloy by dissolving Mn in the Mg crystal grains. Disclosure of the invention
  • the metal paper weave of the alloy greatly affects its properties. For this reason, in order to obtain a magnesium alloy with sufficient strength and creep resistance for use at high temperatures, it is necessary to control the metal texture by making the types and amounts of additive elements appropriate.
  • the present invention reinforces both the crystal grains and the grain boundaries, and exhibits excellent heat resistance.
  • the aim is to use a metal alloy.
  • the heat-resistant magnesium alloy of the present invention comprises the main component magnesium ( ⁇ g), one or more first alloy elements M 1 selected from aluminum (A1) and Eckel (N i), manganese ( Mn), barium (B a), chromium (Cr) and iron (Fe) forces, any one or more of the second alloy element M2 selected from the force, calcium (C a), and
  • “microscopically continuous network” has a macroscopic network structure (three-dimensional network structure), and a state in which crystals are continuously present within the network. (See Fig. 2). Therefore, even if it has a network structure, it does not include the discontinuous state (see Fig. 3) that consists of small crystals inside.
  • the heat-resistant magnesium alloy of the present invention will be described in detail later.
  • the second alloy element M 2 plate-like precipitates are formed in the grain of Mg crystal grains, and microscopically continuous in the grain boundaries. It has grain boundary crystals that form a network. Since plate-like precipitates are present in the Mg crystal grains, the movement of dislocations in the Mg crystal grains is hindered and deformation becomes difficult.
  • the grain boundary crystallized material that forms the network is present microscopically continuously at the grain boundary of the Mg crystal grains, so that the grain boundary strength i is improved.
  • the magnesium alloy of the present invention exhibits high mechanical properties even in a high temperature region.
  • the heat-resistant magnesium alloy of the present invention remarkably improves the characteristics at high temperatures by strengthening both the intragranular and O boundaries of Mg crystal grains.
  • the precipitate is preferably composed of a Laves phase compound having a C15 type crystal structure.
  • the precipitate is preferably precipitated in parallel with the ⁇ 001 ⁇ plane of the Mg crystal.
  • the grain boundary crystallized material forming a microscopic continuous network is preferably composed of an Mg-Ml-Ca-based compound.
  • the Fujimi grain boundary crystallized material is composed of a mixed crystal phase of Laves phase compounds having a C 14 type crystal structure and a C 36 type crystal structure.
  • the mixed crystal structure preferably contains more C14-boiling crystal structure than C36 type crystal structure.
  • the grain boundary crystallized substance is composed of a mixed crystal phase of Laves phase compound of C 14 hard crystal structure and C 3 6 type crystal structure, the compound constituting the network is almost single crystal in appearance without phase separation (Fig. 4) and the area of the crystal grain boundary and the number of crystal grains constituting the net ⁇ are minimized.
  • C 14 type “C 15 type” and “C 36 type” are symbols of Strukturberichte clogging, which are Mg Z n 2 and M in the Laves phase, respectively. It represents three similar ⁇ : like crystal structures represented by g C u 2 and MgN i 2 .
  • the entire heat-resistant magnesium alloy of the present invention is 100% by mass
  • Ca is 2% by mass or more and 4% by mass or less
  • the first alloy element Ml is 0.9% by mass ratio (Ml / Ca) to Ca. or 1.1 or less, wherein comprises a second alloying element M2 of 0.3 mass% or more 0.6 mass 0/0 or less, Shi remainder preferable that consists M g and inevitable impurities les.
  • C a is 1.235 atomic% or more and 2.470 atomic% or less
  • the atomic ratio of the first alloy element M 1 to C a (MlZCa ) 1.34 or more and 1.63 or less, preferably 0.13 atomic% or more and 0.27 atomic% or less of the second alloying element M2, and remaining force SMg and inevitable impurities.
  • the content ratio of the first alloy element, the second alloy element and Ca containing the heat-resistant 14-magnesium alloy power of the present invention within an appropriate range, it is desirable from the viewpoint of the mechanical properties at high temperature, and the metal yarn A heat-resistant raw magnesium alloy with cocoons is obtained.
  • Heat resistance in this specification is evaluated by the mechanical properties of magnesium alloys in high-temperature atmospheres (for example, creep properties by stress relaxation tests and axial force retention tests, or high-temperature strength). Is. Brief Description of Drawings
  • Figure 1 is a metallographic photograph of a cross section of the # 01 test piece observed with a metallographic microscope.
  • Figure 2 is a metallographic image of the # 01 observation sample observed with an electron microscope (TEM).
  • TEM electron microscope
  • Figure 3 is a metal paper weave photograph of # C 1 observed by TEM.
  • Fig. 4 shows a scanning field electron microscope (DF-STEM) image of the observation sample # 01.
  • Fig. 5 is a DF-ST EM image of the observation sample of # C1.
  • Figure 6 shows the TEM image and electron diffraction of the observation sample # 01 (incident direction foil 110
  • Figure 7 shows the TEM image and electron diffraction (incident direction foil 111) of the observation sample # 01.
  • Figure 8 shows the TEM image and electron diffraction of the observation sample of # C 1 (incident direction foil 111
  • Fig. 9 is a DF-S TEM image of the observation sample # 01 observed in the Mg crystal grains. Note that # 01 No. # 01 is a symbol for distinguishing magnesium alloys having different compositions in the examples described later. BEST MODE FOR CARRYING OUT THE INVENTION
  • magnesium alloy The best mode for carrying out the heat-resistant magnesium alloy of the present invention (hereinafter abbreviated as “magnesium alloy”) will be described below.
  • the magnesium alloy of the present invention contains magnesium (M g ) as a main component, first alloy element Ml, second alloy element M2, and calcium (Ca), Mg crystal grains, and Mg crystal grains
  • Mg magnesium
  • a metal paper weave comprising: a plate-like precipitate that precipitates within the grains; a grain boundary crystal that crystallizes at a grain boundary of the Mg crystal grains to form a microscopic continuous network;
  • plate-like precipitates exist in the Mg crystal grains. Plate-like precipitates hinder the movement of dislocations in Mg grains. Crystal deformation occurs when dislocations move on the slip plane.
  • the c-plane of hexagonal Mg crystal In other words, it should be a TO-like precipitate on the ⁇ 001 ⁇ face of the Mg crystal.
  • the plate-like precipitate has a thickness of 2 to 20 nm, and the thicker the wrinkles, the better the leakage characteristics.
  • the precipitate is preferably composed of a Laves phase compound having a C15 type crystal structure. This is because the c-plane of the Mg crystal and the ⁇ 111 ⁇ plane of the C15 structure are likely to form a crystallographically stable interface with each other, and it can be predicted that the formation force S of the plate-like precipitate is promoted.
  • the compound constituting the precipitate having such a crystal structure is preferably an Ml—Ca compound and / or an Mg—Ml—Ca compound.
  • the magnesium alloy of the present invention may further have fine particles in the Mg crystal grains.
  • the fine particles are in the Mg crystal grains and mostly around the plate-like precipitates. It is considered that this fine particle does not directly contribute to the improvement of the strength in the Mg crystal grains even in the Mg crystal grains.
  • the fine particles are related to the formation of precipitates (described later), and the fine particles are fine particles containing M2, such as l-M2 compounds.
  • the fine particles are substantially spherical and have a particle size of 10 to 15 nm ⁇ l.
  • the grain boundary crystallized material forming a microscopic continuous network is crystallized and present at the grain boundary of the Mg crystal grain.
  • the grain boundary crystallized crystallizes at the grain boundary of the Mg crystal grains and forms a network.
  • the magnesium alloy containing M2 does not show microscopic continuous I 1 growth in the grain boundary crystals that form the network.
  • the inclusion of M 2 forms a network in which the grain boundary crystallization products are microscopically continuous.
  • the grain boundary crystallized network is 70% or more of the Mg grain boundary that is linearly seen in the cross section of the magnesium alloy region of about 400 ⁇ 600 ⁇ m. It is desirable to cover “coverage”.
  • the grain boundary crystallization is a Laves phase compound of C 14 type crystal structure and C 36 type crystal structure. It may consist of a mixed crystal phase of the product.
  • the C14 type crystal structure and the C36 type crystal structure are desirable because they are hexagonal and easily form a mixed crystal phase. Since the Laves phase compound in the mixed crystal phase is as close to a single crystal as possible, the grain boundary crystallization is microscopically continuous, and the grain boundary area and grain size of the compound composing the network. The number is minimized.
  • the grain boundary crystallization product is preferably composed of a Mg-M1-Ca compound.
  • Mg 2 Ca has a C 14 type crystal structure, and when M 1 is dissolved in Mg 2 Ca, a mixed crystal phase of a C 14 type crystal structure and a C 36 type crystal structure is formed. Guessed. At this time, the mixed crystal phase preferably contains more C14 type crystal structure than C36 type crystal structure.
  • the magnesium alloy of the present invention having the metal paper weave as described above contains the main component of magnesium (Mg), the first alloy element Ml, the second alloy element M2, and calcium (Ca).
  • the first alloy element Ml at least one selected from aluminum (A 1) and nickel (Ni) can be used. Both A1 and Ni react with Ca to form a compound and have a C15-type Laves structure. However, Mg 2 C a, which has a C14-type Laves structure, is dominant. , A 1 and / or Ni dissolve in Mg 2 C a to form a mixed crystal phase of C 14 type Laves structure and C 36 type Laves structure.
  • the second alloy element M 2 at least one selected from manganese (Mn), barium (Ba), chromium (Cr), and iron (Fe) forces can be used.
  • Mn manganese
  • Ba barium
  • Cr chromium
  • Fe iron
  • the second alloy element M 2 needs to react at a higher temperature than the first alloy element M 1 and T 3 and be difficult to dissolve in Mg.
  • the second alloy element at least one selected from manganese (Mn), norlium (Ba), throat (Cr) and iron (F e) force is used among the transition elements. be able to.
  • These elements have the same atomic structure, have similar crystal structures, and form compounds only between Ml and a relatively high temperature region, specifically between T 1 and T 3.
  • the magnesium alloy of the present invention contains at least one kind of the above-mentioned first alloy element and second alloy element.
  • One kind of each of the first element and the second element may be included, or one or both of the forces and the displacement force may be included.
  • the magnesium alloy of the present invention has two masses of Ca when the total is 100% by mass. / 0 or more and 4% by mass or less, and the first alloy element M 1 is 0.9 to 1.1 by mass ratio (M1 / C a) to C a, and the second alloy element M2 is 0.3% by mass or more. It is preferable that the content is 0.6% by mass or less and the balance is Mg and inevitable impurities.
  • the magnesium alloy of the present invention has a Ca content of 1.235 atomic% or more and 2.470 atomic% or less, and the tooth 1st alloy element M 1 is an atom with respect to C a when the total is 10 ° atomic%.
  • the ratio (Ml / Ca) is 1.34 or more and 1.63 or less
  • the second alloy element M 2 is contained in an amount of 0.13 atomic% or more and 0.27 atomic% or less, with the balance being Mg and inevitable impurities. preferable. .
  • & is less than 0.9 by mass (ie, less than 1.34 by atomic ratio)
  • the content of Ca is large and the forgery is considered, which is not preferable.
  • Ml-no-Ca exceeds 1.1 by mass (ie, exceeds 1.63 by atomic ratio)
  • the grain boundary crystallization is unlikely to become a mixed crystal phase, and only C 36 type Laves structure This is preferable because the composed crystal grains are easily formed and phase separation occurs.
  • the C36 crystal structure is exposed to high temperatures. Then, it is easy to make a phase transition to CI 5 type crystal structure (Scripta Material ia 51 (2004) 1005- 1010).
  • the C 15 crystal structure tends to be agglomerated in a high temperature region and does not form a microscopically continuous crystallized network, so that the properties at high temperatures are significantly reduced.
  • a more preferable M 1 / Ca value is 0.95 or more and 1.05 or less (that is, 1.4 2 to 1.5 6 in terms of atomic ratio).
  • the content ratio of the second alloy element M 2 is less than 0.3% by mass (that is, 0.1 3 atom 0 /.), It is possible to add M l constituting the precipitate as a compound in the P process (solidification process). This is not preferable because the precipitate cannot be sufficiently precipitated. In addition, a large amount of M 1 force 2 does not form a crystal, and it does not take a mixed crystal structure as a grain boundary crystallized product. On the other hand, when the content ratio of ⁇ 2 exceeds 0.6 mass% (that is, 0.27 atomic%), the compound containing ⁇ 2 precipitates in the grain boundary crystallized product. Further, the lower limit of the content ratio of ⁇ 2 is 0.34% by mass (that is, 0.15 atomic%) or more. The upper limit is 0.5 5 mass% (ie 0.25 atomic%) or less, and further 0.5 mass% (that is, 0.23 atomic%) or less.
  • C a is an element that forms C 14 and C 36 Laves structures together with Mg. If the Ca content is less than 2% by mass (ie, 1.235% by atom), precipitates and grain boundary crystals are not sufficiently formed, and the effect of improving heat resistance is not sufficient. It ’s not. On the other hand, if the Ca content exceeds 4% by mass (that is, 2.470% by atom), the amount of precipitates and grain boundary crystallized products will increase and cause problems in post-processing. This is not preferable. More preferably, the Ca content is 2.5 mass% or more and 3.5 mass% or less (that is, 1.5 4 atomic% or more and 2. 16 atomic% or less). Not limited to gravity, but it can also be die-cast.
  • ⁇ used for forging does not matter whether it is a sand mold or a mold.
  • the cooling rate in the solidification process is no particular limitation on the cooling rate in the solidification process, but it is preferable to cool in the air.
  • the use of the magnesium alloy of the present invention extends to various fields such as space, military and aviation, as well as automobiles and home electric Saito.
  • the magnesium alloy strength of the present invention can be applied to products that are used in high-temperature environments by taking advantage of its heat resistance, such as engines, transmissions, compressors for air conditioners or related products that are installed in the engine compartment of automobiles. If used, it is more preferable. Specific examples include cylinder heads for internal combustion engines, cylinder plugs, oil pans, turbocharger impellers for internal combustion engines, transmission cases used in automobiles, and the like.
  • Chloride-based flux was applied to the inner surface of an iron crucible preheated in an electric furnace, and weighed pure magnesium ingot, pure Al, and Mg-Mn alloy as required, were dissolved. In addition, weighed Ca was added during this easy, which was maintained at 75 ° C.
  • the molten metal was sufficiently stirred to completely dissolve the raw materials, and then kept calm for a while.
  • a mixed gas of carbon dioxide gas and SF 6 gas was sprayed on the hot metal surface, and flux was appropriately sprayed on the hot metal surface.
  • the various alloy melts thus obtained were poured into a mold having a predetermined shape (a pouring process) and solidified in an atmosphere (solidification process).
  • a 3 O ramX 30 O mmX 4 O ram test piece was manufactured by gravity.
  • the obtained specimens were designated as # 0 1 (Example including Mn) and # C 1 (Comparative example not including Mn). Table 1 shows the chemical composition of each specimen.
  • Specimens # 01 and # C1 were observed with a metal microscope or a transmission electron microscope (TEM). .
  • Figure 1 is a metallographic photograph of a cross section of the # 01 test piece observed with a metallographic microscope.
  • Mg crystal grains (bright parts) and grain boundary crystallized grains (black parts) appearing in a network form at the grain boundaries of Mg crystal grains were observed.
  • a metal paper weaving photograph similar to that in Fig. 1 was obtained by observing the cross section of the specimen # C1. In other words, macroscopically, grain-like crystallized crystals were observed in the specimens of the les and misalignments.
  • each test piece was used as a flaky observation sample and observed using a TEM.
  • Figures 2 and 3 are metal paper weaving photographs of # 01 and # C1 observed with TEM, respectively. In both cases, grain boundaries where two or more primary Mg grains were adjacent to each other were observed. In Fig. 2 (# 01), the grain boundary crystallization (black part) grew like a lamellar and was continuous. In Fig. 3 (# C1), the grain boundary crystals were partially discontinuous and discontinuous. The coverage of # 01 network is about 90%.
  • Figures 4 and 5 are dark-field scanning transmission electron microscope (DF-STEM) images of the observed grain boundary crystals of the # 01 and #C 1 samples, respectively.
  • the specimen of # 01 does not show phase separation as shown in Figure 4, but the specimen of #C 1 Phase separation was observed.
  • elemental mapping by energy dispersive X-ray spectroscopy (EDX) is performed on the DF—ST EM images in Figs. 4 and 5, Mg, A 1 and Ca are uniformly distributed in Fig. 4 (# 01).
  • Fig. 5 (# C1) the concentration of A 1 was higher in the grains that were separated into ⁇ and phase separated. Electron diffraction of the C36 crystal structure was obtained from the crystal grains with high A1 concentration.
  • Fig. 1 elemental mapping by energy dispersive X-ray spectroscopy
  • Figures 6 and 7 are TEM images of specimen # 01 and Figure 8 is specimen # (1, 1.
  • Figure 6 shows the Alt direction 110>
  • Figures 7 and 8 show the incident direction 111> Mg.
  • Fig. 6 '(# 01) streaky precipitates parallel to the ⁇ 001 ⁇ plane were observed, and the incident direction was tilted at the same position as in Fig. 6.
  • the precipitate was a plate with 5 Fff on the ⁇ 001 ⁇ plane, and when STEM-EDX analysis was performed on this plate-like precipitate, mainly A 1 and Ca were detected.
  • an electron diffraction pattern of a C 15 type crystal structure corresponding to A 1 2 Ca was obtained from the plate-like precipitate. It was.
  • Figure 9 is a DF-STEM image of the observed # 01 observation sample in the Mg crystal grains. A plurality of fine particles were observed around the plate-like precipitate. When elemental analysis was performed on fine particles (B in Fig. 9), Mn was detected. Even when the plate-like precipitate was analyzed (A in Fig. 9), Mn was not detected.
  • Specimens # 01 and # (shown in Table 1): AXE662, A E42, and AZ91D (all AS TM standards) shown in Table 2 were subjected to stress relaxation tests.
  • the heat resistance (creep characteristics) of the magnesium alloy was investigated
  • the stress relaxation test measures the process in which the stress when a load is applied to a specified amount of deformation during the test time decreases with time. Specifically, in an air atmosphere at 150 ° C, a compressive stress of 10 OMPa was applied to the specimen, and the displacement of the specimen at that time was kept constant along with the passage of time.
  • Table 2 and Table 3 show the alloy composition of each specimen and the stress after 40 hours of the stress relaxation test, with the magnesium alloy compositions in Table 2 and Table 3. The balance is Mg, and “RE” is Misch Metal.
  • Specimen # 01 showed a particularly low rate of decrease in applied stress compared to other specimens, and exhibited high creep resistance even at high temperatures. This is because, due to the presence of Mn, a strong microscopically continuous network was formed at the grain boundary of the Mg crystal grains, and the dislocation movement was suppressed by the plate-like precipitates in the Mg crystal grains. This is because the deformation resistance increased and the strength of specimen # 01 improved.

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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Abstract

La présente invention concerne un alliage de magnésium résistant à la chaleur comprenant du Mg comme composant principal ; au moins l'un quelconque choisi parmi du Al et du Ni comme premier élément d'alliage (M1) ; au moins l'un quelconque choisi parmi du Mn, du Ba, du Cr et du Fe comme second élément d'alliage (M2) ; et du Ca. Cet alliage de magnésium résistant à la chaleur présente une structure métallographique contenant des grains cristallins de Mg ; des précipités de type plaques ayant précipité à l'intérieur des grains cristallins de magnésium ; et des cristallisats aux joints de grain ayant cristallisé aux joints entre les grains cristallins de Mg et formant un réseau continu au niveau microscopique. Grâce à la présence des précipités de type plaques à l'intérieur des grains cristallins de Mg, le transfert de dislocation à l'intérieur des grains cristallins de Mg est bloqué afin de restreindre ainsi toute déformation. En outre, grâce à la présence continue au niveau microscopique de cristallisats aux joints de grain formant un réseau aux joints entre les grains cristallins de Mg, la résistance des joints de grain est augmentée. Cet alliage de magnésium ayant l'intérieur et les joints de ses grains cristallins de Mg simultanément renforcées présente des propriétés mécaniques élevées, même dans la région des hautes températures.
PCT/JP2008/052085 2007-04-03 2008-02-01 Alliage de magnésium résistant à la chaleur WO2008120497A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US12/594,508 US20100116378A1 (en) 2007-04-03 2008-02-01 Heat-resistant magnesium alloy
EP08710964A EP2135965A4 (fr) 2007-04-03 2008-02-01 Alliage de magnésium résistant à la chaleur
JP2009507427A JPWO2008120497A1 (ja) 2007-04-03 2008-02-01 耐熱性マグネシウム合金

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JP2007-097760 2007-04-03
JP2007097760 2007-04-03

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EP (1) EP2135965A4 (fr)
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CN (1) CN101652489A (fr)
WO (1) WO2008120497A1 (fr)

Cited By (2)

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JP2011070785A (ja) * 2009-09-24 2011-04-07 Gs Yuasa Corp 非水電解質二次電池用負極活物質、非水電解質二次電池用負極及び非水電解質二次電池
US20110176955A1 (en) * 2008-10-03 2011-07-21 Kabushiki Kaisha Toyota Jidoshokki Heat-resistant magnesium alloy

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US8435444B2 (en) 2009-08-26 2013-05-07 Techmag Ag Magnesium alloy
JP6048216B2 (ja) * 2013-02-28 2016-12-21 セイコーエプソン株式会社 マグネシウム基合金粉末およびマグネシウム基合金成形体
CN106119646A (zh) * 2016-08-17 2016-11-16 浙江特富锅炉有限公司 一种锅炉管及其制作工艺

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JPH08269609A (ja) * 1995-03-27 1996-10-15 Toyota Central Res & Dev Lab Inc ダイカスト性に優れたＭｇ−Ａｌ−Ｃａ合金
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EP2135965A1 (fr) 2009-12-23
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JPWO2008120497A1 (ja) 2010-07-15
EP2135965A4 (fr) 2010-03-31

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