WO2003095689A1 - Agent d'affinage de grain pour produits coules en magnesium - Google Patents

Agent d'affinage de grain pour produits coules en magnesium Download PDF

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Publication number
WO2003095689A1
WO2003095689A1 PCT/CA2003/000715 CA0300715W WO03095689A1 WO 2003095689 A1 WO2003095689 A1 WO 2003095689A1 CA 0300715 W CA0300715 W CA 0300715W WO 03095689 A1 WO03095689 A1 WO 03095689A1
Authority
WO
WIPO (PCT)
Prior art keywords
particles
nucleation
refining agent
grain refining
ductile material
Prior art date
Application number
PCT/CA2003/000715
Other languages
English (en)
Inventor
Sabin Boily
Houshang Darvishi Alamdari
Original Assignee
Groupe Minutia Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Groupe Minutia Inc. filed Critical Groupe Minutia Inc.
Priority to AU2003229453A priority Critical patent/AU2003229453A1/en
Publication of WO2003095689A1 publication Critical patent/WO2003095689A1/fr

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Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention pertains to improvements in the field of cast metals and metal alloys. More particularly, the invention relates to a grain refining agent for cast magnesium products.
  • Grain refiners are widely used to reduce the grain size and to control the microstracture of cast metals and alloys. Adding grain refiners to molten metal or alloy during casting enhances the heterogeneous solidification and results in a fine-structured material with equiaxed grains. The resulting material shows improved mechanical properties such as high yield strength and toughness. This effect is more pronounced on Mg-based alloys with an HCP structure than metals with an FCC structure such as Al, Cu, or Ni. With a fine microstracture the machinability of the cast products is improved, the porosity is reduced and the pores are distributed more evenly within the products, and heat treatment is more effective due to the small diffusion distances.
  • the GRF of a number of elements has been reported by Y.C. Lee et al. in Metallurgical and Materials Transactions A, Vol. 31 A, 2000, pp. 2895- 2906.
  • Zr, Ca, Si and Ni have the highest GRF.
  • the addition of small amounts of these elements in pure magnesium shows that the mean grain size decreases drastically, reaching a constant value at high addition levels (>0.3%). At these addition levels, a mean grain size of 100-500 ⁇ m can be obtained.
  • Zirconium is the most efficient solute element for grain refining, but it interferes with aluminum and thus cannot be added in Mg-based alloys containing aluminum.
  • AZ91 alloy containing 9 wt. % of aluminum, is a commonly used Mg-based alloy.
  • the aluminum in this alloy has a beneficial effect on the mean grain size.
  • This alloy due to a high concentration of aluminum, has a very fine microstracture and a sand cast AZ91 alloy has normally a mean grain size of about 120 ⁇ m. Further addition of refining elements such as strontium has no significant effect on the mean grain size.
  • Carbon inoculation is another method providing a very good refining effect and it has become the major industrial grain refining practice for Mg-based alloys. Carbon can be added in molten magnesium in form of carbon containing solids or gases.
  • the most commonly used grain refiner for magnesium is C 2 C1 6 .
  • C 2 C1 6 is a low cost material which decomposes in liquid magnesium.
  • the grain refinement effect of carbon is attributed to the formation of aluminum carbide particles (A1 4 C 3 ) which act as nucleation sites for magnesium solidification. The problem encountered with this refiner is the emission of toxic chlorinated gases.
  • a grain refining agent for cast magnesium products comprising particles formed of a matrix of a ductile material, in which are uniformly dispersed nucleation particles of at least one element or compound selected from the group consisting of zirconium, silicon carbide, titanium carbide and mixtures of carbon with silicon or titanium, the nucleation particles having an average particle size of 0.05 to 5 ⁇ m.
  • cast magnesium product refers to a cast product comprising magnesium or an alloy thereof.
  • the average particle size of the nucleation particles must be within a range of from 0.05 to 5 ⁇ m. When the average particle size is greater than 5 ⁇ m, the number of nucleation particles introduced into the melt for a given addition level is too small. On the other hand, when the average particle size is smaller than 0.05 ⁇ m, the heterogeneous nucleation of molten magnesium is not effective.
  • Applicant has found quite unexpectedly that the dispersion of the nucleation particles within a matrix of ductile material improves their wettability, overcomes the problems caused by gas absorption on the surface of the particles and reduces their agglomeration during inoculation into molten magnesium or alloy thereof.
  • the present invention also provides, in another aspect thereof, a method of preparing a grain refining agent as defined above.
  • the method of the invention comprises the steps of:
  • step (a) mixing particles of a ductile material with nucleation particles of at least one element or compound selected from the group consisting of zirconium, silicon carbide, titanium carbide and mixtures of carbon with silicon or titanium, to form a powder mixture, the nucleation particles having an average particle size of 0.05 to 5 ⁇ m; and b) subjecting the powder mixture obtained in step (a) to high- energy ball milling to uniformly disperse the nucleation particles within the ductile material, thereby obtaining particles formed of a matrix of the ductile material, in which are uniformly dispersed the nucleation particles.
  • Typical examples of ductile material include aluminum, magnesium and zinc. Aluminum and magnesium are preferred.
  • the particles of ductile material have an average particle size of 0.05 to 5 mm.
  • the nucleation particles preferably have an average particle size of 0.1 to 2 ⁇ m, more preferably between 0.1 and 0.5 ⁇ m. It is also possible to use a ductile material comprising an alloy selected from the group consisting of aluminum-based alloys, magnesium-based alloys and zinc-based alloys.
  • nucleation particles of the desired size can be obtained by subjecting coarse particles of the aforesaid element or compound having an average particle size greater than 0.05 ⁇ m to a preliminary high-energy ball milling to reduce the size of the coarse particles of the element or compound to a size from 0.05 to 5 ⁇ m.
  • the milling time can be adjusted.
  • the milling time generally ranges from 1 hour to 20 hours.
  • the impact forces during the ball milling of step (b) cause plastic deformations of the ductile material and during these plastic deformations the nucleation particles are trapped in the ductile material to form a composite comprising a matrix of ductile material in which the nucleation particles are uniformly dispersed.
  • the ball milling of step (b) can be carried out for a period of time ranging from 0.5 hour to 5 hours.
  • the preliminary ball milling and the milling of step (b) are carried out in a vibratory ball mill operated at a frequency of 8 to 25 Hz, preferably about 17 Hz. It is also possible to conduct these two steps in a rotary ball mill operated at a speed of 150 to 1500 r.p.m., preferably about 1000 r.p.m.
  • the preliminary ball milling and the ball milling of step (b) are carried out under an inert gas atmosphere such as a gas atmosphere comprising argon or nitrogen, in order to prevent oxidation of the grain refining agent.
  • an atmosphere of argon is preferred.
  • the grain refining agent according to the invention is in powder form, it may be difficult to handle. Consolidation is thus preferred to facilitate manipulations and also to ensure that the grain refining agent is homogeneously dispersed in the magnesium melt to be cast.
  • the powder can be compacted to form pellets, discs or bricks by uniaxial pressing, hot or cold isostatic pressing, with or without a suitable binder.
  • the powder can also be formed into a cored wire by wrapping the powder with a suitable foil which is preferably made of the same metal or alloy to be cast or of an element having a melting point lower than that of the metal or alloy to be cast.
  • a suitable foil which is preferably made of the same metal or alloy to be cast or of an element having a melting point lower than that of the metal or alloy to be cast.
  • a grain refining agent was prepared by ball milling a 70%Si- 30%C powder mixture in a hardened steel crucible, using a SPEX 8000 (trademark) vibratory ball mill operated at a frequency of 17 Hz.
  • the initial particle size of the silicon powder was -100 mesh and that of the carbon powder was 1-5 ⁇ m.
  • the operation was performed under a controlled argon atmosphere to prevent oxidization.
  • the crucible was sealed with a rubber O- ring. A milling time of 15 hours was chosen for this operation.
  • the resulting grain refining agent in powder form having an average particle size of 0.5-3 ⁇ m was mixed with an aluminum powder in a Al/refiner ratio of 4:1 and the mixture was milled for 1 hour under a controlled argon atmosphere, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz, to disperse the refiner particles within the ductile aluminum.
  • the Al/refiner composite in powder form thus obtained was then uniaxially pressed and added into a AZ91 magnesium melt to provide 250 ppm of silicon in the melt.
  • a grain refining agent was prepared by ball milling a 80%Ti- 20%C powder mixture in a hardened steel crucible, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz.
  • the initial particle size of the titanium was -100 mesh and that of the carbon powder was l-5 ⁇ m.
  • the operation was performed under a controlled argon atmosphere to prevent oxidization.
  • the crucible was sealed with a rubber 0-ring. A milling time of 5 hours was chosen for this operation.
  • the resulting grain refining agent in powder form having an average particle size of 0.5-3 ⁇ m was mixed with an aluminum powder in a Al/refiner ratio of 4:1 and the mixture was milled for 1 hour under a controlled argon atmosphere using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz, to disperse the refiner particles within the ductile aluminum.
  • the Al/refiner composite in powder form thus obtained was then uniaxially pressed and added into a AZ91 magnesium melt to provide 400 ppm of titanium in the melt.
  • a grain refining agent was prepared by ball milling a SiC powder in a tungsten carbide crucible, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz.
  • the initial particle size of the SiC powder was -100 mesh.
  • the operation was performed under a controlled argon atmosphere to prevent oxidization.
  • the crucible was sealed with a rubber O-ring. A milling time of 10 hours was chosen for this operation.
  • the resulting grain refining agent in powder form having an average particle size of 0.5-3 ⁇ m was mixed with an aluminum powder in a Al/refiner ratio of 4:1 and the mixture was milled for 1 hour under a controlled argon atmosphere, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz, to disperse the refiner particles within the ductile aluminum.
  • the Al/powder composite in powder form thus obtained was then uniaxially pressed and added into a AZ91 magnesium melt to provide 400 ppm of SiC in the melt.
  • a grain refining agent was prepared by ball milling a TiC powder in a tungsten carbide crucible, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz.
  • the initial size of the TiC powder was -325 mesh.
  • the operation was performed under argon atmosphere to prevent oxidization.
  • the crucible was sealed with a rubber O-ring. A milling time of 10 hours was chosen for this operation.
  • the resulting grain refining agent having an average particle size of 0.5-3 ⁇ m was mixed with an aluminum powder in a Al/refiner ratio of 4:1 and the mixture milled for 1 hour under a controlled argon atmosphere, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz, to disperse the refiner particles within the ductile aluminum.
  • the Al/powder composite in powder form thus obtained was then uniaxially pressed and added into a AZ91 magnesium melt to provide 400 ppm of TiC in the melt.
  • a grain refining agent was prepared by ball milling a 96 wt.% of a zirconium powder and 4 wt.% of stearic acid (lubricant) in a tungsten carbide cracible using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz.
  • the initial particle size of the zirconium powder was -100 mesh.
  • the operation was performed under a controlled argon atmosphere to prevent oxidization.
  • the cracible was sealed with a rubber O-ring. A milling time of 10 hours was chosen for this operation.
  • the resulting grain refining agent in powder form having an average particle size of 1-5 ⁇ m was mixed with a zinc powder in a Zn/refiner ratio of 9:1 and the mixture was milled for 5 hours under a controlled argon atmosphere, using a SPEX 8000 vibratory ball mill operated at a frequency of 17 Hz, to disperse the refiner particles within the ductile zinc.
  • the resulting Zn/refiner composite in powder form thus obtained was then uniaxially pressed and added into a AZ91 magnesium melt to provide 300 ppm of zirconium in the melt.

Abstract

L'invention concerne un agent d'affinage de grain pour produits coulés en magnésium, qui comprend des particules formées d'une matrice d'un corps ductile dans lequel sont dispersées uniformément des particules de nucléation d'au moins un élément ou composé sélectionné dans un groupe constitué de zircone, de carbure de silicium, de carbure de titane et de mélanges de carbone avec du silicium et du titane, les particules de nucléation ayant une taille moyenne des particules entre 0,05 et 5 µm. La dispersion des particules de nucléation à l'intérieur d'une matrice de corps ductile améliore leur mouillabilité, permet de résoudre les problèmes dus à absorption de gaz à la surface des particules et réduit leur agglomération durant l'inoculation dans du magnésium moulé ou son alliage.
PCT/CA2003/000715 2002-05-14 2003-05-14 Agent d'affinage de grain pour produits coules en magnesium WO2003095689A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003229453A AU2003229453A1 (en) 2002-05-14 2003-05-14 Grain refining agent for cast magnesium products

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA 2386334 CA2386334A1 (fr) 2002-05-14 2002-05-14 Agent d'affinage du grain pour des produits en magnesium moules
CA2,386,334 2002-05-14

Publications (1)

Publication Number Publication Date
WO2003095689A1 true WO2003095689A1 (fr) 2003-11-20

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AU (1) AU2003229453A1 (fr)
CA (1) CA2386334A1 (fr)
WO (1) WO2003095689A1 (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1611980A1 (fr) * 2004-06-28 2006-01-04 Gkss-Forschungszentrum Geesthacht Gmbh Procédé de production d'un affineur de grains pour métaux, affineur de grains et métal ou alliage métallique
WO2006120322A1 (fr) * 2005-05-06 2006-11-16 Bernard Closset Agent d’affinage de grain comportant du nitrure de titane et procede de fabrication d’un tel agent
DE102007058225A1 (de) 2007-12-03 2009-06-04 Volkswagen Ag Kornfeinungsmittel und Verfahren zum Herstellen des Kornfeinungsmittels
CN102146530A (zh) * 2011-03-15 2011-08-10 新星化工冶金材料(深圳)有限公司 镁及镁合金晶粒细化剂及其制备方法
CN102146529A (zh) * 2011-03-15 2011-08-10 新星化工冶金材料(深圳)有限公司 铝-锆-碳中间合金的制备方法
US8016957B2 (en) * 2006-02-03 2011-09-13 GM Global Technology Operations LLC Magnesium grain-refining using titanium
WO2011135289A3 (fr) * 2010-04-27 2012-04-26 Aerospace Metal Composites Limited Métal composite
EP2532763A1 (fr) * 2011-06-10 2012-12-12 Shenzhen Sun Xing Light Alloys Materials Co., Ltd. Application d'alliage intermédiaire aluminium-zirconium-titane-carbone dans un processus de déformation de magnésium et d'alliages de magnésium
CN107385252A (zh) * 2017-08-03 2017-11-24 哈尔滨工业大学 一种Ti弥散强化超细晶高强镁合金的制备方法
CN114369741A (zh) * 2022-01-04 2022-04-19 湖南化工职业技术学院（湖南工业高级技工学校） 一种Mg-3.0Zn医用镁合金的SiC孕育处理工艺

Families Citing this family (4)

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Publication number Priority date Publication date Assignee Title
CN110735057A (zh) * 2019-09-26 2020-01-31 安徽中体新材料科技有限公司 一种细化晶粒的3d打印用金属粉末的制备方法
CN112853040B (zh) * 2020-12-31 2022-05-27 东北大学 一种440c不锈轴承钢晶粒细化剂及其制备方法
CN113444909B (zh) * 2021-06-08 2022-03-04 上海航天精密机械研究所 一种用于大规格半连铸镁合金锭的晶粒细化方法
CN115229197B (zh) * 2022-07-29 2023-07-21 西北工业大学 一种使不连续增强体在高强度铝合金中均匀分散的方法

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JP2001342528A (ja) * 2000-06-01 2001-12-14 Toyota Motor Corp マグネシウム合金の細粒化剤およびその製造方法およびそれを用いた微細化方法

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CAI Y ET AL: "Nucleation phenomenon in SiC particulate reinforced magnesium composite", SCRIPTA MATERIALIA, ELSEVIER, NEW YORK, NY, US, VOL. 41, NR. 9, PAGE(S) 967-971, ISSN: 1359-6462, XP004325837 *
MA QIAN STJOHN D H ET AL: "Characteristic zirconium-rich coring structures in Mg-Zr alloys", SCRIPTA MATERIALIA, ELSEVIER, NEW YORK, NY, US, VOL. 46, NR. 9, PAGE(S) 649-654, ISSN: 1359-6462, XP004350566 *
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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1611980A1 (fr) * 2004-06-28 2006-01-04 Gkss-Forschungszentrum Geesthacht Gmbh Procédé de production d'un affineur de grains pour métaux, affineur de grains et métal ou alliage métallique
WO2006120322A1 (fr) * 2005-05-06 2006-11-16 Bernard Closset Agent d’affinage de grain comportant du nitrure de titane et procede de fabrication d’un tel agent
US8016957B2 (en) * 2006-02-03 2011-09-13 GM Global Technology Operations LLC Magnesium grain-refining using titanium
DE102007058225A1 (de) 2007-12-03 2009-06-04 Volkswagen Ag Kornfeinungsmittel und Verfahren zum Herstellen des Kornfeinungsmittels
WO2011135289A3 (fr) * 2010-04-27 2012-04-26 Aerospace Metal Composites Limited Métal composite
CN102146529A (zh) * 2011-03-15 2011-08-10 新星化工冶金材料(深圳)有限公司 铝-锆-碳中间合金的制备方法
WO2012027992A1 (fr) * 2011-03-15 2012-03-08 新星化工冶金材料(深圳)有限公司 PROCÉDÉ DE PRÉPARATION D'UN ALLIAGE-MÈRE Al-Zr-C
WO2012027990A1 (fr) * 2011-03-15 2012-03-08 新星化工冶金材料(深圳)有限公司 Produit d'affinage du grain pour magnésium ou alliage de magnésium et procédé de préparation correspondant
CN102146530A (zh) * 2011-03-15 2011-08-10 新星化工冶金材料(深圳)有限公司 镁及镁合金晶粒细化剂及其制备方法
GB2494354A (en) * 2011-03-15 2013-03-06 Shenzhen Sunxing Light Alloys Materials Co Ltd Preparation method of Al-Zr-C master alloy
GB2494352A (en) * 2011-03-15 2013-03-06 Shenzhen Sunxing Light Alloys Materials Co Ltd Grain refiner for magnesium and magnesium alloy and preparation method thereof
GB2494354B (en) * 2011-03-15 2013-05-15 Shenzhen Sunxing Light Alloys Materials Co Ltd Method for producing aluminium-zirconium-carbon intermediate alloy
GB2494352B (en) * 2011-03-15 2013-10-30 Shenzhen Sunxing Light Alloys Materials Co Ltd Grain refiner for magnesium and magnesium alloys and method for producing the same
EP2532763A1 (fr) * 2011-06-10 2012-12-12 Shenzhen Sun Xing Light Alloys Materials Co., Ltd. Application d'alliage intermédiaire aluminium-zirconium-titane-carbone dans un processus de déformation de magnésium et d'alliages de magnésium
EP2532763A4 (fr) * 2011-06-10 2014-07-02 Shenzhen Sun Xing Light Alloys Materials Co Ltd Application d'alliage intermédiaire aluminium-zirconium-titane-carbone dans un processus de déformation de magnésium et d'alliages de magnésium
CN107385252A (zh) * 2017-08-03 2017-11-24 哈尔滨工业大学 一种Ti弥散强化超细晶高强镁合金的制备方法
CN114369741A (zh) * 2022-01-04 2022-04-19 湖南化工职业技术学院（湖南工业高级技工学校） 一种Mg-3.0Zn医用镁合金的SiC孕育处理工艺

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Publication number Publication date
CA2386334A1 (fr) 2003-11-14
AU2003229453A1 (en) 2003-11-11

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