WO2003103879A1 - Production de composites a matrice metallique - Google Patents

Production de composites a matrice metallique Download PDF

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Publication number
WO2003103879A1
WO2003103879A1 PCT/US2003/017139 US0317139W WO03103879A1 WO 2003103879 A1 WO2003103879 A1 WO 2003103879A1 US 0317139 W US0317139 W US 0317139W WO 03103879 A1 WO03103879 A1 WO 03103879A1
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WO
WIPO (PCT)
Prior art keywords
powder
metal
die
pellets
aluminum
Prior art date
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Ceased
Application number
PCT/US2003/017139
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English (en)
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DWA Technologies Inc
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DWA Technologies Inc
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Filing date
Publication date
Application filed by DWA Technologies Inc filed Critical DWA Technologies Inc
Priority to AU2003275096A priority Critical patent/AU2003275096A1/en
Publication of WO2003103879A1 publication Critical patent/WO2003103879A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/148Agglomerating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the present invention generally relates to the field of manufacturing and producing metal alloy composite products from particulate starting materials. More particularly, the present invention relates to methods of manufacturing and producing metal alloy composite products containing reinforcement materials.. The present methods are particularly adapted for use with aluminum and aluminum alloy wrought products and their manufacture involving the use of powdered starting materials.
  • powder metallurgy has been gaining increasing attention in efforts to obtain new microstructures and improved mechanical properties in alloys of aluminum.
  • the idea has been one of consolidating a powder to form a basic workpiece, which often corresponds to the usual ingot or billet.
  • the workpiece can then be hot worked according to conventional methods to produce the desired wrought mill product, such as an extrusion, or forging or sheet.
  • the oxide film on aluminum or magnesium cannot be reduced to metal in situ.
  • the oxide film on aluminum and its alloys consists almost exclusively of aluminum and magnesium oxides and their hydrates. These aluminum or magnesium oxide films inhibit the particle-to-particle bonding necessary in forming both good compacts and final products of acceptable ductility and toughness as well as strength.
  • the formation of aluminum powder products is far more difficult and technically completely distinct from the powder metallurgy of metals with in-situ reducible oxides, such as copper, iron and their alloys.
  • a porous compact is formed by cold isostatic pressing the powder to about 70% of the theoretical density of the alloy being used.
  • the loading of the blended powder into the isostatic rubber mold is a dangerous operation that must be carried out in a controlled manner that eliminates the escape of powder that might form an explosive cloud of metal powder.
  • the compact is encapsulated in a closely- fitting aluminum-alloy container or can.
  • air is then evacuated from the can and the compact is heated to about 520degree C for about 6 to 7 hours in a high vacuum.
  • the canned compact While this temperature and vacuum continue to be maintained inside the can, the canned compact is sealed and then compressed to full density at pressures above about 140 MPa. (620 MPa is generally used.)
  • the compact is then cooled and the container is machined away to expose uncontaminated but fully consolidated billet. Removal of the container is necessary but costly step, since the container is typically formed from an alloy that is compositional different than the powder blend used to form the billet. In addition, since the container typically buckles during compaction, the final machined billet size is often greatly reduced compared to the initial diameter of the consolidated powder to insure that all of the container is removed, resulting in reduced product recovery.
  • the billet is then heated and extruded in a conventional manner to produce a wrought product or is otherwise hot worked as by forging.
  • the container may be evacuated by vacuum, back filled with a depurative gas such as dry nitrogen, and again vacuum evacuated to facilitate the overall degassing process.
  • a depurative gas such as dry nitrogen
  • the powder can be packed directly into the container, whereby the initial step of cold forming a compact is simply omitted. The hot consolidating step cannot be omitted.
  • Powder blends with greater than approximately 25 volume percent reinforcement require pressures greater than the capacity of commercial isostatic presses, 80,000 psi, for compaction to the desired "green" density of between 88 and 94 percent theoretical.
  • Billets manufactured by the cold isostatic press/sinter process with reinforcement contents at or above 25 volume percent have interconnected porosity and internally oxidize during re-heating for extrusion or other metalworking operation.
  • United States No. 5,965,829 issued to Haynes et.al. (Hereafter "Haynes") described a variation of the composite taught by Garden. In Haynes, the reinforcement is limited to boron carbide with a tight particle size distribution.
  • the body of the patent describes a cold isostatic press and vacuum sinter process that is similar to that of Carden.
  • the body of the patent further describes extrusion processes that are common to industry, that can also be applied to metal matrix composites.
  • the claims concentrate on the geometric spacing of the boron carbide and the boron- 10 isotope content of the boron carbide and the chemical composition limits for secondary elements in the boron carbide rather than the manufacturing methods.
  • Commercial cold isostatic presses are available to manufacture billets that are approximately 8 inch in diameter by 36 inch long.
  • elemental, master alloy or prealloyed metal powders and reinforcement powders, whiskers or fibers are introduced into a blender and suitably blended;
  • These processes typically also include the step of loading blended powder into a mold. Due to the nature of the operation, this powder loading operation is very difficult to seal completely and some metal powders always escape to air. This step is harmful to the operators and to environment and is inefficient. The step is also a dangerous operation for aluminum powder. The escape of aluminum powder might form an explosive cloud of aluminum powder.
  • the present invention is a novel and unique method of manufacturing and producing metal matrix composites.
  • the present invention concerns powder metallurgy and is aimed at making a billet or similar workpiece, which is suitable for being hot-worked to produce a wrought metal product.
  • the basic process of the present invention method includes the following sequential steps:
  • elemental, master alloy or prealloyed metal powders and reinforcement powders, whiskers and fibers are introduced into a commercial blender and suitably blended;
  • the billet is removed from the die for subsequent processing.
  • one of the most time consuming and dangerous procedures in the powder process method for manufacture of metal matrix composites involves the introduction of the blended powder into dies for compaction and further processing to produce billets.
  • Blended fine metal powders have very low densities, typically less than 30% of theoretical. Moving the blended powder often results in the formation of clouds of the powder in the area around the area of movement. Aluminum powder in a dust cloud condition becomes explosive with sufficient amount of aluminum particles in the air and the presence of an ignition source, such as a static electrical charge.
  • the present invention deals with the blended powder immediately after the blending operation.
  • the powder is rendered safe by being compacted into pellets that are too large to escape to air, yet small enough to be poured easily into appropriate containers.
  • moving powders from powder containers to blending machine and then to pelletizing equipment can be well sealed. Therefore, the present invention allows the manufacturing process of metal matrix composite become dustless.
  • the present invention also increases the efficient of loading blended powder to a die and make it possible to automate whole powder handling process without generating metal dust.
  • Blended powder is mechanically fed to the gap between two counter rotating rolls with pellet shaped depression in the roll surfaces.
  • the powder is compacted as the rolls rotate to the point of closest approach.
  • the compacted pellets and uncompacted powder is released on to a series of screens as the rolls rotate past the point of closest approach.
  • Pellets are separated by the screens and the powder that passes through the screens is recycled through the compacting rolls.
  • a commercial device that performs these operations Chilsonator® manufactured by the Fitzpatrick Company in Elmhurst, Illinois.
  • Example 1 is a sample of a typical prior art process.
  • Examples 2 to 5 are samples of the present invention.
  • Powder blend of 6092 aluminum is blended with boron carbide particles in a 85 volume percent aluminum 15 volume percent boron carbide composition.
  • the blended powder is transferred to a metal die arid compacted to a theoretical density of 65 percent.
  • the die is 125 mm (8 inches) in diameter and approximately 500 mm (20 inches) tall.
  • the filling of the die must be done slowly to maintain a safe working environment. This process takes approximately 4 hours to complete.
  • the die and powder is placed in a vacuum retort and heated to an elevated temperature under vacuum and pressed to greater than 97 percent theoretical density.
  • the billet is heated and extruded to a plate with an extrusion ratio of 20:1.
  • Tensile tests are conducted on samples oriented in the extrusion direction and 90 degrees from the extrusion direction. Samples are taken from the start of the extrusion, in the middle of the extrusion and at the end of the extrusion. The test data are contained in Table 1.
  • Powder blend of 6092 aluminum is blended with boron carbide particles in a 85 volume percent aluminum 15 volume percent boron carbide composition.
  • the blended powder is introduced into a mechanical device that contains roll dies that densities the powder into pellets that vary in size from approximately 3 mm to 15 mm in diameter. The particles that are smaller than 3 mm are passed through the rolls another time to produce the proper sized pellets.
  • the pellets are placed in storage drums, 55 gallon shipping drums or equivalent.
  • the pellets are introduced into a metal die and are further compacted to a density of approximately 65 to 80 percent. Add additional pellets to fill the die cavity.
  • the die and powder is placed in a vacuum retort and heated to an elevated temperature under vacuum and densified to greater than 97 percent theoretical density.
  • the billet is heated and extruded to a plate with an extrusion ratio of 20:1.
  • Tensile tests are conducted on samples oriented in the extrusion direction and 90 degrees from the extrusion direction. Samples are taken from the start of the extrusion, in the middle of the extrusion and at the end of the extrusion.
  • the test data are similar to those from the extrusion made from the standard processing, Table 1. Two important features were observed, 1, the strain at failure was not altered by the pelletized powder and 2, the fracture surface showed no evidence of the prior pelletized powder. TABLE 1
  • the pellets produced in example 2 are introduced into a rubber mold made to produce 89 mm (3.5 inch) diameter billets, the mold is sealed and evacuated and cold compacted to a theoretical density of approximately 90%.
  • the compacted "green" billet is then vacuum-sintered.
  • the sintered billet is heated to approximately 425 degrees C (800 degrees F) and extruded to a rod with a diameter of 14.3 mm (0.560 inch), the area ratio of the extrusion is 44: 1.
  • the rod is machined into tensile samples, heat treated and tested.
  • the test data is similar to that from the standard process with a small increase in strain to failure, which is attributed to the higher level of extrusion, 44: 1 verses 20: 1.
  • the fracture surfaces also show no evidence of prior pelletized powder.
  • the pellets produced in example 2 are blended with aluminum pellets prior to being introduced into the die body.
  • the die and powder is placed in a vacuum retort and heated to an elevated temperature under vacuum and densified to greater than 97 percent theoretical density.
  • the resulting billet is hot extruded to produce a material with improved impact resistance.
  • Pellets produced in example 2 are placed in a die in a layer. Pellets with other SiC contents are also produced. Pellets containing 20 volume percent SiC are added as a layer above the original 15 volume percent SiC pellet layer. Additional layers of pellets containing different amounts of SiC and aluminum alloy are added to the die. The die and powder is placed in a vacuum retort and heated to an elevated temperature under vacuum and densified to greater than 97 percent theoretical density. The resulting billet is hot extruded to produce a material with graded properties.
  • pellets containing between 15 and 40 volume percent SiC are added to produce a material with elastic modulus variations between 96 and 138 MPa (14 and 20 Msi) along with a coefficient of thermal expansion variation between 19 and 12 ppm/ C along the length of the extrusion.
  • Material with other gradient properties can also be produced by combining appropriate pellets with different reinforcement contents.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

Cette invention concerne un procédé de fabrication et de production de produits composites en alliage métallique à partir de matières de base particulaires, qui se prêtent particulièrement bien à une utilisation avec des produits semi-ouvrés en aluminium ou en alliage d'aluminium, et leur fabrication reposant sur l'emploi de matières de base en poudre. Le procédé consiste pour l'essentiel à: introduire des poudres de métal élémentaire, d'alliage-mère ou de métal pré-allié et des poudres de renforcement, des trichites et des fibres dans un mélange commercial correctement dosé; tasser la poudre mélangée sous forme de granules; introduire les granules dans une matrice et les comprimer, façonner la poudre comprimée en billettes par pressage à chaud sous vide ou par pressage isostatique à froid/frittage ; et extraction de la billette hors de la matrice avant poursuite du traitement.
PCT/US2003/017139 2002-06-10 2003-05-28 Production de composites a matrice metallique Ceased WO2003103879A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003275096A AU2003275096A1 (en) 2002-06-10 2003-05-28 Method for producing metal matrix composites

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US38778102P 2002-06-10 2002-06-10
US60/387,781 2002-06-10

Publications (1)

Publication Number Publication Date
WO2003103879A1 true WO2003103879A1 (fr) 2003-12-18

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PCT/US2003/017139 Ceased WO2003103879A1 (fr) 2002-06-10 2003-05-28 Production de composites a matrice metallique

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AU (1) AU2003275096A1 (fr)
WO (1) WO2003103879A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2882948A1 (fr) * 2005-03-14 2006-09-15 Forges De Bologne Soc Par Acti Procede ameliore de preparation de composites a matrice metallique et dispositif de mise en oeuvre d'un tel procede

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3785801A (en) * 1968-03-01 1974-01-15 Int Nickel Co Consolidated composite materials by powder metallurgy
US4097415A (en) * 1975-03-03 1978-06-27 Societe Lignes Telegraphiques Et Telephoniques Production of improved anodes for solid electrolyte capacitors
US4141719A (en) * 1977-05-31 1979-02-27 Fansteel Inc. Tantalum metal powder
GB2042376A (en) * 1979-02-28 1980-09-24 British Steel Corp Pelletising waste materials
US6248150B1 (en) * 1999-07-20 2001-06-19 Darryl Dean Amick Method for manufacturing tungsten-based materials and articles by mechanical alloying

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3785801A (en) * 1968-03-01 1974-01-15 Int Nickel Co Consolidated composite materials by powder metallurgy
US4097415A (en) * 1975-03-03 1978-06-27 Societe Lignes Telegraphiques Et Telephoniques Production of improved anodes for solid electrolyte capacitors
US4141719A (en) * 1977-05-31 1979-02-27 Fansteel Inc. Tantalum metal powder
GB2042376A (en) * 1979-02-28 1980-09-24 British Steel Corp Pelletising waste materials
US6248150B1 (en) * 1999-07-20 2001-06-19 Darryl Dean Amick Method for manufacturing tungsten-based materials and articles by mechanical alloying

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2882948A1 (fr) * 2005-03-14 2006-09-15 Forges De Bologne Soc Par Acti Procede ameliore de preparation de composites a matrice metallique et dispositif de mise en oeuvre d'un tel procede
WO2006097622A3 (fr) * 2005-03-14 2007-03-01 Bologne Forges Procede ameliore de preparation de composites a matrice metallique et dispositif de mise en œuvre d'un tel proced
US8329093B2 (en) 2005-03-14 2012-12-11 Forges De Bologne Method for preparing metal-matrix composite and device for implementing said method

Also Published As

Publication number Publication date
AU2003275096A1 (en) 2003-12-22

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