WO2006076260A1 - Synthese de metaux nanostructures totalement denses, en vrac, et composites a matrice metallique - Google Patents

Synthese de metaux nanostructures totalement denses, en vrac, et composites a matrice metallique Download PDF

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Publication number
WO2006076260A1
WO2006076260A1 PCT/US2006/000598 US2006000598W WO2006076260A1 WO 2006076260 A1 WO2006076260 A1 WO 2006076260A1 US 2006000598 W US2006000598 W US 2006000598W WO 2006076260 A1 WO2006076260 A1 WO 2006076260A1
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reinforcement
metal
temperature
aluminum
powder
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PCT/US2006/000598
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English (en)
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Julie M. Schoenung
Jichun Ye
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The Regents Of The University Of California
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • 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
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. 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
    • 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
    • B22F2009/049—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by pulverising at particular temperature
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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 relates to the production of nanostructured materials through cryomilling and spark plasma sintering.
  • Nanostructured material is material with a microstructure the characteristic length of which is on the order of a few (typically 1-500) nanometers.
  • Microstructure refers to the chemical composition, the arrangement of the atoms (the atomic structure), and the size of a solid in one, two, or three dimensions.
  • Nanostructured materials have received increasing attention due to their superior physical and mechanical properties. They are used in the electronic industry, telecommunication, electrical, magnetic, structural, optical, catalytic, biomedical, drug delivery, and in consumer goods.
  • Nanostructured materials have generally been produced by ( 1 ) powder metallurgy,
  • nanostructured materials are commonly made via mechanical milling of powder and subsequent consolidation of the powder into bulk materials.
  • contamination is unavoidable during mechanical milling, either from the processing media or atmosphere, and grain growth during consolidation can occur. Modification of these methods, however, can lead to the development of processes that are more practical. For instance, it has been reported that mechanical milling under liquid nitrogen can prevent the powders from being severely oxidized from air, and small nitride or oxy-nitride particles, which are within the size of 2-10 nm, are produced in-situ during milling.
  • These dispersoids can both strengthen the metal and enhance the thermal stability (i.e., control the grain growth) of the nanostructured materials.
  • the temperature and/or period to consolidate nanostructured powders into fully dense bulk materials can be reduced, severe grain growth can be suspended and thus the nanostructure can again be retained.
  • sol-gel solution-gelation
  • Physical or thermal processing involves the formation and collection of nanoparticles through the rapid cooling of a supersaturated vapor (gas phase condensation, U.S. Patent No. 5,128,081).
  • Thermal processes create the supersaturated vapor in a variety of ways, including laser ablation, plasma torch synthesis, combustion flame, exploding wires, spark erosion, electron beam evaporation, sputtering (ion collision), hi laser ablation, for example, a high-energy pulsed laser is focused on a target containing the material to be processed.
  • the high temperature of the resulting plasma greater than 10,000 0 K) vaporizes the material quickly allowing the process to operate at room temperature.
  • the process is capable of producing a variety of nanostructured materials on the laboratory scale, but it has the disadvantage of being extremely expensive due to the inherent energy inefficiency of lasers, and, therefore, is not suitable for industrial scale production.
  • Cryogenic milling or cryomilling is a modified mechanical milling technique where the mechanical milling is carried out at cryogenic temperatures, usually in liquid nitrogen or a similar chilled atmosphere.
  • Cryomilling has been employed to successfully fabricate nanostructured aluminum alloy powders and powders for aluminum metal matrix composites, which exhibit good thermal stability, because the cryogenic temperature retards the recovery of the aluminum. Strain is accumulated during cryomilling, leading to dislocation activity, ultimately causing the formation of nanoscaled grains within the cryomilled powder.
  • cryomilled aluminum alloys and aluminum metal matrix composite powders have nanoscaled structures with very good thermal stability. Also, cryomilling can be easily scaled up to produce tonnage quantities. Thus, cryomilling is one of the few processing approaches available for the fabrication of large quantities of nanostructured metal powders.
  • U.S. Patent No. 4,818,481 to Luton et al. discloses the use of cryomilling to disperse a second phase within an aluminum alloy where the repeated fracture and cold-welding of metal powder involved in ball milling causes strain energy to be stored within the milled particles. This strain energy is introduced through the formation of dislocations, which result in decreased grain size compared to that of the starting powders. The decreased grain size also corresponds to a dispersed secondary phase within the alloy which, in turn, results in improved mechanical properties in the finished product. Different types of oxide dispersions can be dispersed within aluminum alloys by this method.
  • the present invention provides methods for the synthesis of fully dense nanostructured materials, such as nanostructured aluminum alloys and aluminum metal matrix composites.
  • the compositions thus synthesized find use in the defense industry, aerospace industry, electronics industry, and in biotechnology and drug delivery, among others.
  • the invention provides methods for the synthesis of nanostructured materials where the starting materials are cryogenically milled and consolidated by spark plasma sintering.
  • the invention provides nanostructured aluminum alloys and aluminum metal matrix composites with improved mechanical properties, such as microhardness or strength.
  • the nanostructured aluminum alloys and aluminum metal matrix composites thus produced find use in the defense industry, aerospace industry, electronics industry, and in biotechnology and drug delivery, among others.
  • the invention provides methods for producing nanostructured materials, where the methods comprise (a) providing metal powder and optionally a reinforcement, (b) mechanically milling (a) at cryogenic temperatures to provide nanostructured powders, (c) removing gaseous components from the cryomilled powders, and (d) consolidating the cryomilled powder by spark plasma sintering.
  • the metal powder can be Al, Be, Ca, Sr, Ba, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, W, or combinations thereof, and preferably is an aluminum alloy.
  • the reinforcement can be oxides, carbides, nitrides, borides, metals, intermetallics, or alloys. Thus, the reinforcement can be boron carbide, silicon carbide, aluminum nitride, or aluminum oxide.
  • the invention provides methods for producing nanostructured aluminum alloys, the methods comprising (a) providing aluminum alloy and a reinforcement, (bj mechanically milling (a) at a temperature of about -150 °C to about -300 0 C, (c) removing gaseous components from (b), and (d) consolidating (c) by spark plasma sintering.
  • the aluminum alloy can additionally contain a metal powder such as Fe, Co, Ni, Cu, Zn, Y, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, W, or combinations thereof.
  • the reinforcement can be oxides, carbides, nitrides, borides, metals, intermetallics, or alloys.
  • the reinforcement can be boron carbide, silicon carbide, aluminum nitride, or aluminum oxide.
  • Figure 1 illustrates a bright field transmission electron microscopy (TEM) image for the bulk 5083 Al processes by cryomilling and SPS.
  • TEM transmission electron microscopy
  • Figure 2 illustrates a dark field TEM image for the bulk 5083 Al processes by cryomilling and SPS.
  • nanostructured material generally refers to a material having average grain sizes on the order of nanometers.
  • nanostructured materials may include those alloys having an average grain size of 500 nanometers (nm) or less.
  • cryomilling describes the fine milling of metallic constituents at extremely low temperatures. Cryomilling takes place within a ball mill such as an attritor with metallic or ceramic balls. During milling, the mill temperature is lowered by using liquid nitrogen, liquid argon, liquid helium, liquid neon, liquid krypton or liquid xenon. In an attritor, energy is supplied in the form of motion to the balls within the attritor, which impinge portions of the metal alloy powder within the attritor, causing repeated fracturing and welding of the metal.
  • the term “powder” or “particle” are used interchangeably and encompass oxides, carbides, nitrides, borides, chalcogenides, halides, metals, intermetallics, ceramics, polymers, alloys, and combinations thereof.
  • the term includes single metal, multi- metal, and complex compositions. Further, the terms include one-dimensional materials (fibers, tubes), two-dimensional materials (platelets, films, laminates, planar), and three-dimensional materials (spheres, cones, ovals, cylindrical, cubes, monoclinic, parallelepipeds, dumbbells, hexagonal, truncated dodecahedron, irregular shaped structures, and the like).
  • nanopowders or “nanostructured powders,” are used interchangeably and refer to powders having a mean grain size less than about 500 nm, preferably less than about 250 nm, or more preferably less than about 100 nm.
  • the term "alloy" describes a solid comprising two or more elements, such as aluminum and a second metal selected from magnesium, lithium, silicon, titanium, and zirconium.
  • the alloy may contain metals such as Be, Ca, Sr, Ba, Ra, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, W, or combinations thereof.
  • the present invention discloses methods for synthesizing nanostructured materials, and compositions thereof.
  • the synthesis employs a combined processing route where cryomilling and spark plasma sintering (SPS) are used to synthesize and consolidate nanostructured materials.
  • SPS spark plasma sintering
  • the methods of the invention have the advantage of having shorter consolidation time and lower consolidation temperature.
  • the inventive methods do not require the use of high pressure gases, such as high pressure argon that is normally required by the existing methods, e.g. HIP.
  • the inventive methods allow for suspending severe grain growth and maintaining the nanostructure due to the lower consolidation temperature and shorter consolidation time.
  • the inventive methods do not require secondary consolidation steps, e.g.
  • the sintering occurs in vacuum in the presence of a strong reducing agent, e.g., the graphite that is used as the film and die.
  • a strong reducing agent e.g., the graphite that is used as the film and die.
  • the consolidation of the nanostructured material to foil density does not require a degassing step, and the consolidated materials have good thermal stability, i.e., grains remain in the nanometer scale even after consolidation and use.
  • the SPS sample contains two distinct regions with different grain sizes. The small (nano) sized grains contribute to high strength, while the large (submicron) sized grains enhance the ductility of the materials.
  • the lower processing cost of SPS compensates for the higher processing cost of cryomilling, thus making the combined processing route economically feasible and scalable.
  • the methods of the present invention can be used with metals with low melting temperatures, such as Ni, Fe, Cu, and Al, and mixtures thereof, or with refractory metals, such as Ti, Nb, Mo, Ta, and W, metal matrix composites, and intermetallics.
  • the metal powder to be processed is pre-alloyed powder that can be used directly in the cryomilling process.
  • the powder to be processed is non-alloyed powder wherein two or more different metal powders are added to the cryomill, and the cryomilling process is used to mix together the metal constituents thereby alloying the metals.
  • the methods of the present invention can be used with low melting metals, such as
  • the starting metals are manipulated in a substantially oxygen free atmosphere.
  • the metal is aluminum
  • the aluminum is preferably supplied by atomizing the aluminum from an aluminum source and collecting and storing the atomized aluminum in a container under an argon or nitrogen atmosphere.
  • the inert atmosphere prevents the surface of the aluminum particles from excessive oxidation and prevents contaminants such as moisture from reacting with the raw metal powder.
  • other metals that can readily oxidize are treated in the same manner as aluminum prior to and after milling.
  • the metal for use in the invention can be selected from a Group 2A metal, such as Be or Mg, and mixtures thereof, a Group 3 A metal, such as Al, and mixtures thereof, a Group 4A metal, such Sn or Pb, and mixtures thereof, a Group V metal, such as V or Nb, and mixtures thereof, a Group VI metal including Cr, W, or Mo, and mixtures thereof, VII metal, such as, Mn, or Re, a Group VIII metal including Co, Ni, Ru, Rh, Pd, Os, Ir, Pt, and mixtures thereof, the lanthanides, such as Ce, Eu, Er, or Yb and mixtures thereof, or transition metals such as Cu, Ag, Au, Zn, Cd, Sc, Y, or La and mixtures thereof.
  • a Group 2A metal such as Be or Mg, and mixtures thereof
  • a Group 3 A metal such as Al, and mixtures thereof
  • a Group 4A metal such Sn or Pb
  • a Group V metal such
  • mixtures of metals such as bimetallics, which may be employed by the present invention include Fe — Al, Al- — Mg, Co-Cr, Co-W, Co— Mo, Ni-Cr, Ni-W, Ni-Mo, Ru-Cr, Ru-W, Ru-Mo, Rh-Cr, Rh-W, Rh- Mo, Pd-Cr, Pd-W, Pd-Mo, Ir-Cr, Ir-W, Pt-W, and Pt-Mo.
  • the metal is aluminum, iron, cobalt, nickel, titanium, copper, molybdenum, or a mixture thereof.
  • the metal or mixture of metals can be processed to obtain the desired grain size and grain size distribution.
  • elemental compositions include, but are not limited to, (a) precious metals such as platinum, palladium, gold, silver, rhodium, ruthenium and their alloys; (b) base and rare earth metals such as iron, nickel, manganese, cobalt, aluminum, copper, zinc, titanium, samarium, cerium, europium, erbium, and neodymium; (c) semi-metals such as boron, silicon, tin, indium, selenium, tellurium, and bismuth; (d) non-metals such as carbon, phosphorus, and halogens; and (e) alloys such as steel, shape memory alloys, aluminum alloys, manganese alloys, and superplastic alloys.
  • precious metals such as platinum, palladium, gold, silver, rhodium, ruthenium and their alloys
  • base and rare earth metals such as iron, nickel, manganese, cobalt, aluminum, copper, zinc, titanium, sama
  • the starting metal powder can additionally be mixed with a certain amount of reinforcement, also called ceramic composition (oxide, carbide, nitride, boride, chalcogenide), or an intermetallic composition (aluminide, suicide) or an elemental composition.
  • ceramic composition oxide, carbide, nitride, boride, chalcogenide
  • intermetallic composition aluminide, suicide
  • Ceramic composition examples include, but are not limited to (a) simple oxides such as aluminum oxide, silicon oxide, zirconium oxide, cerium oxide, yttrium oxide, bismuth oxide, titanium oxide, iron oxide, nickel oxide, zinc oxide, molybdenum oxide, manganese oxide, magnesium oxide, calcium oxide, and tin oxide; (b) multi-metal oxides such as aluminum silicon oxide, copper zinc oxide, nickel iron oxide, magnesium aluminum oxide, calcium aluminum oxide, calcium aluminum silicon oxide, indium tin oxide, yttrium zirconium oxide, calcium cerium oxide, scandium yttrium zirconium oxide, barium titanium oxide, barium iron oxide and silver copper zinc oxide; (c) carbides such as silicon carbide, boron carbide, iron carbide, titanium carbide, zirconium carbide, hafnium carbide, molybdenum carbide, and vanadium carbide; (d) nitrides such as silicon nitride, boron nitride, iron nitrid
  • the starting metal powders can be mixed with some compounds other than ceramics.
  • Such compounds may include, for instance, organometallic compounds such as metal alkoxides, as well as nitrates, carbonates, sulfates, and hydroxides. These may be in the form of a powder or a liquid.
  • the molar ratio of metals to added ceramic reinforcement is preferably 1000:1 to about 1:1, preferably about 500:1 to about 5:1, and more preferably about 100:1 to about 10:1
  • powders can be cryomilled, wherein fracturing and welding of the metal particles is carried out in a very low temperature environment.
  • the milling can be using shaker type mills, attritor mills, planetary mills, ball mills, or rotary mills.
  • the cryomilling of the metal powder takes place within an attritor.
  • the attritor is typically a cylindrical vessel filled with a large number of ceramic or metallic spherical balls.
  • a single fixed-axis shaft is disposed within the attritor vessel, and there are several radial arms extending from the shaft.
  • the arms cause the spherical balls to move about the attritor.
  • the attritor contains metal powder and the attritor is activated, portions of the metal powder are impinged between the metal balls as they move about the attritor. The force of the metal balls repeatedly impinges the metal particles and causes the metal particles to be continually fractured and welded together.
  • the milling of the powders at low temperatures imparts a high degree of plastic strain within the powder particles.
  • the repeated deformation causes a buildup of dislocation substructure within the particles.
  • the dislocations evolve into cellular networks that become high-angle grain boundaries sepa the very small grains of the metal. Grain size as small as approximately 10 " meter have observed via electron microscopy and measured by x-ray diffraction. Structures having dimensions smaller than 10 "7 meter, such as those found in the material produced at this the invented process, are commonly referred to as nanostructured.
  • an organic polymer such as polyethylene glycol, polyviny alcohol, and the like, or organic acids, such as stearic acid, ethyl acetate, ethylene bidisfc and dodecane may be added as one of the components to be milled with the metal powd addition of organic components promotes the fracturing of metal particles during millin] prevents the severe adhesion of the metal powders onto the milling media and milling tc
  • the temperature of the metal powder is preferably about -1 lower, such as about -300 °C.
  • the temperature of the metal powder is reduce using liquefied inert gases, such as liquid nitrogen (bp -196 0 C), liquid argon (bp -186 ' liquid helium (bp -269 0 C), liquid neon, liquid krypton or liquid xenon.
  • liquefied inert gases such as liquid nitrogen (bp -196 0 C), liquid argon (bp -186 ' liquid helium (bp -269 0 C), liquid neon, liquid krypton or liquid xenon.
  • liq ⁇ is a convenient way to lower the temperature of the entire cryomilling system.
  • surrounding the metal powder in liquid gases limits exposure of the metal powder to ox moisture, ha operation, the liquid gas is placed inside the attritor, in contact with the rm particles and the attritor balls.
  • a 150 liter (40 gal) attritor is preferably operated at a speed of about 100 1 rpm.
  • the amount of powder added to the attritor is dependent upon the size and numbe within the attritor vessel.
  • For a 150 liter attritor filled with 640 kg of 0.25" diameter ste up to approximately 20 kg of metal powder may be milled at any one time. Milling is c for a time sufficient to reach an equilibrium nanostructured grain size within the metal.
  • the metal alloy powder is a homogenous solid solution of al and the secondary metal, optionally having other added tertiary metal components and optionally having minor amounts of metallic precipitate interspersed within the alloy ai optionally having ceramic reinforcements interspersed within the alloy.
  • Grain structure the alloy is very stable and grain size is less than 500 nm. Depending on the alloy and ⁇ milling the average grain size is less than about 300 nm, and preferably may be lower than about 100 nm.
  • the metal alloy powder After the metal alloy powder, with the proper composition and grain structure, is produced, it is consolidated into a form that may be shaped into a useful object.
  • the consolidation may be by hot pressing (HP), hot isostatic pressing (HIP), cold isostatic pressing (CIP), or spark plasma sintering (SPS).
  • the consolidation is preferably by HIP or SPS, more preferably SPS. If consolidation is by HIP, the metal powder can be canned, degassed, and then compacted and welded. After consolidating, the solid mass of the metal may be worked and shaped. The consolidated metal can be extruded into a usable metal component, and forged if necessary. Further, there are no particular limitations concerning the conditions of the HIP treatment and can be varied.
  • the HIP treatment above may be carried out under an inert atmosphere such as of nitrogen, argon, or helium and the retention time at the treatment temperature and pressure may be in a range of from 0.5 to 3 hours, and particularly, approximately in a range of from 1 to 2 hours.
  • an inert atmosphere such as of nitrogen, argon, or helium
  • the retention time at the treatment temperature and pressure may be in a range of from 0.5 to 3 hours, and particularly, approximately in a range of from 1 to 2 hours.
  • the metal alloy is preferably consolidated by SPS .
  • the SPS system can be commercially obtained, such as Dr. Sinter 1050 apparatus (Sumitomo Coal Mining Co., Japan).
  • Dr. Sinter 1050 apparatus Suditomo Coal Mining Co., Japan.
  • a graphite die with an inner diameter of about 20 mm to about 100 mm is used. The larger inner diameter is selected for the fabrication of large pieces of bulk materials.
  • the uniaxial pressure for SPS can be applied by the top and bottom graphite punches thereby eliminating the need for high-pressure argon.
  • the alloy from cryomilling is degassed to remove the gaseous materials, including stearic acid.
  • the removal of gaseous components is preferably carried out at a temperature between about 200 °C and 600 °C, more preferably at a temperature between about 300 0 C and 500 °C. Then, the alloy in the SPS system is heated at a rate of about 10-500 °C/min and held at the sintering temperature for about 1 min to about 60 min, preferably about 2 min to about 15 min.
  • the sintering temperature is carried out at a temperature between about 40 % and 100% of the absolute melting temperature of the metal phase, preferably between about 60% and about 95% of the absolute melting temperature of the metal phase, more preferably about 80% and about 95% of the absolute melting temperature of the metal phase.
  • the sintered alloy obtained by cryomilling and SPS consolidation has a relative density with respect to the theoretical density of about 99.0% or higher, preferably about 99.6% or higher, more preferably about 99.7% or higher, and particularly preferably, about 99.8% or higher.
  • a relative density lower than 99.0% is not preferred, because the resulting alloy exhibits impaired strength and hardness at room temperature as well as at high temperatures.
  • the density of aluminum 5083 according to the present invention is preferably 2.63 g/cm 3 , and more preferably, 2.65 g/cm 3 or higher (the upper limit is the theoretical density of the resulting material). Setting the density in the above range is preferred, because the sintered materials can be sufficiently densif ⁇ ed for improving strength and hardness, while also improving abrasion resistance.
  • the alloy powder is handled in an inert atmosphere, such as a dry nitrogen or an argon atmosphere or in vacuum.
  • the inert atmosphere prevents oxidation of the surface of the alloy powder particles.
  • the inert atmosphere further prevents the introduction of moisture to the alloy and prevents other contaminants, which might be problematic in the extruded solid, from entering the powder.
  • the size and distribution of grains within the nanostructured material produced by the present invention may be verified by any suitable method.
  • One method of verification uses an X-ray diffraction pattern (XRD). XRD measurements can be performed using Cu K ⁇ radiation in a Siemens D5000 diffractometer equipped with a graphite monochromator. The grain size of the material can be calculated on the basis of the peak broadening. The methods described above may be used to produce nanostructured materials with a certain size distribution.
  • the sintered aluminum according to the present invention has an average grain size of 500 run or smaller, preferably from 1 nm to about 300 nm, more preferably, from 3 nm to about 200 nm, further preferably, from 5 nm to about 150 nm.
  • the nanostructured materials comprise grains between about 3 nm and about 10 nm in size.
  • the nanostructured materials comprise grains between about 5 nm and about 50 nm in size, hi still another embodiment, the nanostructured materials comprise grains between about 20 nm and about 40 nm in size.
  • the calculation from XRD peak broadening shows us the average grain size is 25 nm for as-cryomilled Al powders, 40 nm for degassed powders, and 44-60 nm for SPS-consolidated powders depending on the sintering parameters.
  • TEM transmission electron microscopy
  • a suitable model is the Phillips CM300 FEG TEM that is commercially available from FEI Company of Hillsboro, OR.
  • the metal nanoparticles are typically thinned to achieve a foil that is thin enough for an electron beam to pass through.
  • the TEM samples can be prepared using any of the known art procedures. For example, the powders and epoxy can be mixed to create a slurry, which can then be mounted into a stainless steel nut, sliced from a stainless steel pipe with an outside diameter of 3 mm and an inside diameter of 2 mm, to form a 3-mm diameter disk.
  • the disk can be ground and dimpled to a thickness of approximately 30 ⁇ m using a dimpler fitted with alumina grinders.
  • the particle size of the alumina grinders descend from a 3 ⁇ m grade to a 1 ⁇ m grade.
  • Further thinning perforation process can be carried out using a Gatan 600 argon ion mill at the temperature of near liquid nitrogen temperature (the extension of sample holder can be soaked in liquid nitrogen) with an angle range from 22° to 10°.
  • the TEM apparatus is then used to obtain micrographs of the particles that can be used to determine the grain size and grain size distribution of the nanostructure powder created.
  • the methods of the present invention synthesize sintered aluminum 5083 having high strength and hardness. More specifically, the sintered aluminum 5083 yields a Vicker's hardness of 100 or higher, preferably 120 or higher, and more preferably, 160 or higher.
  • the nanostructured materials of the present invention have numerous applications in industries such as, but not limited to, space shuttle and satellite components, jet aircraft components, helicopter roof control spiders and swashplates, combustion engine components, brake rotors, gear box components, missile components, armor vehicle body and components, diesel pistons, bicycle frames and components, automotive propeller shaft, corrosion sensitive applications, biomedical, sensor, electronic, telecommunications, optics, electrical, photonic, thermal, piezo, magnetic and electrochemical products.
  • industries such as, but not limited to, space shuttle and satellite components, jet aircraft components, helicopter roof control spiders and swashplates, combustion engine components, brake rotors, gear box components, missile components, armor vehicle body and components, diesel pistons, bicycle frames and components, automotive propeller shaft, corrosion sensitive applications, biomedical, sensor, electronic, telecommunications, optics, electrical, photonic, thermal, piezo, magnetic and electrochemical products.
  • B 4 C were synthesized by cryomilling and spark plasma sintering.
  • a small amount of stearic acid (0.2 wt%) was added into the milling chamber as a process control agent to prevent severe adhesion of the powders onto the chamber and milling balls.
  • the cryomilled powder was degassed at 400 °C, and loaded into a graphite die and cold pressed through the punches under a load of 2000 pounds for one minute.
  • the powder was consolidated using spark plasma sintering apparatus under vacuum.
  • the ramping time from room temperature to 350 0 C was 3 minutes.
  • the powders were then kept at 350 0 C for 3 minutes under the uniaxial sintering pressure of 80 MPa.
  • the densities of the compacts thus obtained were measured using Archimedes method.
  • the hardness at room temperature for the sintered composite was obtained by the Vicker's hardness measurement method under a load of 2.942N.
  • the density of the bulk materials is 2.64 g/cm 3 , 99.9% of the theoretical density.
  • the hardness for this bulk composite is 288.7 HV and the average grain size in the aluminum 5083 matrix is 56 nm.
  • the x-ray diffraction (XRD) pattern of sintered B 4 C reinforced aluminum composites shows that the compacts are nanostructured materials.
  • the densities of the compacts thus obtained were measured using Archimedes method.
  • the densities of the bulk materials were 2.65g/cm 3 , 100% of the theoretical density.
  • XRD, and hardness testing were used to characterize the consolidated compacts, and results showed that the hardness for this bulk composite is 233.3 HV with an average grain size of 44.8 nm in the matrix.
  • the grain size for SPS 5083 Al in the small-grained region is comparable to the Al grains in the as-cryomilled 5083 Al powders, indicating that the small grain size can be retained after consolidation by SPS.
  • Some grains in the cryomilled powders grew during SPS, forming the region containing the larger grains. These larger grains have a wide distribution in size, from 50 to 200 nm.
  • the presence of the small grains in the SPS 5083 Al contributes to the higher strength of the material, while the presence of the large grains contributes to the ductility of the material.
  • the densities of the compacts thus obtained were measured using Archimedes method.
  • the densities of the bulk materials were 2.63g/cm 3 , 99.0% of the theoretical density.
  • XRD, and hardness testing were used to characterize the consolidated compacts, and results showed that the hardness for this bulk material is 165.3 HV with an average grain size of 56.6 nm.

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  • Mechanical Engineering (AREA)
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Abstract

Selon l'invention, des alliages nanostructurés en vrac, tels que les alliages d'aluminium 5083 renforcés par 10 % en poids de B4C particulaire, sont synthétisés par cryo-boyage et frittage plasma par étincelage. Les matériaux pour l'alliage sont sélectionnés et les matériaux bruts sélectionnés sont cryo-broyés, c'est-à-dire broyés mécaniquement à des températures cryogéniques, afin de fabriquer des alliages nanostructurés à basses températures. Les poudres cryo-broyées sont ensuite dégazées et consolidées par frittage plasma par étincelage en matériaux en vrac denses. Les matériaux ainsi obtenus présentent une densité quasi-totale, tout en conservant leur nature nanocristalline. Les densités de ces comprimés ont été mesurées au moyen du principe d'Archimède. La diffraction des rayons X, la microscopie électronique à balayage, la microscopie électronique à transmission et des essais de dureté sont utilisés pour caractériser ces poudres cryo-broyées et comprimés consolidés.
PCT/US2006/000598 2005-01-10 2006-01-09 Synthese de metaux nanostructures totalement denses, en vrac, et composites a matrice metallique WO2006076260A1 (fr)

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