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WO1997019201A1 - Procede d'obtention d'articles composites de metal-ceramique de formes complexes - Google Patents

Procede d'obtention d'articles composites de metal-ceramique de formes complexes Download PDF

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Publication number
WO1997019201A1
WO1997019201A1 PCT/US1996/017759 US9617759W WO9719201A1 WO 1997019201 A1 WO1997019201 A1 WO 1997019201A1 US 9617759 W US9617759 W US 9617759W WO 9719201 A1 WO9719201 A1 WO 9719201A1
Authority
WO
WIPO (PCT)
Prior art keywords
ceramic
metal
shaped
metal body
article
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/US1996/017759
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English (en)
Inventor
Kevin J. Nilsen
Aleksander J. Pyzik
Jack J. Ott
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dow Chemical Co
Original Assignee
Dow Chemical Co
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 Dow Chemical Co filed Critical Dow Chemical Co
Publication of WO1997019201A1 publication Critical patent/WO1997019201A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate

Definitions

  • the invention relates to a process for the preparation of complex-shaped ceramic-metal composite articles, preferably thin, complex-shaped ceramic-metal composite articles such as computer hard disks and computer hard disk drive components
  • Ceramics are typically known as low-density materials with high hardness and stiffness, however, their b ⁇ ttleness limits their usefulness Furthermore, ceramics are typically formed by creating a densified compact that requires significant and expensive grinding to achieve a final shape, due to the large amount of shrinkage that occurs during densification of the compact Metals are typically non- brittle, non-breakable mate ⁇ als, however, they lack some of the desirable properties of the ceramics, such as high hardness and stiffness Therefore, combining a ceramic with a metal can create a composite material that exhibits the properties of a ceramic and a metal
  • U S Patent 4,605,440 discloses a method for making boron-carbide-reactive metal composites compnsing co-dispersing the boron-carbide and reactive metal powders and consolidating the co- dispersed powders into a green body and reacting the green body at temperatures of 800°C to 1400°C for varying times, such that the desired composition is produced
  • U S Patent 5,308,422 discloses a process for making ceramic-metal composites involving forming layers of ceramic mate ⁇ al, sintering the layers of ceramic material into a porous ceramic compact, and then infiltrating the porous compact with a metal by immersing the porous body in a bath of molten metal Both processes involve several costly and time-consuming processing steps, such as formation of the porous compact or green body and sintering of the compact Furthermore, sintering can cause considerable shrinkage of the final product, which is undesirable
  • U S Patent 4,834,938 discloses a method for making boron-carbide-reactive
  • the process of the invention is used to prepare ceramic-metal composite articles of complex shape comprising one or more metal phases and one or more ceramic phases
  • the process can be used to prepare thin ceramic-metal composite articles of complex shape
  • the complex-shaped articles of this invention are solid articles, wherein solid article refers to an article that has no completely internal cavities which have been defined solely by an external surface of the formed metal body
  • the solid complex articles of this invention may have areas of complex geometry such as blind holes, through holes and complex radii or curvature
  • the complex-shaped ceramic metal composite article preferably comprises at least three phases Preferably, each of the phases is present in an amount of at least 2 volume percent, based on the volume of the multi-phase ceramic-based mate ⁇ al
  • the ceramic-metal composite article preferably has a residual free metal content of 2 volume percent or greater
  • the ceramic-metal composite article preferably has a residual free metal content of 75 volume percent or less, more preferably 50 volume percent or less, and even more preferably 25 volume percent or less
  • the process of this invention
  • Preferable metals for use herein include silicon, magnesium, aluminum, titanium, vanadium, chromium, iron, copper, nickel, cobalt, tantalum, tungsten, molybdenum, zirconium, niobium or mixtures and alloys thereof More preferred metals are aluminum, silicon, titanium and magnesium or mixtures and alloys thereof Aluminum and alloys thereof are preferred because they exhibit high toughness, good electrical conductivity and machinability, and have good wettability with a chosen ceramic, such as boron carbide, for example Aluminum is best employed as an alloy which provides improved stiffness relative to pure aluminum Alloys of aluminum with one or more of Cu, Mg, Si, Mn, Cr, Zn are preferred Alloys such as AlCu, AlMg, AlSi, AlMnMg and AlCuMgCrZn and mixtures thereof are more preferred Examples of such alloys are 6061TM alloy, 7075TM alloy, and 1350TM
  • the crystalline particles may be in the shape of equiaxed grains, rods, or platelets
  • Examples of preferred ceramic-metal combinations for use in forming multi-phase ceramic metal composite articles comprises B 4 C/A1, SiC/Al, A1N/A1, TiBVAl, Al.O/Al, SiBx/Al, S1 3 N/AI, SiC/Mg, S1C/T1, SiC/Mg-Al, SiBx Ti, B C/N ⁇ , B 4 C T ⁇ , B 4 C/Cu, Al 2 0,/Mg, Al,0,/T ⁇ , TiN/Al, TiC/Al, ZrByAl, ZrC/Al, A1B, AI, A1B./A1, A1B M Q/A], A1B, 2 /T ⁇ , A1B 24 C 4 /T ⁇ , T1N/T1, T1C T1, ZrO Ti, T ⁇ B B 4 C/Al, S1C/T1B AI, T1C/M0/C0, ZrC/ZrC/ZrB2/Zr, T1
  • the mate ⁇ als forming the complex- shaped ceramic-metal composite article of the present invention are chemically reactive systems such as aluminum-boron-carbide
  • the metal component after infiltration, can be depleted to form ceramic phases that modify article properties such as hardness
  • the aluminum boron-carbide composite material includes at least one boron-carbide-containing phase and at least one aluminum-containing phase Additionally the phases may be admixed with a filler ceramic The filler provides material for the finished article that does not adversely affect the
  • the most preferred material is a multi-phase material made of B 4 C, Al, and at least three other ceramic phases, preferably, A1B, 4 C 4 , A1,BC A1 4 BC, and AIB,
  • the B 4 C grains are preferably surrounded by aluminum boride and aluminum-boron-carbide
  • the composite article has a continuous ceramic network of aluminum boron, boron carbide, and aluminum-boron-carbide
  • the starting materials used for the process of the invention depend upon the product desired
  • the metal and ceramic must be selected so as to facilitate infiltration
  • Infiltration is the process by which a metal, upon melting, forms a solid-liquid interface with a ceramic, with the metal as the liquid and the ceramic as the solid, and the metal moves into the pores of the ceramic material by capillary action
  • the wetting contact angle, as defined by Young's Equation, at which infiltration occurs is preferably less than 90 degrees, more preferably less than 45 degrees, and most preferably less than 30 degrees
  • the process of the invention involves a series of steps to be performed in order to achieve a ceramic-metal composite article of complex shape comprising one or more metal and one or more ceramic
  • the first step comprises forming the selected metal into a desired article shape This step can be accomplished by a variety of ductile metal-forming processes as discussed hereinafter
  • the ceramic material is then contacted with the surface(s) of the shaped metal body
  • the ceramic powder can be contacted with the shaped metal body by any means which
  • the selected metal is formed into the near net finished article shape
  • Any metal-forming process or processes may be used which allows the formation of complex-shaped parts at or near net size and shape
  • Such metal-forming processes are well known in the art, for example, casting, molding, spinning, extrusion, drawing, forging, powder metallurgy, stamping, punching, rolling, mechanical machining and chemical machining
  • Preferred metal forming processes include those that form thin metal sheet, shapes from said sheet, and complex thin walled shapes (for example, tubes) Examples of said preferred processes include spinning, extrusion, stamping, punching, rolling and chemical machining
  • the shaped metal body is formed from a thin metal sheet, wherein the thin sheet is a sheet that is less than 6 mm thick, preferably less than 2 mm. more preferably less than 1 mm, and even more preferably less than 0 5 mm thick
  • the metal sheet is formed by a flat rolling process
  • Flat rolling to form a metal sheet is a process which reduces the thickness of a long piece of metal by compressive forces applied through a set of rolls
  • Rolling processes can also form, for example, seamless tubes and rings having a complex cross-sectional geometry
  • the metal sheet can also be formed into more complex shapes by any number of metal-forming processes such as stamping, drawing, chemical machining, spinning, punching and combinations thereof
  • stamping imparts the desired end geometry to the article by shearing and compressing a metal blank (that is metal sheet) in a die and then removing said part from the die
  • stamping imparts the desired end geometry to the article by shearing and compressing a metal blank (that is metal sheet) in a die and
  • the metal Before contacting the shaped metal body with a ceramic, the metal may be cleaned using well-known methods such as solvent, emulsion, alkaline, acid, pickling, ultrasonic, or plasma cleaning, each being described by Handbook of Tnbologv Material. Coatings and Surface Treatments. B Bhushan and B K Gupta, 1991
  • the next step of the process involves contacting the ceramic powder with the shaped metal body in order to form a layer of the ceramic material on the surface(s) of the shaped metal body
  • the ceramic powder can be contacted with the shaped metal body by any means which results in the formation of a layer of the ceramic material on the surface(s) of the shaped metal body, such as thermal spraying (for example, plasma spraying), atomized liquid spraying, dipping, spinning, brushing, rolling, padding, screening (for example, screen printing), soluble gel coating electrostatic spraying, electrophoretic depositing, casting (tape casting) and combinations thereof See, for example, Principles of Ceramic Processing. James Reed, 1988, or Handbook of Tnbologv. Mate ⁇ als. Coatings and Surface Treatments.
  • the layer can be a continuous layer or a layer can be deposited in a pattern on a metal body Patterns may be formed by a screen printing or a masking technique
  • more than one layer of ceramic material may be used to form the ceramic-metal composite article, or more than one ceramic may be used in a single layer
  • the ceramic powder is blended with a solvent into a slurry mixture in order to improve its ability to be contacted with the surface of the shaped metal body
  • the ceramic slurry comprises a liquid solvent, a binder, plasticizer, dispersant and the ceramic powder
  • Preferable solvents are water, alcohols and hydrocarbons
  • Preferable binders are wax, resin, gums, polyethylene, latex, acrylics, lanolin, polypropylene, polystyrene, and other thermoplastic polymers
  • Preferable plasticizers are glycols, low molecular weight polymers (for example, liquid at room temperature), oils, fats, and soaps
  • Preferable dispersants are nonionic dispersants such as ethoxylated nonylphenol, anionic dispersants such as magnesium stearate, cationic dispersants such as dodecylaminc hydrochloride, and ampholytic dispersants such as dodecyl betaine After mill
  • the contacting of the ceramic with the shaped metal body is performed by atomized liquid spraying (spraying), tape casting, or screen printing the ceramic material in a layer onto the surface of the shaped metal body See, for example, James Reed, Principles of Ceramic Processing.
  • a more preferred method of contacting the ceramic with the shaped metal body involves the use of spraying Spraying typically involves an atomizer with a spray chamber having an inert atmosphere After the ceramic powder slurry previously desc ⁇ bed is atomized during the spray deposition process, it is evenly deposited on the shaped metal body Spraying involves the controlled atomization of a slurry and the directed flow of the atomized droplets onto the surface of the shaped metal body On impact with the surface of the shaped metal body, the droplets deform and coalesce into a thick layer The slurry is dried slowly to prevent cracking of the ceramic layer and the drying temperature is controlled below the flash point of the chosen solvent system The time of drying vanes depending upon the solvent used and the thickness of the layer of the ceramic on the shaped metal body It may be necessary to debinder the ceramic material which can be done by any conventional debinde ⁇ ng technique, for example, by heating under a vacuum or in an inert atmosphere
  • the thickness of the sprayed Iayer is dependent on the spray geometry, solids content of the slurry, working distance, spraying time or sequence, rebound loss, and film flow Spraying generally results in uniformity of the layering of the ceramic upon the metal
  • the layer thickness generally is any thickness which is sufficient to provide a uniform layer on the surface of the formed metal body such that a complete contacting between the selected ceramic and the selected metal is achieved
  • the layer thickness is dependent on the amount of metal and layer porosity
  • the prefened layer thickness is 1 particle diameter or greater, more preferably 10 particle diameters or greater, and even more preferably 25 particle diameters or greater
  • the preferred layer thickness is 2 mm or less, more prefened 1 mm or less, and even more preferred 0 25 mm or less
  • Another method of contacting the ceramic powder slurry with a shaped metal body is by tape casting, which allows the formation of a film of controlled thickness of the ceramic material
  • Tape casting provides ceramic substrates with relatively smooth surfaces that are thin, flat and uniform Du ⁇ ng tape casting, the ceramic powder sluny previously described is tape cast in a layer on the surface of a shaped metal body
  • Tape casting is a process of forming a film of controlled thickness when a slurry flows down an inclined substrate or under a blade onto a supporting surface
  • screen printing could also be used to impart some geometry or texturing of the ceramic layer on the surface of the shaped metal body, thus further defining the geometry of the composite body
  • a printing screen is utilized to impart the desired ceramic pattern upon the shaped metal body during screen printing, and the printed image is dried Screen p ⁇ ntmg processes are further described in greater detail in Kosloff, Screen Printing Techniques. Signs of the Times Publishing Co , Cincinnati, Ohio, 1981
  • the third step in the process involves infiltrating the ceramic mate ⁇ al with the metal of the shaped metal body such that a shaped ceramic-metal composite article is formed
  • Infiltration is the process by which a metal, upon melting, forms a solid-liquid interface with a ceramic, with the metal as the liquid and the ceramic as the solid, and the metal moves into the pores of the ceramic mate ⁇ al by capillary action
  • This process preferably forms a uniformly dispersed and fully dense ceramic-metal composite mate ⁇ al Infiltration can be performed by any method that is known in the industry, for example, U S
  • the infiltration time for a metal selected from the preferred class of metals and a ceramic selected from the prefened class of ceramics is 0 1 hour or greater, more preferably 0 5 hour or greater, and even more preferably 1 hour or greater
  • the infiltration time for a metal selected from the preferred class of metals and a ceramic selected from the prefened class of ceramics is 24 hours or less, more preferably 12 hours or less, and even more preferably 6 hours or less
  • the preferred time for infiltration of aluminum into a 1 mm thick layer of boron carbide at 1100°C is 10 minutes
  • Infiltration can be accomplished at atmospheric pressure, subatmosphe ⁇ c pressures or superatmosp
  • heat treatment may be optionally performed on the ceramic-metal composite article in order to further tailor mechanical properties of the article
  • a preferred method of alte ⁇ ng the microstructure of already infiltrated ceramic-metal composites involves post-infiltration heat treatments of the previously infiltrated composites
  • the mechanical properties that can be tailored include fracture toughness, fracture strength, and hardness
  • This additional step of heating the ceramic metal composite article at a selected temperature for a selected amount of time will decrease the amount of residual free metal and improve the uniformity of the multi-phase ceramic-based material
  • the temperature at which the heat treatment is performed is a temperature at which the residual free metal will decrease
  • the temperature at which the heat treatment is performed is the lowest temperature at which chemical reactions in the solid state are taking place
  • the infiltrated metal may be machined and polished into a final desired shape It may be desirable to polish the infiltrated article depending upon the end usage for the infiltrated article
  • the desired article is a computer hard disk
  • the surface of the disk should be polished to a substantially uniform average roughness value of between 1 and 2000 A ( 1 x 10 '°m and 2 10 7 m)
  • a coating may be applied to the disk in order to impart texture to the surface of the composite article
  • a suitable coating for example, is a nickel-phosphorus coating, however, other types of coatings can be used such as, for example, metals and polymers If a nickel- phosphorus coating is used on an article such as a computer hard disk, the current industry procedures for manufacturing and utilizing disks may be used
  • the coating method may be any that provides dense coating, such as atomic deposition, particulate deposition, bulk coating, or surface modification
  • the paint on an aluminum beverage can was removed by sand-blasting
  • a fine boron-carbide powder having an average particle size of 3 microns (3 x 10 ' mm) was dispersed by ultrasonic agitation in methanol, creating a slurry containing 25 volume percent of said powder in methanol
  • the boron- carbide powder was deposited on the can by spraying the slurry onto the outer surfaces of the can and treating the can at 45°C for 26 hours in air After said treatment, the can had a d ⁇ ed coating of boron- carbide powder on the surface of the can
  • the boron-carbide powder coating the can was infiltrated by the aluminum of the can by heating the can coated with boron-carbide in a graphite vacuum furnace to 1150°C for 15 minutes at a heating rate of 10°C/m ⁇ nute and under a vacuum of less than 1 Torr ( 133 Pa)
  • the can was cooled by shutting off the power to the furnace The

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

L'invention porte sur un procédé de préparation d'articles composites de céramique-métal de formes pleines, mais complexes consistant: a) former un corps métallique usiné, b) à mettre en contact ledit corps avec un matériau céramique pour former un revêtement céramique sur une ou plusieurs de ses surfaces, c) à inflitrer le matériau céramique avec le métal du corps de manière à produire un articles composite de céramique-métal de formes pleines comportant une ou plusieurs phases métalliques et une ou plusieurs phases céramiques et dont la forme est sensiblement celle du corps métallique de départ.
PCT/US1996/017759 1995-11-21 1996-11-06 Procede d'obtention d'articles composites de metal-ceramique de formes complexes Ceased WO1997019201A1 (fr)

Applications Claiming Priority (2)

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US56223395A 1995-11-21 1995-11-21
US08/562,233 1995-11-21

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WO1997019201A1 true WO1997019201A1 (fr) 1997-05-29

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2896166A1 (fr) * 2006-01-18 2007-07-20 Didier Pierre Rene Dages Protheses metalliques allegees, avec revetements biocompathibles, pour la chirurgie orthopedique
WO2013032626A3 (fr) * 2011-08-31 2013-07-11 TDY Industries, LLC Procédés de formation de couches résistantes à l'usure sur des surfaces métalliques
US8637127B2 (en) 2005-06-27 2014-01-28 Kennametal Inc. Composite article with coolant channels and tool fabrication method
US8697258B2 (en) 2006-10-25 2014-04-15 Kennametal Inc. Articles having improved resistance to thermal cracking
US8790439B2 (en) 2008-06-02 2014-07-29 Kennametal Inc. Composite sintered powder metal articles
US9016406B2 (en) 2011-09-22 2015-04-28 Kennametal Inc. Cutting inserts for earth-boring bits

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4834938A (en) * 1988-04-25 1989-05-30 The Dow Chemical Company Method for making composite articles that include complex internal geometry
WO1991017280A1 (fr) * 1990-05-09 1991-11-14 Lanxide Technology Company, Lp Composites minces a matrice metallique et leurs procedes de production

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4834938A (en) * 1988-04-25 1989-05-30 The Dow Chemical Company Method for making composite articles that include complex internal geometry
WO1991017280A1 (fr) * 1990-05-09 1991-11-14 Lanxide Technology Company, Lp Composites minces a matrice metallique et leurs procedes de production

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8637127B2 (en) 2005-06-27 2014-01-28 Kennametal Inc. Composite article with coolant channels and tool fabrication method
US8808591B2 (en) 2005-06-27 2014-08-19 Kennametal Inc. Coextrusion fabrication method
FR2896166A1 (fr) * 2006-01-18 2007-07-20 Didier Pierre Rene Dages Protheses metalliques allegees, avec revetements biocompathibles, pour la chirurgie orthopedique
EP1810701A1 (fr) * 2006-01-18 2007-07-25 Didier Dages Prothèses métalliques allégées, avec revêtements biocompatibles, pour la chirurgie orthopédique
US8697258B2 (en) 2006-10-25 2014-04-15 Kennametal Inc. Articles having improved resistance to thermal cracking
US8841005B2 (en) 2006-10-25 2014-09-23 Kennametal Inc. Articles having improved resistance to thermal cracking
US8790439B2 (en) 2008-06-02 2014-07-29 Kennametal Inc. Composite sintered powder metal articles
WO2013032626A3 (fr) * 2011-08-31 2013-07-11 TDY Industries, LLC Procédés de formation de couches résistantes à l'usure sur des surfaces métalliques
CN103917692A (zh) * 2011-08-31 2014-07-09 钴碳化钨硬质合金公司 用于在金属表面上形成耐磨损层的方法
US8800848B2 (en) 2011-08-31 2014-08-12 Kennametal Inc. Methods of forming wear resistant layers on metallic surfaces
US9016406B2 (en) 2011-09-22 2015-04-28 Kennametal Inc. Cutting inserts for earth-boring bits

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