WO2004013067A2 - Poudres en suspension pour formage plastique a la temperature ambiante et procedes de formage correspondants - Google Patents

Poudres en suspension pour formage plastique a la temperature ambiante et procedes de formage correspondants Download PDF

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Publication number
WO2004013067A2
WO2004013067A2 PCT/SI2003/000026 SI0300026W WO2004013067A2 WO 2004013067 A2 WO2004013067 A2 WO 2004013067A2 SI 0300026 W SI0300026 W SI 0300026W WO 2004013067 A2 WO2004013067 A2 WO 2004013067A2
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Prior art keywords
suspensions
forming
compacts
suspension
room temperature
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PCT/SI2003/000026
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English (en)
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WO2004013067A3 (fr
Inventor
Ales Dakskobler
Tomaz Kosmac
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Institut Jozef Stefan
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Priority to AU2003254988A priority Critical patent/AU2003254988A1/en
Publication of WO2004013067A2 publication Critical patent/WO2004013067A2/fr
Publication of WO2004013067A3 publication Critical patent/WO2004013067A3/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/227—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by organic binder assisted extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • B32B37/153—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is extruded and immediately laminated while in semi-molten state
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/22—Nickel or cobalt
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    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
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Definitions

  • the object of the invention is to disclose a liquid- phase suspension of ceramic and/or metal powders wherein paraffin oil is used as liquid phase, enabling plastic forming of such suspensions at room temperature, and processes for forming such suspensions which then retain the imparted shape at room temperature.
  • the technical problem overcome by the invention is plastic forming of suspensions of ceramic and/or metal powders with various processes and subsequent retaining of the desired shape at room temperature.
  • the process of preparing suspensions is very simple and the costs involved are comparable to other methods of forming ceramic or metal powders, while offering new potential for forming ceramic or metal products.
  • the capabilities fundamentally depend on the intrinsic properties of the material, reliability, on the other hand, is mainly affected by flaws imputable to the various stages of fabrication of ceramic articles.
  • One of the critical steps in the fabrication of ceramic articles is the step of forming compacts.
  • One such widely used forming process is dry pressing the powder in a die.
  • the feed powder is generally granulated and comprises between 0.5 and 10 % of organic additives which serve as binders, plasticizers and/or lubricants.
  • the main disadvantage of this process is that it is not capable of pressing large compacts, compacts with a relatively high height to base ratio, or intricately shaped compacts.
  • the extrusion method may be used for forming.
  • the main disadvantage of the process is that the compacts are limited geometrically, which is why said process is used for forming products presenting a uniform axial cross-section along their length, such as rods, pipes, or supports for catalytic converters in automobile engines.
  • a further method of forming ceramic compacts known in the art is by injection molding. This technique is commonly used for forming smaller compacts with intricate shapes. For this process an initial suspension of ceramic and/or metal powders of a suitable viscosity as to allow injection into metal molds must be provided.
  • Two processes are known in the art, depending on the pressure applied for injection: a process is called low-pressure injection molding (LPIM) if up to 0.6 mPa of pressure is applied, and high-pressure injection molding (HPIM) if the applied pressure exceeds 0,6 mPa.
  • LPIM low-pressure injection molding
  • HPIM high-pressure injection molding
  • paraffin wax is used as the liquid phase
  • high- pressure injection molding higher polymer materials are used, such as polyethylene, polypropylene or other.
  • the temperature of the suspension ranges from 60 to 80° C for LPIM and from 110 to 160° C for HPIM.
  • Another known forming technique is by tape casting thin layers.
  • This forming method involves a liquid phase comprising volatile organic liquids which contain binders and plasticizers.
  • the tapes are formed by casting the suspension onto the substrate and heating.
  • the volatile components of the liquid phase evaporate from the suspension, the solids loading in the layer increases substantially and the suspension loses its fluid characteristics.
  • the residual components of the liquid phase in the layer enable thus obtained thin layers to be readily handled.
  • the object of the invention is to provide suspensions of ceramic and/or metal powders that will allow .plastic forming by pressing, extruding, rolling, or manual forming at room temperature, with the possibility to retain the desired shape of the compacts at room temperature, and with a simple, cheap and effective preparation procedure.
  • By repeatedly rolling and stacking layers upon layers of various ceramic and/or metal powders composites with a corrugated layered and cellular structure will be fabricated.
  • Suspensions of ceramic and/or metal powders with a 35 to 65 vol. % powder content can be formed by extrusion, pressing, rolling, or manual forming at room temperature provided that they exhibit clay-like properties.
  • This requirement is met by employing a liquid phase of a novel formulation, the primary characteristic of the inventive process for preparing suspensions being that paraffin oil, which is fluid at room temperature, is the major component of the liquid phase, and that suspensions with predetermined rheological properties are obtained by adding divers paraffins having a melting point above room temperature in the range of up to 30 vol.
  • the viscoelasticity of the suspension at room temperature may be changed by changing the dosage of added paraffin (s), whereas for retaining the desired shape after forming the compacts from thus prepared suspension the articles must be cooled below the softening temperature of the liquid phase which depends on the composition thereof, or immersed in water, during which preferential adsorption of water on the surface of the ceramic and/or metal particles takes place, resulting in a high increase in the surface elasticity of the suspension and thereby enabling the shape to be retained and the compact to be handled prior to entering the next stage of article fabrication, consisting in the removal of the binder from the compacts.
  • the invention shall hereinafter be described with reference to the preferred embodiments thereof and illustrations representing:
  • Figure la Structure of plastically formed composites with a corrugated structure
  • Figure lb Structure of plastically formed composites with a cellular structure.
  • the preparation of suspensions of ceramic and/or metal powders allowing plastic forming by extrusion, rolling, pressing or manual forming, and being capable of retaining the desired shape at room temperature comprises the following steps:
  • the optimum quantity- of surface agents Prior to preparing the suspension, the optimum quantity- of surface agents must be determined for each powder.
  • An example of a surface agent that may be used in this process is stearic acid, comprising a polar head, whereby it is bound to the polar surface of particles, and a non-polar tail allowing the particles to be wetted with a non-polar liquid medium.
  • Other carboxylic acids and silanes are also known in the art that can be used as surfactants.
  • the required quantity of surfactant usually 1 % by. weight relative to the solids loading, is added, wherein ceramic and/or metal powder is subsequently dispersed.
  • Dispersion may be carried out at room temperature or above by stirring. There is no time limit to the preparation, seeing that once a homogeneous suspension has been obtained, ulterior stirring has no effect on the properties of the suspension.
  • the suspension is prepared at a higher temperature, it should subsequently be cooled to room temperature.
  • the suspension is then plastically formed at room temperature. Plastic forming may be carried out by pressing, extrusion, rolling, or manual forming.
  • Composites with layered corrugated or cellular structure are fabricated from two or more suspensions, obtained by the above-described process.
  • the final composite structure depends on the rheological properties of the prepared suspensions, which may be controlled by adding the liquid phase with divers paraffins having a melting point above room temperature in the range of up to 30 vol. %, thereby affecting T g and consequently the rheological properties ' of the suspensions.
  • thin (max. 3 mm thick) layers of single suspensions must be prepared by rolling.
  • layers are then stacked in any order (e. g. AB, ABA, BAB, ABC, ...) , whereupon the prepared layered composite is reduced in thickness by an arbitrary amount through rolling.
  • composite is then folded and rolled one more time. The process is repeated until a composite with a corrugated layered or cellular structure is obtained.
  • a suspension of alumina (A16, Alcoa, USA) with 60 vol. % of powder in paraffin oil (paraffin oil, Kemika, Republic) is prepared. Powder dispersion in the liquid medium takes place at 80° C with the aid of a three-roll mill. After preparing the suspension, the same is cooled down to room temperature. From thus obtained suspension, the desired shape of the compact is plastically formed by hand. A plate may be formed by rolling. Thus obtained compacts are then put into water for at least 1 hour, followed by the organic phase removal stage at 200° C for 2 hours, and by sintering at 1600° C for 4 hours.
  • a suspension of zirconium oxide (TZ-3Y, Tosoh, Japan) with 57 vol. % of powder in paraffin oil (paraffin oil, Kemika, Croatia) containing 5 vol. % of INA 58/62 paraffin (INA, Zagreb, Croatia) is prepared.
  • the procedure for preparing the suspension is analogous to the first embodiment. After forming, the plastically formed article is cooled in a refrigerator at 2° C for 8 hours. After removal of the organic phase the compact is sintered at 1500° C for 2 hours.
  • a suspension of alumina (A16, Alcoa, USA) with 60 vol. % of powder in paraffin oil (paraffin oil, Kemika, Republic) is prepared. Powder dispersion in the liquid medium takes place at 80° C with the aid of a three-roll mill. After preparing the suspension, the same is cooled down to room temperature. From thus obtained suspension, 1-mm-thick layers are formed by rolling. Eight such layers are stacked together in a pile and rolled to a thickness of 7.8 mm. Subsequently, the organic phase was removed, followed by sintering at 1600° C for 2 hours.
  • the two suspensions are prepared separately. Powder dispersion in the liquid medium takes place at 80° C with the aid of a three-roll mill. After preparing the suspension, the same is rolled into 1-mm-thick strata by means of a two-roll rolling device.
  • strata are then piled up in the following order: a stratum of alumina - a stratum of zirconium oxide - a stratum of alumina or zirconium oxide - a stratum of alumina - a stratum of zirconium oxide.
  • composite is then rolled from an initial thickness of 3 mm to a thickness of 1 mm.
  • prepared strata are subsequently stacked two by two and rolled once more from the initial thickness of 2 mm to a final thickness of 1 mm.
  • This procedure is repeated, whereby a transition from a layered composite structure to a layered corrugated or cellular structure takes place after a certain number of cycles, as shown in Figs. la and lb.
  • composites are then immersed in water for 1 hour at least, followed by the stage of organic phase removal at 200° C for 2 hours and sintering at 1520° C for 4 hours.
  • the suspensions are prepared according to the procedure of the first embodiment, except that the powders from which the suspensions are prepared are alumina (A16, Alcoa, USA) and nickel powder (dso ⁇ l ⁇ m, Ventron, Germany) , respectively. Both suspensions contain 60 vol. % of powder. After obtaining the suspensions and the strata, a composite with the following stratum sequence was prepared: Al 2 0 3 -Ni- A1 2 0 3 . Thus obtained composites are left in water for at least 1 hour to retain their shape.
  • suspensions, prepared by the disclosed procedure may be plastically formed at room temperature and, in addition, the shape imparted to the articles may be retained by cooling or immersing them in water. Furthermore, the suspension according to the invention are capable of forming articles with a larger volume. Additionally, suspensions in accordance with the invention enable cellular composites to be obtained by stacking layers of different structures and rolling. The process of preparing the inventive suspensions is not expensive, or technically challenging, or requiring special equipment.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Mechanical Engineering (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

Les suspensions de poudres céramiques et/ou métalliques de l'invention se caractérisent par l'emploi d'huile de paraffine en phase liquide que l'on définit comme un mélange d'hydrocarbures aliphatiques non ramifiés avec une chaîne de 9 à 18 atomes de carbone et une charge solide représentant de 35 à 65 % en volume. L'invention offre les avantages suivants: Le suspensions élaborées selon le procédé de l'invention peuvent être formées plastiquement à la température ambiante. Par ailleurs, la forme donnée aux articles peut être conservée par refroidissement ou immersion desdits articles dans l'eau. De plus, les suspensions selon l'invention conviennent pour le formage d'articles volumineux. Ces suspensions permettent également d'obtenir des composites cellulaires par empilement de couches de structures différentes et laminage. Le procédé d'obtention des suspensions selon l'invention est peu coûteux, techniquement facile et ne nécessite pas de matériel spécial.
PCT/SI2003/000026 2002-07-24 2003-07-16 Poudres en suspension pour formage plastique a la temperature ambiante et procedes de formage correspondants WO2004013067A2 (fr)

Priority Applications (1)

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AU2003254988A AU2003254988A1 (en) 2002-07-24 2003-07-16 Powder suspensions for plastic forming at room temperature and forming processes for such suspensions

Applications Claiming Priority (2)

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SI200200185A SI21266A (sl) 2002-07-24 2002-07-24 Suspenzije prahov za plastično oblikovanje pri sobni temperaturi in postopki oblikovanja te suspenzije
SIP-200200185 2002-07-24

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WO2004013067A2 true WO2004013067A2 (fr) 2004-02-12
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005102566A1 (fr) * 2004-04-21 2005-11-03 Höganäs Ab Lubrifiants pour compositions metallurgiques de poudre
US7718082B2 (en) 2004-06-23 2010-05-18 Höganäs Ab Lubricants for insulated soft magnetic iron-based powder compositions

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0404159A1 (fr) * 1989-06-22 1990-12-27 Nkk Corporation Procédé pour la coulée de poudre
EP0458774A1 (fr) * 1990-05-22 1991-11-27 BÖHLERIT G.m.b.H. & Co. KG Lopin de métal dur ou céramique et méthode et outil pour la manufacture de ceux-ci
US5397531A (en) * 1992-06-02 1995-03-14 Advanced Materials Technologies Pte Limited Injection-moldable metal feedstock and method of forming metal injection-molded article
US6008281A (en) * 1998-01-13 1999-12-28 Planet Polymer Technologies, Inc. Powder and binder systems for use in metal and ceramic powder injection molding

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0404159A1 (fr) * 1989-06-22 1990-12-27 Nkk Corporation Procédé pour la coulée de poudre
EP0458774A1 (fr) * 1990-05-22 1991-11-27 BÖHLERIT G.m.b.H. & Co. KG Lopin de métal dur ou céramique et méthode et outil pour la manufacture de ceux-ci
US5397531A (en) * 1992-06-02 1995-03-14 Advanced Materials Technologies Pte Limited Injection-moldable metal feedstock and method of forming metal injection-molded article
US6008281A (en) * 1998-01-13 1999-12-28 Planet Polymer Technologies, Inc. Powder and binder systems for use in metal and ceramic powder injection molding

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DAKSKOBLER A ET AL: "Paraffin-based process for producing layered composites with cellular microstructures" JOURNAL OF THE AMERICAN CERAMIC SOCIETY, APRIL 2002, AMERICAN CERAMIC SOC, USA, vol. 85, no. 4, pages 1013-1015, XP002266714 ISSN: 0002-7820 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005102566A1 (fr) * 2004-04-21 2005-11-03 Höganäs Ab Lubrifiants pour compositions metallurgiques de poudre
KR100852304B1 (ko) * 2004-04-21 2008-08-14 회가내스 아베 윤활제를 포함하는 철계 분말 및 성형품을 만들기 위한방법
US7758804B2 (en) 2004-04-21 2010-07-20 Höganäs Ab Method for making compacted products and iron-based powder comprising lubricant
US7871453B2 (en) 2004-04-21 2011-01-18 Höganäs Ab Coarse iron or iron-based powder composition containing specific lubricant
US7718082B2 (en) 2004-06-23 2010-05-18 Höganäs Ab Lubricants for insulated soft magnetic iron-based powder compositions

Also Published As

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SI21266A (sl) 2004-02-29
AU2003254988A1 (en) 2004-02-23
AU2003254988A8 (en) 2004-02-23
WO2004013067A3 (fr) 2004-07-15

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