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DE4003219A1 - Verfahren zur herstellung von formulierungen aus keramischen und/oder metallischen fasern - Google Patents

Verfahren zur herstellung von formulierungen aus keramischen und/oder metallischen fasern

Info

Publication number
DE4003219A1
DE4003219A1 DE4003219A DE4003219A DE4003219A1 DE 4003219 A1 DE4003219 A1 DE 4003219A1 DE 4003219 A DE4003219 A DE 4003219A DE 4003219 A DE4003219 A DE 4003219A DE 4003219 A1 DE4003219 A1 DE 4003219A1
Authority
DE
Germany
Prior art keywords
ceramic
fibers
polyoxymethylene
boron trifluoride
binder
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.)
Withdrawn
Application number
DE4003219A
Other languages
English (en)
Inventor
Knut Dr Bittler
Maat Johan Herman Hendrik Ter
Hans-Josef Dr Sterzel
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.)
BASF SE
Original Assignee
BASF SE
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
Priority claimed from DE3935276A external-priority patent/DE3935276A1/de
Application filed by BASF SE filed Critical BASF SE
Priority to DE4003219A priority Critical patent/DE4003219A1/de
Priority to US07/596,543 priority patent/US5188782A/en
Priority to JP2279466A priority patent/JPH03146479A/ja
Publication of DE4003219A1 publication Critical patent/DE4003219A1/de
Withdrawn legal-status Critical Current

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    • 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
    • B22F3/22—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
    • B22F3/225—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 injection molding
    • 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
    • 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
    • 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
    • B22F3/002—Manufacture of articles essentially made from metallic fibres
    • 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
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • B22F3/1025—Removal of binder or filler not by heating only
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    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
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    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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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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    • C04B35/74—Ceramic products containing macroscopic reinforcing agents containing shaped metallic materials
    • C04B35/76—Fibres, filaments, whiskers, platelets, or the like
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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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • 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
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    • C04B2235/522—Oxidic
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    • C04B2235/5224—Alumina or aluminates
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  • Crystallography & Structural Chemistry (AREA)
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Description

Gegenstand des Patentes ....... (Patentanmeldung P 39 35 276.5) ist ein Verfahren zur Herstellung von Formlingen aus keramischen und/oder metal­ lischen Fasern durch Verformen eines die Fasern und ein thermoplastisches Bindemittel enthaltenden Gemisches durch Spritzgießen oder Strangpressen und Entfernen des Bindemittels, das dadurch gekennzeichnet ist, daß man als Bindemittel Polyoxymethylen verwendet und dieses nach der Verformung durch Behandeln in einer gasförmigen, säurehaltigen Atmosphäre entfernt.
Es wurde nun gefunden, daß man das Bindemittel auch dadurch entfernen kann, daß man den Polyoxymethylen enthaltenden Formkörper durch Behandeln in einer gasförmigen, Bortrifluorid enthaltenden Atmosphäre entfernt.
Wie beim Patent .. .. ... (Patentanmeldung P 39 35 276.5) angegeben, wird im einzelnen bei dem erfindungsgemäßen Verfahren so vorgegangen, daß man die keramischen oder metallischen Fasern mit dem Polyoxymethylen vermischt und bei Temperaturen oberhalb des Schmelzpunktes zu Granulaten verar­ beitet. Als Fasern kann man keramische oder metallische Fasern aus z. B. Al2O3, ZrO2, SiO2, Y2O3, Si3N4, SiC, Si, Fe, B oder Ti einsetzen. Unter Fasern werden auch Whiskers, z. B. Eisenwhiskers, verstanden. Die Fasern haben einen Durchmesser im Bereich von 0,1-50 µm. Selbstverständlich können anstelle von Fasern aus einem Material auch Fasern verschiedener Materialien eingesetzt werden. Als Polyoxymethylen setzt man sowohl Homo­ polymerisate als auch Copolymerisate mit Molmassen von 25 000 bis 75 000 ein. Unter Copolymerisaten seien z. B. die Polymerisate des Trioxans mit z. B. Ethylenoxid, 1,3-Dioxolan oder Butandiolformal verstanden, die in Mengen von z. B. 2 bis 4 Gew.-% vorliegen können.
Die zu verformenden Mischungen enthalten neben den anorganischen Fasern 30 bis 95 Vol-% Polyoxymethylen.
Zusätzlich können die Mischungen auch Netzmittel, Plastifiziermittel oder andere Hilfsmittel, die die rheologischen Eigenschaften der Mischungen bei der Verformung günstig beeinflussen, enthalten.
Die Herstellung der zu verformenden Massen erfolgt auf übliche Weise in einem Kneter oder Extruder bei Temperaturen von 150 bis 200°C. Falls erwünscht, kann die Masse abkühlen gelassen und anschließend granuliert werden.
Für die Verformung durch Spritzguß können die üblichen Schnecken- und Kolbenspritzgußmaschinen eingesetzt werden und bei Temperaturen von 175 bis 200°C und Drucken von 3000 bis 20 000 kPa in eine Form, die auf 20 bis 80°C gehalten wird, verformt werden.
Die erhaltenen Formkörper werden dann erfindungsgemäß in einer gasförmigen Bortrifluorid enthaltenden Atmosphäre zwecks Entfernung des Bindemittels behandelt. Unter gasförmigen Bortrifluorid enthaltenden Atmosphären kann sowohl reines Bortrifluorid verstanden werden, es können aber auch darunter Mischungen von Bortrifluorid mit einem Trägergas verstanden werden. Als Trägergase kommen beispielsweise Luft oder Stickstoff oder Edelgase in Betracht.
Anstelle von Bortrifluorid können selbstverständlich auch Addukte von Bortrifluorid verwendet werden, die bei den Behandlungstemperaturen reversibel und ohne Zersetzung der Komponenten wieder in die Ausgangs­ komponenten gespalten werden können. Insbesondere geeignet sind die Additionsverbindungen des Bortrifluorids mit Ethern, z. B. Dimethylether, Diethylether, Dibutylether und tert.-Dibutylmethylether.
Der Formkörper wird bei Temperaturen von 20 bis 150°C mit der BF3-haltigen Atmosphäre in Berührung gebracht. Vorzugsweise wendet man Temperaturen von 70 bis 130°C an. Von der Konzentration des BF3 im Gas und der angewandten Temperatur hängt die Behandlungsdauer ab, wobei steigende Temperatur und steigende BF3-Konzentration die Behandlungsdauer abkürzen. Bei Verwendung eines Trägergases wird dieses z. B. zunächst durch das BF3 bzw. BF3-Addukt geleitet und so beladen. Das so beladene Trägergas wird dann auf die Behandlungstemperatur gebracht, die zweckmäßig mindestens 10°C über der Beladungstemperatur liegen sollte, um eine Kondensation zu vermeiden. Nach Verlassen des Behandlungsraumes kann das BF3 aus der Gasmischung, die neben Formaldehyd, Trioxan auch weitere Zersetzungsprodukte des Polyoxy­ methylens enthält, zwecks Wiederverwendung auskondensiert werden.
Das erfindungsgemäße Verfahren hat den Vorteil, daß die Entfernung des Bindemittels bei niedrigen Temperaturen erfolgt und daß keine homogene Zersetzung stattfindet, d. h. daß die Zersetzung ausschließlich von der Grenzfläche Polymer/Gas fortschreitend nach innen verläuft und eine unerwünschte Gasentwicklung im Inneren des Formkörpers nicht stattfindet.
Somit ist eine schnelle, unbehinderte Abfuhr der Zersetzungsgase nach außen sichergestellt. Außerdem ist es möglich, die Behandlung auch weit unterhalb der Erweichungstemperatur (150°C) des Polyoxymethylens durchzuführen. Damit kann eine plastische Verformung des Formkörpers während der Binderentfernung vermieden werden und so die Maßhaltigkeit gewährleistet werden.
Ein weiterer Vorteil des erfindungsgemäßen Verfahrens ist die extrem niedrige Verfahrenstemperatur (20-150°C), bei der die Entfernung gelingt. Bei derart niedrigen Temperaturen wird man im allgemeinen auf die inerte Atmosphäre, die üblicherweise bei nichtoxidischen Fasern und Metallfasern zur Vorbeugung der Oberflächenoxidation eingesetzt wird, verzichten können.
Beispiel
Aus 200 g eines handelsüblichen Copolymerisats von Polyoxymethylen und 2,5 Gew.-% Butandiolformal, 76 g Aluminiumoxidkurzfasern der mittleren Länge 0,5 mm und 12 µm Durchmesser und 2,0 g Polyethylenglykol der Molmasse 400 g/Mol als Schmiermittel wurde mittels eines beheizten Laborkneters bei 180°C ein Granulat gefertigt, das mit einer Spritz­ gußmaschine zu Stäbchen von 6×4×50 mm verarbeitet wurde.
Der Gehalt an Fasern betrug 12 Vol-%.
Ein Stäbchen wurde bei einer Temperatur von 130°C 1 Stunde lang mit einem Gasgemisch aus 98 Vol-% Stickstoff und 2 Vol-% Bortrifluorid behandelt. Der Gewichtsverlust betrug 72,0%, im wesentlichen dem Gehalt des Polyoxymethylens entsprechend. Es fand keine Dimensionsänderung statt.

Claims (1)

  1. Verfahren zur Herstellung von Formlingen aus keramischen und/oder metallischen Fasern durch Verformen eines die Fasern und ein thermo­ plastisches Bindemittel enthaltenden Gemisches durch Spritzgießen oder Strangpressen, wobei als Bindemittel Polyoxymethylen verwendet wird und dieses nach der Verformung entfernt wird nach Patent .. .. ... (Patentanmeldung P 39 35 276.5), dadurch gekennzeichnet, daß man das Polyoxymethylen durch Behandeln des Formkörpers in einer gasförmigen, Bortrifluorid enthaltenden Atmosphäre entfernt.
DE4003219A 1989-10-24 1990-02-03 Verfahren zur herstellung von formulierungen aus keramischen und/oder metallischen fasern Withdrawn DE4003219A1 (de)

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DE4003219A DE4003219A1 (de) 1989-10-24 1990-02-03 Verfahren zur herstellung von formulierungen aus keramischen und/oder metallischen fasern
US07/596,543 US5188782A (en) 1989-10-24 1990-10-03 Production of preforms from ceramic or metallic fibers
JP2279466A JPH03146479A (ja) 1989-10-24 1990-10-19 セラミック繊維および／または金属繊維からなる成形体の製造法

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DE3935276A DE3935276A1 (de) 1989-10-24 1989-10-24 Verfahren zur herstellung von formlingen aus keramischen oder metallischen fasern
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WO1999028069A1 (de) * 1997-11-28 1999-06-10 Gkn Sinter Metals Gmbh & Co. Kg Radevormwald Presshilfsmittel zur herstellung von sinterbaren formteilen aus metallpulver

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US5380179A (en) * 1992-03-16 1995-01-10 Kawasaki Steel Corporation Binder system for use in the injection molding of sinterable powders and molding compound containing the binder system
DE4314694C1 (de) * 1993-05-04 1994-05-11 Basf Ag Verfahren zur Herstellung von Sinterformteilen
CA2133387A1 (en) * 1993-10-01 1995-04-02 Basf K&F Corporation Process for improving the debinding rate of ceramic and metal injection molded products
DE4432459A1 (de) * 1994-09-12 1996-03-14 Basf Ag Verfahren zur Herstellung mehrfarbiger Keramikformteile
DE10304611A1 (de) * 2003-02-05 2004-08-19 Basf Ag Verfahren und Vorrichtung zur Zertrennung pastöser Formmassen
FR3062336B1 (fr) 2017-02-02 2019-04-12 Safran Ceramics Procede de fabrication d'une piece en materiau composite
KR20240111775A (ko) * 2021-11-15 2024-07-17 바스프 에스이 적층 제조에 사용되는 융합 장벽 및 지지 구조용 세라믹 공급원료

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US4624812A (en) * 1983-01-21 1986-11-25 Celanese Corporation Injection moldable ceramic composition containing a polyacetal binder and process of molding
JPS60138914A (ja) * 1983-12-26 1985-07-23 Toshiba Ceramics Co Ltd 半導体拡散炉管の製造方法
US5043121A (en) * 1990-05-03 1991-08-27 Hoechst Celanese Corp. Process for removing polyacetal binder from molded ceramic greenbodies with acid gases

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999028069A1 (de) * 1997-11-28 1999-06-10 Gkn Sinter Metals Gmbh & Co. Kg Radevormwald Presshilfsmittel zur herstellung von sinterbaren formteilen aus metallpulver
US6224823B1 (en) 1997-11-28 2001-05-01 Gkn Sinter Metals Gmbh & Co. Kg Compacting auxiliary agent for producing sinterable shaped parts from a metal powder

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