WO2019145498A1 - Sintering unit and method for spark-plasma sintering - Google Patents

Sintering unit and method for spark-plasma sintering Download PDF

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Publication number
WO2019145498A1
WO2019145498A1 PCT/EP2019/051891 EP2019051891W WO2019145498A1 WO 2019145498 A1 WO2019145498 A1 WO 2019145498A1 EP 2019051891 W EP2019051891 W EP 2019051891W WO 2019145498 A1 WO2019145498 A1 WO 2019145498A1
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WO
WIPO (PCT)
Prior art keywords
sintering
chamber
sintering chamber
die
electrically conductive
Prior art date
Application number
PCT/EP2019/051891
Other languages
German (de)
French (fr)
Inventor
Hermann BÖDINGER
Roman Karmazin
Daniel Kupka
Carsten Schuh
Original Assignee
Siemens Aktiengesellschaft
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Publication of WO2019145498A1 publication Critical patent/WO2019145498A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/003Apparatus, e.g. furnaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F3/03Press-moulding apparatus therefor
    • B22F2003/033Press-moulding apparatus therefor with multiple punches working in the same direction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]

Definitions

  • the invention relates to a sintering unit for spark plasma sintering and a method for spark plasma sintering.
  • Spark plasma sintering is a powder metallurgy pro duction process for the production of workpieces from a pul deformed material.
  • the powdery material is regularly introduced into a pressing tool, a die, pressed and subjected to an electrical sintering current.
  • the Joule heating of the material due to the sintering current leads to its rapid heating and thus enables the efficient sintering of the material.
  • the electrical con tacts by means of which the sintering stream is fed into the pressing tool, cooled to prevent damage to the pressing tool and the contacts themselves.
  • the conductive material must be heated with a sufficiently high heating rate and a sufficiently spatially homogeneous temperature distribution.
  • the pressing tool should be sufficiently robust for industrial production.
  • pressing tools made of metal would certainly be sufficiently robust, but have no sufficiently high heating rate, tempera ture and corrosion resistance or sufficiently homogeneous temperature distribution.
  • the sintering unit according to the invention is used for spark plasma sintering of electrically conductive materials.
  • the erfindungsge Permitted sintering unit has a sintering chamber and a ers th and a second electrical contact, wherein the first and second contacts are arranged to direct sintering current when filling the Sin terhunt with electrically conductive material along a leading through the sintering chamber sintering flow path.
  • a heat-insulating element which forms a thermal insulator and an electrical conductor, is arranged on a section of the sintering flow path extending from the first and / or second contact to the sintering chamber.
  • thermal insulator and “electrical conductor” follow the common technical understanding of these terms.
  • a thermal insulator in the context of this invention is to be understood in particular as meaning a material which has a heat conductivity of at most 8 W / mK, preferably a material of at most 3 W / mK and ideally of at most 1 W / mK.
  • thermal insulation elements By means of a thermal insulator forming thermal insulation elements can be advantageously avoided in the sintering unit according to the invention that heat flows away from the sintering chamber in the direction of the first electrical contact. Since the heating element also forms an electrical conductor is ensures that electrical sintering current can enforce the thermal insulation element. In this way, in the inventions to the invention sintering unit sintered flow through the Sinterkam mer conductive, while the heat due to the sintering through the material evolving heat in or at least near the sintering chamber remains, so that sufficient material for sintering the material amount of heat in the sintering chamber can be reached.
  • the heat-insulating element (s) are / are designed and arranged such that the heat is reliably reliably insulated at this section of the heat-flow path.
  • the thermal insulation element closes thermally sealed with other parts of the Sinteraggre gats and / or the sintering chamber.
  • the sintering chamber is formed with a die made of or with metal.
  • the sintering chamber is formed with graphite.
  • the sintering chamber can basically be formed from or with metal, so that the life of the sintering unit according to the invention does not have to be limited as a result of the choice of material.
  • the die has a substantially cylindrical shell-shaped stared up.
  • this embodiment of the invention can be realized along the cylinder axis in a simple manner, a guide of the or the ram, so that the sintering chamber is easily pressurized.
  • the die surrounds a longitudinal axis.
  • the longitudinal axis forms a sintered flow path for the sintering stream.
  • the sintering chamber is formed with at least one or at least two pressing dies which are / are designed and / or arranged to apply force in one direction along the longitudinal axis.
  • the sintering chamber is formed with at least one press ram or the at least one press ram, wherein the at least one press ram is formed with metal.
  • the sintering unit comprises at least one separating element, which in the sintering chamber
  • the separating element preferably divides the sintering chamber into at least two sintering spaces and / or fills a region of the sintering chamber adjoining the die.
  • the separating element is a metal plate.
  • two or more workpieces can be sintered from the material by means of a sintering chamber divided by separating elements.
  • a dividing element which fills a region of the sintering chamber adjacent to the die, it is possible to effectively prevent adhesion of the material to the die.
  • the sintered workpiece can thus be removed from the die particularly easily.
  • the separating element increases the process reliability since the die is replaced by the separating element. element can be protected.
  • Wanddickenände ments of the die such as when a die must be turned to remove strike marks, be compensated, are provided in the thicker separating elements.
  • the at least one separating element has an electrical insulating layer, in particular insulating layer formed with boron nitride.
  • Purpose is moderately filled with the boron nitride coated separating element an adjacent to the die area of the sintering chamber.
  • boron nitride adhesions of material can be prevented material on the separator.
  • boron nitride forms an electrical insulator, so that the sintering flow can be effectively limited spatially to the area of the material of the sintering chamber. In this way, a FITS efficient heating of the material is guaranteed.
  • the at least one separating element is expediently formed with an electrically conductive layer, in particular with Gra fitfolie or titanium diboride.
  • the separating elements are electrically conductive, so that the separating elements allow the simultaneous production of several workpieces, at the same time not interrupt the sintering current path un, so that the sintered current path for efficient pro duction can pass through the separating elements.
  • the method according to the invention is a method for spark plasma sintering of an electrically conductive material.
  • a sintering unit is used as described above.
  • the sintering chamber of the sintering unit according to the invention is filled with an electrically conductive material.
  • a sintering flow is passed through the material along a sintering flow path passing through the sintering chamber.
  • a sintering flow path passing through the sintering chamber.
  • the sintering flow is passed through the sintering chamber while the heat developing due to the sintering flow through the material is held in or at least near the sintering chamber, so that the material is sintered in the sintering chamber.
  • the single drawing figure 1 shows a sintering unit 10 according to the invention for carrying out the method according to the invention, schematically in longitudinal section.
  • the sintering unit 10 according to the invention shown in FIG. 1 is designed for spark plasma sintering of an electrically conductive and powdery material 20.
  • the sintering unit 10 comprises in a conventional manner a pressing tool 30 comprising on the one hand a cylinder-shaped mold 40 of metal, in the illustratedariessbei play steel.
  • a pressing tool 30 comprising on the one hand a cylinder-shaped mold 40 of metal, in the illustratedariessbei play steel.
  • the pressing tool comprises a first 50 and egg NEN second punch 60, which are axially in the die 40, that is guided along the longitudinal axis 70, so that the ram 50, 60 in the axial direction to each other to be movable Lich.
  • the press punches 50, 60 delimit with the die 40 in a manner known per se a sintering chamber, in which the material 20 to be sintered by means of the press punches 50, 60 is subjected to force so that the material 20 pressed together and thus compressed.
  • the ram 50, 60 are also made of a metal, in the illustrated embodiment steel. In wide ren, not specifically illustrated embodiments, which otherwise correspond to the illustrated embodiment, the ram 50, 60 made of a different metal, for example TZM manufactured.
  • the ram 50, 60 are each at their Sinterkam mer far front side 90, 100 electrically connected to a rule electrical feed: the first ram 50 is connected to a first electrical feed contact (not explicitly shown) and the second ram 60 is with egg nem second electrical contact (not explicitly ge shows) connected.
  • First electrical feed and two ter electrical feed contact serve to initiate a flowing between the first and second feed contact sintering current, which flows in filled with electrically conductive material 20 sintering chamber in the axial direction through the sintering chamber through.
  • the longitudinal axis 70 of the cylindrical shape of the die 40 thus forms a sintering flow path, along which the sintering flow flows when the sintering chamber is filled.
  • the first press die 50 and the second press die 60 are not directly electrically contacted to the respective electrical feed contact. Rather, the sintering unit 10 has a first 110 and a second thermal insulation board 120 for electrical contact.
  • the first press ram 50 is connected to the first heat-insulating plate 110 to the first electrical feed contact and the second ram 60 is connected to the second heat-insulating plate 120 to the second electrical rule feeder contact.
  • the thermal insulation panels 110, 120 are located on each of the sintering chamber distant end face of the respective press ram 50, 60 between the sem and the respective electrical feed contact.
  • the thermal insulation panels 110, 120 are in each case designed as cylindrical flat disks which are oriented coaxially to the longitudinal axis 70 of the cylinder form of the die 40.
  • a pyrometer bore 130 is introduced, which is remote from that of the sintering chamber
  • the material 20 to be sintered is separated from the die 40 by means of steel sheets 140, which can be inserted into the die 40.
  • the steel sheets 140 are provided with an electrically insulating layer 150, for example boron nitride, by means of which adhesions of material to the steel sheet 140 can be avoided.
  • the sintering chamber is designed for the simultaneous sintering of a plurality of workpieces made of the material 20.
  • axial sections of the sintering chamber by means of steel discs 160 are spatially divided Lich, which are coated in the illustrated embodiment with a graphite foil 170, ie by means of an electrically conductive material, so that adhesions of the material to the steel discs are avoidable.
  • a layer of titanium diboride is present.
  • the method according to the invention for spark plasma sintering is carried out. leads by filling in the sintering chamber of the electrically conductive material 20, which ben by means of steel discs 160 is separated from each other at the same time to manufacture several pieces. By means of the electrical supply contacts, the sintering chamber is supplied with electrical current, so that forms along the sintering flow path 70 of the sintering stream. According to the invention teraggregat 10, the workpieces are manufactured with the invention.

Abstract

The sintering unit serves for the spark-plasma sintering of electrically conductive materials. The sintering unit has a sintering chamber and also a first contact and a second contact, wherein the first contact and the second contact are arranged for conducting sintering current along a sintering current path leading through the sintering chamber during the filling of the sintering chamber with electrically conductive material. In the sintering unit according to the invention, a heat-insulating element that forms a thermal insulator and an electrical conductor is arranged on a portion of the sintering current path running from the first contact to the sintering chamber and such an element is arranged on a portion of the sintering current path running from the second contact to the sintering chamber.

Description

Beschreibung description
Sinteraggregat und Verfahren zum Spark-Plasma-Sintern Sintering unit and method for spark plasma sintering
Die Erfindung betrifft ein Sinteraggregat zum Spark-Plasma- Sintern sowie ein Verfahren zum Spark-Plasma-Sintern. The invention relates to a sintering unit for spark plasma sintering and a method for spark plasma sintering.
Das Spark-Plasma-Sintern ist ein pulvermetallurgisches Ferti gungsverfahren zur Fertigung von Werkstücken aus einem pul verförmigen Werkstoff. Der pulverförmige Werkstoff wird dazu regelmäßig in ein Presswerkzeug, eine Matrize, eingebracht, gepresst und mit einem elektrischen Sinterstrom beaufschlagt. Spark plasma sintering is a powder metallurgy pro duction process for the production of workpieces from a pul deformed material. The powdery material is regularly introduced into a pressing tool, a die, pressed and subjected to an electrical sintering current.
Im Falle eines leitfähigen Werkstoffs führt die aufgrund des Sinterstroms entstehende Joul'sche Erwärmung des Werkstoffs zu seinem schnellen Aufheizen und ermöglicht so das effizien te Sintern des Werkstoffs. Zudem werden die elektrischen Kon takte, mittels welchen der Sinterstrom in das Presswerkzeug eingespeist wird, gekühlt, um Schäden an dem Presswerkzeug und den Kontakten selbst zu vermeiden. In the case of a conductive material, the Joule heating of the material due to the sintering current leads to its rapid heating and thus enables the efficient sintering of the material. In addition, the electrical con tacts, by means of which the sintering stream is fed into the pressing tool, cooled to prevent damage to the pressing tool and the contacts themselves.
Beim Spark-Plasma-Sintern bleiben einige Randbedingungen zu berücksichtigen: So muss einerseits der leitfähige Werkstoff mit einer hinreichend hohen Aufheizrate und einer hinreichend räumlich homogenen Temperaturverteilung erwärmt werden. Ande rerseits sollte das Presswerkzeug für eine industrielle Fer tigung hinreichend robust sein. In spark plasma sintering, a few boundary conditions must be taken into account: On the one hand, the conductive material must be heated with a sufficiently high heating rate and a sufficiently spatially homogeneous temperature distribution. On the other hand, the pressing tool should be sufficiently robust for industrial production.
Es sind Presswerkzeuge aus Graphit bekannt, welche eine hin reichend hohe Aufheizrate aufweisen. Jedoch ist die Lebens dauer von Presswerkzeugen aus Graphit häufig zu gering. There are known pressing tools made of graphite, which have a sufficiently high heating rate. However, the life of graphite press tools is often too low.
Presswerkzeuge aus Metall hingegen wären durchaus hinreichend robust, weisen aber keine genügend hohe Aufheizrate, Tempera tur- und Korrosionsbeständigkeit oder hinreichend homogene Temperaturverteilung auf. In contrast, pressing tools made of metal would certainly be sufficiently robust, but have no sufficiently high heating rate, tempera ture and corrosion resistance or sufficiently homogeneous temperature distribution.
Es ist daher Aufgabe der Erfindung, ein verbessertes Sinter aggregat zum Spark-Plasma-Sintern elektrisch leitfähiger Werkstoffe anzugeben, welches die aus dem Stand der Technik bekannten Nachteile nicht aufweist. Ferner ist es Aufgabe der Erfindung, ein verbessertes Verfahren zum Spark-Plasma- Sintern anzugeben. It is therefore an object of the invention, an improved sintering aggregate for spark plasma sintering electrically conductive Specify materials that does not have the disadvantages known from the prior art. It is another object of the invention to provide an improved method for spark plasma sintering.
Diese Aufgabe der Erfindung wird mit einem Sinteraggregat mit den in Anspruch 1 angegebenen Merkmalen sowie mit einem Ver fahren mit den in Anspruch 10 angegebenen Merkmalen gelöst. Bevorzugte Weiterbildungen der Erfindung sind in den zugehö rigen Unteransprüchen, der nachfolgenden Beschreibung und der Zeichnung angegeben. This object of the invention is achieved with a sintering unit with the features specified in claim 1 and with a United with the features specified in claim 10. Preferred embodiments of the invention are set forth in the associated dependent claims, the following description and the drawings.
Das erfindungsgemäße Sinteraggregat dient zum Spark-Plasma- Sintern elektrisch leitfähiger Werkstoffe. Das erfindungsge mäße Sinteraggregat weist eine Sinterkammer sowie einen ers ten und einen zweiten elektrischen Kontakt auf, wobei erster und zweiter Kontakt angeordnet sind, bei Befüllung der Sin terkammer mit elektrisch leitfähigem Material entlang eines durch die Sinterkammer hindurch führenden Sinterstrompfades Sinterstrom zu leiten. Dabei ist bei dem erfindungsgemäßen Sinteraggregat an einem vom ersten und/oder zweiten Kontakt zur Sinterkammer verlaufenden Abschnitt des Sinterstrompfades je ein Wärmedämmelernent angeordnet, welcher einen thermischen Isolator und einen elektrischen Leiter bildet. The sintering unit according to the invention is used for spark plasma sintering of electrically conductive materials. The erfindungsge Permitted sintering unit has a sintering chamber and a ers th and a second electrical contact, wherein the first and second contacts are arranged to direct sintering current when filling the Sin terkammer with electrically conductive material along a leading through the sintering chamber sintering flow path. In this case, in the sintering unit according to the invention, a heat-insulating element, which forms a thermal insulator and an electrical conductor, is arranged on a section of the sintering flow path extending from the first and / or second contact to the sintering chamber.
Die Begriffe „thermischer Isolator" und „elektrischer Leiter" folgen dem üblichen technischen Verständnis dieser Begriffe. Unter einem thermischen Isolator im Sinne dieser Erfindung ist insbesondere ein Material zu verstehen, welches eine Wär meleitfähigkeit von höchstens 8 W/mK aufweist, vorzugsweise ein Material von höchstens 3 W/mK und idealerweise von höchs tens 1 W/mK. The terms "thermal insulator" and "electrical conductor" follow the common technical understanding of these terms. A thermal insulator in the context of this invention is to be understood in particular as meaning a material which has a heat conductivity of at most 8 W / mK, preferably a material of at most 3 W / mK and ideally of at most 1 W / mK.
Mittels des einen thermischen Isolator bildenden Wärmedämm elements lässt sich bei dem erfindungsgemäßen Sinteraggregat vorteilhaft vermeiden, dass Wärme von der Sinterkammer in Richtung des ersten elektrischen Kontakts abfließt. Da das Wärmelement zugleich einen elektrischen Leiter bildet, ist gewährleistet, dass elektrischer Sinterstrom das Wärmedämm element durchsetzen kann. Auf diese Weise ist bei dem erfin dungsgemäßen Sinteraggregat Sinterstrom durch die Sinterkam mer leitbar, während die infolge des Sinterstroms durch den Werkstoff sich entwickelnde Wärme in oder zumindest nah der Sinterkammer verbleibt, sodass eine zur Sinterung des Werk stoffs hinreichende Wärmemenge in der Sinterkammer erreichbar ist . By means of a thermal insulator forming thermal insulation elements can be advantageously avoided in the sintering unit according to the invention that heat flows away from the sintering chamber in the direction of the first electrical contact. Since the heating element also forms an electrical conductor is ensures that electrical sintering current can enforce the thermal insulation element. In this way, in the inventions to the invention sintering unit sintered flow through the Sinterkam mer conductive, while the heat due to the sintering through the material evolving heat in or at least near the sintering chamber remains, so that sufficient material for sintering the material amount of heat in the sintering chamber can be reached.
Zweckmäßig ist/sind bei dem erfindungsgemäßen Sinteraggregat das/die Wärmedämmelernent/e derart ausgebildet und angeordnet, dass die Wärme an diesem Abschnitt des Wärmestrompfades zu verlässig gedämmt wird. Insbesondere schließt das Wärmedämm element thermisch dicht mit übrigen Teilen des Sinteraggre gats und/oder der Sinterkammer ab. Suitably, in the sintering unit according to the invention, the heat-insulating element (s) are / are designed and arranged such that the heat is reliably reliably insulated at this section of the heat-flow path. In particular, the thermal insulation element closes thermally sealed with other parts of the Sinteraggre gats and / or the sintering chamber.
In einer bevorzugten Weiterbildung des erfindungsgemäßen Sin teraggregats ist das Wärmedämmelernent mit kohlefaserverstärk tem Graphit und/oder kohlefaserverstärktem Kohlenstoff gebil det. Ein solcher kohlefaserverstärkter Graphit und/oder Koh lenstoff stellt ein kommerziell erhältliches und hinreichend gut elektrisch leitfähiges und wärmeisolierendes Material für das Wärmedämmelernent dar. In a preferred embodiment of the invention Sin teraggregats the Wärmedämmelernent is gebil det with carbon fiber reinforced graphite graphite and / or carbon fiber reinforced carbon. Such a carbon fiber-reinforced graphite and / or Koh lenstoff represents a commercially available and sufficiently well electrically conductive and heat-insulating material for the Wärmedämmelernent.
Zweckmäßig ist bei dem erfindungsgemäßen Sinteraggregat die Sinterkammer mit einer Matrize aus oder mit Metall gebildet. Vorteilhaft ist es erfindungsgemäß nicht erforderlich, dass die Sinterkammer mit Graphit gebildet ist. Vielmehr kann die Sinterkammer grundsätzlich aus oder mit Metall gebildet sein, sodass die Lebensdauer des erfindungsgemäßen Sinteraggregats nicht infolge der Materialwahl begrenzt sein muss. Zweckmäßig ist das Metall Stahl oder TZM (TZM = „Titan-Zirkon- Molybdän") . Insbesondere diese letztgenannten Materialien weisen eine deutlich längere Lebensdauer auf als herkömmliche Grafitmatrizen . Suitably, in the sintering unit according to the invention, the sintering chamber is formed with a die made of or with metal. Advantageously, it is not necessary according to the invention that the sintering chamber is formed with graphite. Rather, the sintering chamber can basically be formed from or with metal, so that the life of the sintering unit according to the invention does not have to be limited as a result of the choice of material. The metal is expediently steel or TZM (TZM = "titanium-zirconium-molybdenum") .In particular, these latter materials have a significantly longer service life than conventional graphite matrices.
Vorzugsweise weist bei dem Sinteraggregat gemäß der Erfindung die Matrize eine im Wesentlichen zylindermantelförmige Ge- stalt auf. In dieser Weiterbildung der Erfindung kann auf einfache Weise eine Führung des oder der Pressstempel entlang der Zylinderachse realisiert sein, sodass die Sinterkammer leicht druckbeaufschlagbar ist. Preferably, in the sintering unit according to the invention, the die has a substantially cylindrical shell-shaped stared up. In this embodiment of the invention can be realized along the cylinder axis in a simple manner, a guide of the or the ram, so that the sintering chamber is easily pressurized.
Geeigneterweise umgibt bei dem erfindungsgemäßen Sinteraggre gat die Matrize eine Längsachse. Zweckmäßig bildet die Längs achse einen Sinterstrompfad für den Sinterstrom. Suitably, in the Sinteraggre invention the die surrounds a longitudinal axis. Suitably, the longitudinal axis forms a sintered flow path for the sintering stream.
Bevorzugt ist bei dem erfindungsgemäßen Sinteraggregat die Sinterkammer mit mindestens einem oder mindestens zwei Press- stempel/n gebildet, welche/r zur Kraftbeaufschlagung in einer Richtung entlang der Längsachse ausgebildet und angeordnet ist/sind . Preferably, in the sintering unit according to the invention, the sintering chamber is formed with at least one or at least two pressing dies which are / are designed and / or arranged to apply force in one direction along the longitudinal axis.
In einer vorteilhaften Weiterbildung der Erfindung ist bei dem Sinteraggregat die Sinterkammer mit mindestens einem Pressstempel oder dem mindestens einen Pressstempel gebildet, wobei der mindestens eine Pressstempel mit Metall gebildet ist. Auf diese Weise lässt sich eine besonders hohe Lebens dauer der Pressstempel und folglich auch des erfindungsgemä ßen Sinteraggregats realisieren. In an advantageous development of the invention, in the sintering unit, the sintering chamber is formed with at least one press ram or the at least one press ram, wherein the at least one press ram is formed with metal. In this way, a particularly high lifetime of the press ram and consequently also of the sintering unit according to the invention can be realized.
Zweckmäßig umfasst das erfindungsgemäße Sinteraggregat min destens ein Trennelement, welches in die Sinterkammer Suitably, the sintering unit according to the invention comprises at least one separating element, which in the sintering chamber
einbringbar ist. Vorzugsweise teilt das Trennelement dabei die Sinterkammer in zumindest zwei Sinterräume auf und/oder füllt einen an die Matrize angrenzenden Bereich der Sinter kammer aus. Insbesondere ist das Trennelement eine Metall platte. Auf diese Weise können aus dem Werkstoff etwa mittels einer mittels Trennelementen aufgeteilten Sinterkammer zeit gleich zwei oder mehr Werkstücke gesintert werden. Ferner lässt sich mittels eines einen an die Matrize angrenzenden Bereich der Sinterkammer füllenden Trennelements eine Anhaf tung des Werkstoffs an der Matrize wirksam verhindern. Das gesinterte Werkstück lässt sich somit besonders leicht aus der Matrize herausnehmen. Insbesondere erhöht das Trennele ment die Prozesssicherheit, da die Matrize durch das Trenn- element geschützt werden kann. Zudem können Wanddickenände rungen der Matrize, etwa wenn eine Matrize zur Entfernung von Schlagspuren ausgedreht werden muss, ausgeglichen werden, in dem dickere Trennelemente vorgesehen werden. can be introduced. In this case, the separating element preferably divides the sintering chamber into at least two sintering spaces and / or fills a region of the sintering chamber adjoining the die. In particular, the separating element is a metal plate. In this way, two or more workpieces can be sintered from the material by means of a sintering chamber divided by separating elements. Furthermore, by means of a dividing element which fills a region of the sintering chamber adjacent to the die, it is possible to effectively prevent adhesion of the material to the die. The sintered workpiece can thus be removed from the die particularly easily. In particular, the separating element increases the process reliability since the die is replaced by the separating element. element can be protected. In addition, Wanddickenände ments of the die, such as when a die must be turned to remove strike marks, be compensated, are provided in the thicker separating elements.
Bei dem Sinteraggregat gemäß der Erfindung weist das mindes tens eine Trennelement eine elektrische Isolierschicht, ins besondere mit Bornitrid gebildete Isolierschicht, auf. Zweck mäßig ist mit dem mit Bornitrid beschichteten Trennelement ein an die Matrize angrenzender Bereich der Sinterkammer ausfüllbar. Mittels Bornitrid können Anhaftungen von Werk stoff an dem Trennelement verhindert werden. Zudem bildet Bornitrid einen elektrischen Isolator, sodass der Sinterstrom wirksam räumlich auf den Bereich des Werkstoffs der Sinter kammer begrenzt werden kann. Auf diese Weise ist eine beson ders effiziente Aufheizung des Werkstoffs gewährleistet. Im Falle eines die Sinterkammer aufteilenden mindestens einen Trennelements ist das mindestens eine Trennelement zweckmäßig mit einer elektrisch leitenden Schicht, insbesondere mit Gra fitfolie oder Titandiborid, gebildet. Auf diese Weise sind die Trennelemente elektrisch leitend ausgebildet, sodass die Trennelemente die zeitgleiche Fertigung mehrerer Werkstücke erlauben, zugleich den Sinterstrompfad allerdings nicht un terbrechen, sodass der Sinterstrompfad zur effizienten Ferti gung durch die Trennelemente hindurch treten kann. In the sintering unit according to the invention, the at least one separating element has an electrical insulating layer, in particular insulating layer formed with boron nitride. Purpose is moderately filled with the boron nitride coated separating element an adjacent to the die area of the sintering chamber. By means of boron nitride adhesions of material can be prevented material on the separator. In addition, boron nitride forms an electrical insulator, so that the sintering flow can be effectively limited spatially to the area of the material of the sintering chamber. In this way, a FITS efficient heating of the material is guaranteed. In the case of the at least one separating element dividing the sintering chamber, the at least one separating element is expediently formed with an electrically conductive layer, in particular with Gra fitfolie or titanium diboride. In this way, the separating elements are electrically conductive, so that the separating elements allow the simultaneous production of several workpieces, at the same time not interrupt the sintering current path un, so that the sintered current path for efficient pro duction can pass through the separating elements.
Das erfindungsgemäße Verfahren ist ein Verfahren zum Spark- Plasma-Sintern eines elektrisch leitfähigen Werkstoffs. Bei dem erfindungsgemäßen Verfahren wird ein Sinteraggregat wie oben beschrieben herangezogen. The method according to the invention is a method for spark plasma sintering of an electrically conductive material. In the method according to the invention, a sintering unit is used as described above.
Geeigneterweise wird bei dem erfindungsgemäßen Verfahren die Sinterkammer des erfindungsgemäßen Sinteraggregats mit einem elektrisch leitfähigen Werkstoff gefüllt. Suitably, in the method according to the invention, the sintering chamber of the sintering unit according to the invention is filled with an electrically conductive material.
Mittels des ersten und des zweiten elektrischen Kontakts wird ein Sinterstrom entlang eines durch die Sinterkammer hindurch führenden Sinterstrompfades durch den Werkstoff geleitet. Bei dem erfindungsgemäßen Verfahren wird an einem vom ersten und/oder zweiten Kontakt zur Sinterkammer verlaufenden Ab schnitt des Sinterstrompfades je ein Wärmedämmelernent heran gezogen, welcher einen thermischen Isolator und einen elekt rischen Leiter bildet. By means of the first and the second electrical contact, a sintering flow is passed through the material along a sintering flow path passing through the sintering chamber. In the method according to the invention is depending on a running from the first and / or second contact to the sintering chamber from the sintered Sinterstrompfades pulled near a Wärmedämmelernent, which forms a thermal insulator and an electrical ladder.
Auf diese Weise wird der Sinterstrom durch die Sinterkammer geleitet, während die infolge des Sinterstroms durch den Werkstoff sich entwickelnde Wärme in oder zumindest nah der Sinterkammer gehalten wird, sodass der Werkstoff in der Sin terkammer gesintert wird. In this way, the sintering flow is passed through the sintering chamber while the heat developing due to the sintering flow through the material is held in or at least near the sintering chamber, so that the material is sintered in the sintering chamber.
Nachfolgend wird die Erfindung anhand eines in der Zeichnung dargestellten Ausführungsbeispiels näher erläutert. The invention will be explained in more detail with reference to an embodiment shown in the drawing.
Die einzige Zeichnungsfigur 1 zeigt ein erfindungsgemäßes Sinteraggregat 10 zur Ausführung des erfindungsgemäßen Ver fahrens schematisch im Längsschnitt. The single drawing figure 1 shows a sintering unit 10 according to the invention for carrying out the method according to the invention, schematically in longitudinal section.
Das in Fig. 1 dargestellte erfindungsgemäße Sinteraggregat 10 ist ausgebildet zum Spark-Plasma-Sintern eines elektrisch leitfähigen und pulverförmigen Werkstoffs 20. The sintering unit 10 according to the invention shown in FIG. 1 is designed for spark plasma sintering of an electrically conductive and powdery material 20.
Das Sinteraggregat 10 umfasst in an sich bekannter Weise ein Presswerkzeug 30 umfassend zum einen eine zylindermantelför mige Matrize 40 aus Metall, im dargestellten Ausführungsbei spiel Stahl. In weiteren, nicht eigens dargestellten Ausfüh rungsbeispielen ist die Matrize 40 aus einem anderen Metall, beispielsweise TZM (TZM = Titan-Zirkon -Molybdän) gebildet. The sintering unit 10 comprises in a conventional manner a pressing tool 30 comprising on the one hand a cylinder-shaped mold 40 of metal, in the illustrated Ausführungsbei play steel. In further, not specifically illustrated Ausfüh approximately examples, the die 40 from another metal, such as TZM (TZM = titanium zirconium molybdenum) is formed.
Zum anderen umfasst das Presswerkzeug einen ersten 50 und ei nen zweiten Pressstempel 60, die in der Matrize 40 axial, d.h. entlang der Längsachse 70, geführt sind, sodass die Pressstempel 50, 60 in axialer Richtung aufeinander zu beweg lich sind. Die Pressstempel 50, 60 begrenzen mit der Matrize 40 in an sich bekannter Weise eine Sinterkammer, in welcher der zu sinternde Werkstoff 20 mittels der Pressstempel 50, 60 kraftbeaufschlagt wird, sodass der Werkstoff 20 zusammenge presst und folglich verdichtet wird. On the other hand, the pressing tool comprises a first 50 and egg NEN second punch 60, which are axially in the die 40, that is guided along the longitudinal axis 70, so that the ram 50, 60 in the axial direction to each other to be movable Lich. The press punches 50, 60 delimit with the die 40 in a manner known per se a sintering chamber, in which the material 20 to be sintered by means of the press punches 50, 60 is subjected to force so that the material 20 pressed together and thus compressed.
Die Pressstempel 50, 60 sind ebenfalls aus einem Metall, im dargestellten Ausführungsbeispiel Stahl, gefertigt. In weite ren, nicht eigens dargestellten Ausführungsbeispielen, welche im Übrigen dem dargestellten Ausführungsbeispiel entsprechen, sind die Pressstempel 50, 60 aus einem anderen Metall, bei spielsweise TZM, gefertigt. The ram 50, 60 are also made of a metal, in the illustrated embodiment steel. In wide ren, not specifically illustrated embodiments, which otherwise correspond to the illustrated embodiment, the ram 50, 60 made of a different metal, for example TZM manufactured.
Die Pressstempel 50, 60 sind jeweils an ihrer der Sinterkam mer fernen Stirnseite 90, 100 elektrisch mit einem elektri schen Speisekontakt verbunden: der erste Pressstempel 50 ist mit einem ersten elektrischen Speisekontakt (nicht explizit gezeigt) verbunden und der zweite Pressstempel 60 ist mit ei nem zweiten elektrischen Speisekontakt (nicht explizit ge zeigt) verbunden. Erster elektrischer Speisekontakt und zwei ter elektrischer Speisekontakt dienen zur Einleitung eines zwischen erstem und zweitem Speisekontakt fließenden Sinter stroms, welcher bei mit elektrisch leitfähigem Werkstoff 20 befüllter Sinterkammer in axialer Richtung durch die Sinter kammer hindurch fließt. Die Längsachse 70 der Zylinderform der Matrize 40 bildet folglich einen Sinterstrompfad aus, entlang welchem der Sinterstrom bei befüllter Sinterkammer fließt . The ram 50, 60 are each at their Sinterkam mer far front side 90, 100 electrically connected to a rule electrical feed: the first ram 50 is connected to a first electrical feed contact (not explicitly shown) and the second ram 60 is with egg nem second electrical contact (not explicitly ge shows) connected. First electrical feed and two ter electrical feed contact serve to initiate a flowing between the first and second feed contact sintering current, which flows in filled with electrically conductive material 20 sintering chamber in the axial direction through the sintering chamber through. The longitudinal axis 70 of the cylindrical shape of the die 40 thus forms a sintering flow path, along which the sintering flow flows when the sintering chamber is filled.
Der erste Pressstempel 50 und der zweite Pressstempel 60 sind nicht direkt mit dem jeweiligen elektrischen Speisekontakt elektrisch kontaktiert. Vielmehr weist das Sinteraggregat 10 eine erste 110 und eine zweite Wärmedämmplatte 120 zur elekt rischen Kontaktierung auf. Dazu ist der erste Pressstempel 50 mit der ersten Wärmedämmplatte 110 an den ersten elektrischen Speisekontakt angebunden und der zweite Pressstempel 60 ist mit der zweiten Wärmedämmplatte 120 an den zweiten elektri schen Speisekontakt angebunden. Die Wärmedämmplatten 110, 120 befinden sich dazu jeweils an der der Sinterkammer fernen Stirnseite des jeweiligen Pressstempels 50, 60 zwischen die sem und dem jeweiligen elektrischen Speisekontakt. Die Wärme- dämmplatte 110, 120 ist zur elektrischen Anbindung der Press stempel 50, 60 jeweils aus einem Material gebildet, welches einen elektrischen Leiter und zugleich einen thermischen Iso lator bildet, im dargestellten Ausführungsbeispiel ein kohle faserverstärkter Graphit und/oder Kohlenstoff (CFC = (engl.) „Carbon Fiber Composite") . Die Wärmedämmplatten 110, 120 sind jeweils als zylindrische Flachscheiben ausgebildet, welche koaxial zur Längsachse 70 der Zylinderform der Matrize 40 orientiert sind. The first press die 50 and the second press die 60 are not directly electrically contacted to the respective electrical feed contact. Rather, the sintering unit 10 has a first 110 and a second thermal insulation board 120 for electrical contact. For this purpose, the first press ram 50 is connected to the first heat-insulating plate 110 to the first electrical feed contact and the second ram 60 is connected to the second heat-insulating plate 120 to the second electrical rule feeder contact. The thermal insulation panels 110, 120 are located on each of the sintering chamber distant end face of the respective press ram 50, 60 between the sem and the respective electrical feed contact. The heat- insulation board 110, 120 is for electrical connection of the press stamp 50, 60 each formed of a material which forms an electrical conductor and at the same time a thermal Iso lator, in the illustrated embodiment, a carbon fiber reinforced graphite and / or carbon (CFC = (engl.) The thermal insulation panels 110, 120 are in each case designed as cylindrical flat disks which are oriented coaxially to the longitudinal axis 70 of the cylinder form of the die 40.
Im oberen zusammengesetzten Bauteil aus erstem Pressstempel 50 und erster Wärmedämmplatte 110 ist eine Pyrometerbohrung 130 eingebracht, welche von dem der Sinterkammer fernen In the upper composite component of the first press ram 50 and the first thermal insulation panel 110, a pyrometer bore 130 is introduced, which is remote from that of the sintering chamber
Stirnende der ersten Wärmedämmplatte 110 am ersten Pressstem pel 50 in axialer Richtung auf die Sinterkammer zu durch die Wärmedämmplatte 110 hindurch und in den Pressstempel 50 hin ein ragt. Front end of the first thermal insulation board 110 on the first Pressstem pel 50 in the axial direction of the sintering chamber to through the thermal insulation board 110 and into the ram 50 out a protrudes.
Der zu sinternde Werkstoff 20 ist von der Matrize 40 mittels Stahlblechen 140 getrennt, welche sich in die Matrize 40 ein- legen lassen. Die Stahlbleche 140 sind mit einer elektrisch isolierenden Schicht 150, beispielsweise Bornitrid, versehen, mittels welchen Anhaftungen von Werkstoff an dem Stahlblech 140 vermeidbar sind. The material 20 to be sintered is separated from the die 40 by means of steel sheets 140, which can be inserted into the die 40. The steel sheets 140 are provided with an electrically insulating layer 150, for example boron nitride, by means of which adhesions of material to the steel sheet 140 can be avoided.
Die Sinterkammer ist zur zeitgleichen Sinterung mehrerer Werkstücke aus dem Werkstoff 20 ausgebildet. Dazu sind axiale Abschnitte der Sinterkammer mittels Stahlscheiben 160 räum lich aufgeteilt, welche im dargestellten Ausführungsbeispiel mit einer Grafitfolie 170, also mittels eines elektrisch leitfähigen Materials, beschichtet sind, sodass Anhaftungen des Werkstoffs an den Stahlscheiben vermeidbar sind. In wei teren Ausführungsbeispielen, welche im Übrigen dem darge stellten Ausführungsbeispiel entsprechen, ist anstelle einer Grafitfolie eine Schicht aus Titandiborid vorhanden. The sintering chamber is designed for the simultaneous sintering of a plurality of workpieces made of the material 20. For this axial sections of the sintering chamber by means of steel discs 160 are spatially divided Lich, which are coated in the illustrated embodiment with a graphite foil 170, ie by means of an electrically conductive material, so that adhesions of the material to the steel discs are avoidable. In white direct embodiments, which, moreover, the Darge presented embodiment correspond, instead of a graphite foil, a layer of titanium diboride is present.
Mittels des erfindungsgemäßen Sinteraggregats 10 wird das er findungsgemäße Verfahren zum Spark-Plasma-Sintern durchge- führt, indem in die Sinterkammer der elektrisch leitfähige Werkstoff 20 eingefüllt wird, welcher mittels der Stahlschei ben 160 voneinander getrennt wird um zeitgleich mehrere Werk stücke zu fertigen. Mittels der elektrischen Speisekontakte wird die Sinterkammer mit elektrischem Strom beaufschlagt, sodass sich entlang des Sinterstrompfades 70 der Sinterstrom ausbildet. Entsprechend werden mit dem erfindungsgemäßen Sin teraggregat 10 die Werkstücke gefertigt. By means of the sintering unit 10 according to the invention, the method according to the invention for spark plasma sintering is carried out. leads by filling in the sintering chamber of the electrically conductive material 20, which ben by means of steel discs 160 is separated from each other at the same time to manufacture several pieces. By means of the electrical supply contacts, the sintering chamber is supplied with electrical current, so that forms along the sintering flow path 70 of the sintering stream. According to the invention teraggregat 10, the workpieces are manufactured with the invention.

Claims

Patentansprüche claims
1. Sinteraggregat zum Spark-Plasma-Sintern elektrisch leitfä higer Werkstoffe, 1. sintering unit for spark plasma sintering of electrically conductive materials,
aufweisend eine Sinterkammer sowie einen ersten und einen zweiten elektrischen Kontakt, wobei erster und zweiter Kon takt angeordnet sind, bei Befüllung der Sinterkammer mit elektrisch leitfähigem Material (20) entlang eines durch die Sinterkammer hindurch führenden Sinterstrompfades (70) einen Sinterstrom zu leiten, wobei an einem vom Kontakt zur Sinter kammer verlaufenden Abschnitt des Sinterstrompfades ein Wär medämmelement (110, 120) angeordnet ist, welches einen ther mischen Isolator und einen elektrischen Leiter bildet. comprising a sintering chamber and a first and a second electrical contact, wherein the first and second con tact are arranged to guide a sintering flow when filling the sintering chamber with electrically conductive material (20) along a through the sintering chamber passing sintering flow path (70), wherein one of the contact to the sintering chamber extending portion of the sintering flow path, a heat medämmelement (110, 120) is arranged, which forms a ther mix insulator and an electrical conductor.
2. Sinteraggregat nach dem vorhergehenden Anspruch, bei wel chem das Wärmedämmelernent (110, 120) mit kohlefaserverstärk tem Graphit und/oder kohlefaserverstärktem Kohlenstoff gebil det ist. 2. Sinteraggregat according to the preceding claim, at wel chem the Wärmedämmelernent (110, 120) is gebil det with carbon fiber reinforced graphite graphite and / or carbon fiber reinforced carbon.
3. Sinteraggregat nach einem der vorhergehenden Ansprüche, bei welchem die Sinterkammer mit einer Matrize (40) aus oder mit Metall gebildet ist. 3. sintering unit according to one of the preceding claims, wherein the sintering chamber is formed with a die (40) made of or with metal.
4. Sinteraggregat nach einem der vorhergehenden Ansprüche, bei welchem die Matrize (40) eine im Wesentlichen zylinder mantelförmige Gestalt aufweist. 4. sintering unit according to one of the preceding claims, wherein the die (40) has a substantially cylindrical shell-like shape.
5. Sinteraggregat nach einem der vorhergehenden Ansprüche, bei welchem die Matrize (40) eine Längsachse (70) umgibt. 5. sintering unit according to one of the preceding claims, wherein the die (40) surrounds a longitudinal axis (70).
6. Sinteraggregat nach einem der vorhergehenden Ansprüche, bei welcher die Sinterkammer mit mindestens einem Pressstem pel (50, 60) gebildet ist, welcher zur Kraftbeaufschlagung in einer Richtung entlang der Längsachse (70) angeordnet sind. 6. sintering unit according to one of the preceding claims, wherein the sintering chamber with at least one Pressstem pel (50, 60) is formed, which are arranged for applying force in a direction along the longitudinal axis (70).
7. Sinteraggregat nach einem der vorhergehenden Ansprüche, bei welchem die Sinterkammer mit mindestens einem Pressstem- pel (50, 60) oder dem mindestens einen Pressstempel (50, 60) gebildet ist, der aus oder mit Metall gebildet ist. 7. sintering unit according to one of the preceding claims, wherein the sintering chamber with at least one pressing Stem pel (50, 60) or the at least one press ram (50, 60) is formed, which is made of or with metal.
8. Sinteraggregat umfassend mindestens ein Trennelement (140, 160), welches in die Sinterkammer einbringbar ist, insbeson dere umfassend eine Metallplatte, wobei das Trennelement (140, 160) die Sinterkammer in zumindest zwei Sinterräume aufteilt und/oder einen an die Matrize (40) angrenzenden Be reich der Sinterkammer ausfüllt. 8. sintering unit comprising at least one separating element (140, 160) which can be introduced into the sintering chamber, in particular comprising a metal plate, wherein the separating element (140, 160) divides the sintering chamber into at least two sintered spaces and / or one of the die (40 ) adjacent Be rich the sintering chamber fills.
9. Sinteraggregat nach dem vorhergehenden Anspruch, bei wel chem das mindestens eine Trennelement (140, 160) eine elekt rische Isolierschicht (150), insbesondere mit Bornitrid ge bildete Isolierschicht oder eine elektrisch leitende Schicht (170), insbesondere mit Graphit oder mit Titandiborid gebil dete Schicht aufweist. 9. Sinteraggregat according to the preceding claim, wherein wel chem the at least one separating element (140, 160) elec- tric insulating layer (150), in particular with boron nitride ge formed insulating layer or an electrically conductive layer (170), in particular with graphite or with titanium diboride gebil Dete layer has.
10. Verfahren zum Spark-Plasma-Sintern eines elektrisch leit fähigen Werkstoffs, bei welchem ein Sinteraggregat (10) nach einem der vorhergehenden Ansprüche herangezogen wird. 10. A method for spark plasma sintering of an electrically conductive material, in which a sintering unit (10) is used according to one of the preceding claims.
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