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WO2017064177A1 - Production of ceramics without piezo-electric properties in an aqueous environment - Google Patents

Production of ceramics without piezo-electric properties in an aqueous environment Download PDF

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Publication number
WO2017064177A1
WO2017064177A1 PCT/EP2016/074570 EP2016074570W WO2017064177A1 WO 2017064177 A1 WO2017064177 A1 WO 2017064177A1 EP 2016074570 W EP2016074570 W EP 2016074570W WO 2017064177 A1 WO2017064177 A1 WO 2017064177A1
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WO
WIPO (PCT)
Prior art keywords
suspension
freezing
liquid
gaseous
distribution
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Ceased
Application number
PCT/EP2016/074570
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German (de)
French (fr)
Inventor
Friederike Assmann
Tanja Einhellinger-Müller
Hans-Jürgen SCHREINER
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Ceramtec GmbH
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Ceramtec GmbH
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Publication of WO2017064177A1 publication Critical patent/WO2017064177A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/62605—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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising

Definitions

  • the present invention relates to a process for the production of ceramics without piezoelectric properties in predominantly aqueous dispersants.
  • the prior art a method for producing ceramics using organic dispersing agents is known.
  • Aqueous dispersions are also known per se in the production of ceramics, such as, for example.
  • the disadvantage of the process known from the prior art with aqueous dispersions is that alkalis can be leached out during the mixing of these aqueous dispersions and segregate on drying. This results in the problem that the materials are distributed inhomogeneous in the ceramic and the ceramic therefore has poorer material properties.
  • the object of the present invention was to develop a process which does not have the disadvantages mentioned.
  • the object is achieved by the inventive method for producing ceramics without piezoelectric properties, are used in the predominantly aqueous dispersion medium.
  • the method for producing ceramics without piezoelectric properties comprises the mixing of the raw materials, the grinding, the freezing of the isotropic distribution with subsequent temperature treatment, as well as the pellets production, shaping and sintering.
  • the process steps of mixing the raw materials and grinding are carried out in predominantly aqueous dispersants and segregation of the soluble constituents from the insoluble constituents, which leads to inhomogeneous materials, is prevented by the process control.
  • the segregation of the soluble constituents from the insoluble constituents is prevented in particular by fixing the isotropic distribution present in the aqueous suspension and subsequent removal of the suspension medium without any segregation taking place.
  • the fixation of the isotropic distribution can be done by freezing the suspension.
  • the freezing preferably takes place in a cooling medium (liquid, solid or gaseous) whose temperature is below the melting temperature of the suspension.
  • the temperature of the cooling medium is preferably well below the melting temperature of the suspension and allows shock freezing of the suspension.
  • the cooling medium is selected from the group consisting of liquid or gaseous nitrogen, liquid or gaseous air, liquid or gaseous oxygen, other liquid or gaseous organic or inorganic media.
  • the fixation of the isotropic distribution can also be effected by freezing the suspension by means of physical methods, such as pressure changes, solid media or similar methods.
  • the fixing can also be done by means of a gelation process or the like.
  • the fixation takes place by means of flocculation of the dispersion.
  • the addition of one or more additives is possible to achieve the fixation.
  • the removal of the suspending agent according to the invention is carried out with the exclusion of capillary forces and without a significant liquid phase being formed, whereby the frozen distribution is maintained.
  • the removal of the suspending agent is preferably carried out by sublimation of the predominantly aqueous dispersing agent to a certain, low residual moisture under suitable pressure / temperature conditions.
  • the freezing takes place by means of injection into a freezing medium and from it at the same time Protogranulat arises.
  • This protogranulate is converted by freeze-drying to a granulate which can be processed further.
  • the removal of the sublimation agent can also be done by means of a chemical process.
  • the transfer of the fixed distribution into the desired ceramic material without piezoelectric properties is achieved by means of a reaction process.
  • This reaction process is preferably a temperature treatment (calcination) of the fixed distribution, whereby a calcinate is formed.
  • a moldable powder can be prepared by spray-drying or other granulation methods.
  • Such a granulation process for preparing a press powder from calcine is preferably spray freeze granulation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to a method for producing ceramics without piezoelectric properties in predominantly aqueous dispersion means.

Description

Herstellung von Keramiken ohne piezoelektrische Eigenschaften in  Production of ceramics without piezoelectric properties in

wässriger Umgebung  aqueous environment

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Keramiken ohne piezoelektrische Eigenschaften in überwiegend wässrigen Dispersionsmitteln. The present invention relates to a process for the production of ceramics without piezoelectric properties in predominantly aqueous dispersants.

Im Stand der Technik ist ein Verfahren zum Herstellen von Keramiken bekannt, bei dem organische Dispersionsmittel verwendet werden. Wässrige Dispersionen sind bei der Herstellung von Keramiken, wie beispielsweise, an sich ebenfalls bekannt. Der Nachteil des aus dem Stand der Technik bekannten Verfahrens mit wässrigen Dispersionen ist, dass beim Mischen dieser wässrigen Dispersionen Alkalien herausgelöst werden können und beim Trocknen segregieren. Dadurch ergibt sich das Problem, dass die Stoffe in der Keramik inhomogen verteilt werden und die Keramik daher schlechtere Werkstoffeigenschaften aufweist. Die Aufgabe der vorliegenden Erfindung war, ein Verfahren zu entwickeln, welches die genannten Nachteile nicht aufweist. Die Aufgabe wird durch das erfindungsgemäße Verfahren zur Herstellung von Keramiken ohne piezoelektrische Eigenschaften gelöst, bei dem überwiegend wässrigen Dispersionsmittel verwendet werden. Erfindungsgemäß umfasst das Verfahren zur Herstellung von Keramiken ohne piezoelektrische Eigenschaften das Mischen der Rohstoffe, das Mahlen, das Einfrieren der isotropen Verteilung mit nachfolgender Temperaturbehandlung, sowie die Pressgranulatherstellung, Formgebung und Sinterung. In the prior art, a method for producing ceramics using organic dispersing agents is known. Aqueous dispersions are also known per se in the production of ceramics, such as, for example. The disadvantage of the process known from the prior art with aqueous dispersions is that alkalis can be leached out during the mixing of these aqueous dispersions and segregate on drying. This results in the problem that the materials are distributed inhomogeneous in the ceramic and the ceramic therefore has poorer material properties. The object of the present invention was to develop a process which does not have the disadvantages mentioned. The object is achieved by the inventive method for producing ceramics without piezoelectric properties, are used in the predominantly aqueous dispersion medium. According to the invention, the method for producing ceramics without piezoelectric properties comprises the mixing of the raw materials, the grinding, the freezing of the isotropic distribution with subsequent temperature treatment, as well as the pellets production, shaping and sintering.

Die Verfahrensschritte Mischen der Rohstoffe und Mahlen werden in überwiegend wässrigen Dispersionsmitteln durchgeführt und eine Segregation der löslichen Bestandteile von den unlöslichen Bestandteilen, was zu inhomogenen Materialien führt, wird durch die Prozessführung verhindert. Die Segregation der löslichen Bestandteile von den unlöslichen Bestandteilen wird insbesondere durch ein Fixieren der in der wässrigen Suspension vorhandenen isotropen Verteilung und anschließendes Entfernen des Suspensionsmediums, ohne dass eine Entmischung („Segregation") stattfindet, verhindert. The process steps of mixing the raw materials and grinding are carried out in predominantly aqueous dispersants and segregation of the soluble constituents from the insoluble constituents, which leads to inhomogeneous materials, is prevented by the process control. The segregation of the soluble constituents from the insoluble constituents is prevented in particular by fixing the isotropic distribution present in the aqueous suspension and subsequent removal of the suspension medium without any segregation taking place.

Das Fixieren der isotropen Verteilung kann durch ein Einfrieren der Suspension erfolgen. Das Einfrieren findet vorzugsweise in einem Kühlmedium (flüssig, fest oder gasförmig) statt, dessen Temperatur unterhalb der Schmelztemperatur der Suspension liegt. Die Temperatur des Kühlmediums ist bevorzugt weit unterhalb der Schmelztemperatur der Suspension und ermöglicht ein Schockgefrieren der Suspension. The fixation of the isotropic distribution can be done by freezing the suspension. The freezing preferably takes place in a cooling medium (liquid, solid or gaseous) whose temperature is below the melting temperature of the suspension. The temperature of the cooling medium is preferably well below the melting temperature of the suspension and allows shock freezing of the suspension.

Das Kühlmedium ist ausgewählt aus der Gruppe, bestehend aus flüssiger oder gasförmiger Stickstoff, flüssige oder gasförmige Luft, flüssiger oder gasförmiger Sauerstoff, andere flüssige oder gasförmige organische oder anorganische Medien. The cooling medium is selected from the group consisting of liquid or gaseous nitrogen, liquid or gaseous air, liquid or gaseous oxygen, other liquid or gaseous organic or inorganic media.

Das Fixieren der isotropen Verteilung kann auch durch ein Einfrieren der Suspension mittels physikalischer Methoden, wie Druckveränderungen, feste Medien oder ähnlichen Methoden erfolgen. Das Fixieren kann auch mittels eines Gelationsprozesses o. ä. erfolgen. Andererseits ist es auch möglich dass die Fixierung mittels Flockung der Dispersion stattfindet. Auch die Zugabe von einem oder mehreren Additiven ist möglich, um die Fixierung zu erreichen. The fixation of the isotropic distribution can also be effected by freezing the suspension by means of physical methods, such as pressure changes, solid media or similar methods. The fixing can also be done by means of a gelation process or the like. On the other hand, it is also possible that the fixation takes place by means of flocculation of the dispersion. Also, the addition of one or more additives is possible to achieve the fixation.

Die Entfernung des Suspensionsmittels wird erfindungsgemäß unter Ausschluss von Kapillarkräften und ohne dass eine nennenswerte flüssige Phase entsteht durchgeführt, wodurch die eingefrorene Verteilung erhalten bleibt. Die Entfernung des Suspensionsmittels erfolgt bevorzugt durch Sublimation des überwiegend wässrigen Dispersionsmittels bis zu einer bestimmten, geringen Restfeuchte unter geeigneten Druck/ Temperaturverhältnissen erfolgt. The removal of the suspending agent according to the invention is carried out with the exclusion of capillary forces and without a significant liquid phase being formed, whereby the frozen distribution is maintained. The removal of the suspending agent is preferably carried out by sublimation of the predominantly aqueous dispersing agent to a certain, low residual moisture under suitable pressure / temperature conditions.

In einer bevorzugten Ausführungsform der erfindungsgemäßen Lehre erfolgt das Einfrieren mittels Eindüsen in ein Gefriermedium und daraus gleichzeitig ein Protogranulat entsteht. Dieses Protogranulat wird durch Gefriertrocknen zu einem weiterverarbeitungsfähigen Granulat. In a preferred embodiment of the teaching according to the invention, the freezing takes place by means of injection into a freezing medium and from it at the same time Protogranulat arises. This protogranulate is converted by freeze-drying to a granulate which can be processed further.

Die Entfernung des Sublimationsmittels kann aber auch mittels eines chemischen Prozesses erfolgen. Die Überführung der fixierten Verteilung in das gewünschte keramische Material ohne piezoelektrische Eigenschaften wird mittels eines Reaktionsprozesses erreicht. Dieser Reaktionsprozess ist vorzugsweise eine Temperaturbehandlung (Kalzination) der fixierten Verteilung, wodurch ein Kalzinat gebildet wird. The removal of the sublimation agent can also be done by means of a chemical process. The transfer of the fixed distribution into the desired ceramic material without piezoelectric properties is achieved by means of a reaction process. This reaction process is preferably a temperature treatment (calcination) of the fixed distribution, whereby a calcinate is formed.

Aus dem so gebildeteren Kalzinat kann ein pressfähiges Pulver durch Sprühtrocknung oder andere Granulationsverfahren hergestellt werden. Ein solches Granulationsverfahren zur Herstellung eines pressfähigen Pulvers aus dem Kalzinat ist vorzugsweise die Sprühgefriergranulation. From the thus-formed calcinate, a moldable powder can be prepared by spray-drying or other granulation methods. Such a granulation process for preparing a press powder from calcine is preferably spray freeze granulation.

Claims

Ansprüche claims 1 . Verfahren zur Herstellung einer Keramik ohne piezoelektrischen Eigenschaften, dadurch gekennzeichnet, dass der Herstellungsprozess überwiegend in wässrigen Dispersionsmitteln erfolgt. 1 . Process for producing a ceramic without piezoelectric properties, characterized in that the manufacturing process is carried out predominantly in aqueous dispersion media. 2. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass der Herstellungsprozess die Schritte Mischen der Rohstoffe, Mahlen und Pressgranulatherstellung umfasst. 2. The method according to claim 1, characterized in that the manufacturing process comprises the steps of mixing the raw materials, grinding and pressing granulate production. 3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass bei den Schritten Mischen der Rohstoffe und Mahlen eine Segregation der löslichen Bestandteile von den unlöslichen Bestandteilen durch Fixieren der in der wässrigen Suspension vorhandenen isotropen Verteilung und anschließendem Entfernen des Suspensionsmediums verhindert wird. 3. The method according to claim 1 or 2, characterized in that in the steps of mixing the raw materials and grinding a segregation of the soluble constituents is prevented by the insoluble constituents by fixing the present in the aqueous suspension isotropic distribution and subsequent removal of the suspension medium. 4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass diese Fixierung der Verteilung durch ein Einfrieren der Suspension erfolgt und das Suspensionsmittel anschließend so entfernt wird, dass keine Entmischung („Segregation") stattfindet. 4. The method according to claim 3, characterized in that this fixation of the distribution is carried out by freezing the suspension and the suspending agent is then removed so that no segregation ("segregation") takes place. 5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass das Einfrieren der Suspension in einem Kühlmedium (flüssig, fest oder gasförmig) erfolgt, dessen Temperatur unterhalb der Schmelztemperatur der Suspension liegt. 5. The method according to claim 4, characterized in that the freezing of the suspension is carried out in a cooling medium (liquid, solid or gaseous) whose temperature is below the melting temperature of the suspension. 6. Verfahren nach Anspruch 4 oder 5, dadurch gekennzeichnet, dass das Einfrieren der Suspension in einem Kühlmedium (flüssig, fest oder gasförmig) erfolgt, dessen Temperatur weit unterhalb der Schmelztemperatur der Suspension liegt, sodass Schockgefrieren möglich ist. 6. The method according to claim 4 or 5, characterized in that the freezing of the suspension in a cooling medium (liquid, solid or gaseous) takes place, the temperature of which is far below the melting temperature of the suspension, so that shock-freezing is possible. 7. Verfahren nach einem der Ansprüche 4 bis 6, dadurch gekennzeichnet, dass das Kühlmedium aus der Gruppe ausgewählt ist, bestehend aus flüssiger oder gasförmiger Stickstoff, flüssige oder gasförmige Luft, flüssiger oder gasförmiger Sauerstoff, andere flüssige oder gasförmige organische oder anorganische Medien. 7. The method according to any one of claims 4 to 6, characterized in that the cooling medium is selected from the group consisting of liquid or gaseous nitrogen, liquid or gaseous air, liquid or gaseous oxygen, other liquid or gaseous organic or inorganic media. 8. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass das Einfrieren der Suspension mittels physikalischer Methoden, wie Druckveränderungen, feste Medien oder ähnlichen Methoden erfolgt. 8. The method according to claim 4, characterized in that the freezing of the suspension by means of physical methods, such as pressure changes, solid media or similar methods takes place. 9. Verfahren nach nach einem der Ansprüche 4 bis 8, dadurch gekennzeichnet, dass die Entfernung des Suspensionsmittels unter Ausschluss von Kapillarkräften und ohne dass eine nennenswerte flüssige Phase entsteht geschieht, wodurch die eingefrorene Verteilung erhalten bleibt. 9. The method according to any one of claims 4 to 8, characterized in that the removal of the suspending agent with the exclusion of capillary forces and without a significant liquid phase is formed, whereby the frozen distribution is maintained. 10. Verfahren nach einem der Ansprüche 4 bis 9, dadurch gekennzeichnet, dass die Entfernung des Suspensionsmittels durch Sublimation bis zu einer bestimmten, geringen Restfeuchte unter geeigneten Druck/ Temperaturverhältnissen erfolgt, wodurch die eingefrorene Verteilung erhalten bleibt. 10. The method according to any one of claims 4 to 9, characterized in that the removal of the suspending agent is carried out by sublimation to a certain, low residual moisture under suitable pressure / temperature conditions, whereby the frozen distribution is maintained. 1 1 .Verfahren nach einem der Ansprüche 4, dadurch gekennzeichnet, dass das Einfrieren der Suspension durch Eindüsen in ein Gefriermedium erfolgt und daraus gleichzeitig ein Protogranulat entsteht, wobei das Protogranulat durch Gefriertrocknen zu einem weiterverarbeitungsfähigen Granulat wird. 1 1 .Method according to one of claims 4, characterized in that the freezing of the suspension takes place by injection into a freezing medium and at the same time a protogranulate is formed, wherein the protogranulate is by freeze-drying to a further processable granules. 12. Verfahren nach einem der Ansprüche 3 bis 1 1 , dadurch gekennzeichnet, dass fixierte Verteilung mittels eines Reaktionsprozesses, bevorzugt mittels Temperaturbehandlung (Kalzination), in das gewünschte keramische Material (Kalzinat) überführt wird. 12. The method according to any one of claims 3 to 1 1, characterized in that fixed distribution by means of a reaction process, preferably by means of temperature treatment (calcination), in the desired ceramic material (calcine) is transferred. 13. Verfahren nach Anspruch 12, dadurch gekennzeichnet, dass aus dem Kalzinat durch Sprühgefriergranulation ein pressfähiges Pulver hergestellt wird. 13. The method according to claim 12, characterized in that a pressable powder is prepared from the calcine by Sprühgefriergranulation.
PCT/EP2016/074570 2015-10-13 2016-10-13 Production of ceramics without piezo-electric properties in an aqueous environment Ceased WO2017064177A1 (en)

Applications Claiming Priority (2)

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DE102015219797.2 2015-10-13
DE102015219797 2015-10-13

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005030518A1 (en) * 2005-06-29 2007-01-04 Universität Bremen Process for mullite production by suspension of Al powder in an aqueous silica-sol suspension used in building ceramics and fire resistant materials in which silica particles have a specified diameter,
DE102008000100A1 (en) * 2008-01-18 2009-07-23 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Lightweight green and molded body of a ceramic and / or powder metallurgical material and method for its preparation
US20130167447A1 (en) * 2011-12-30 2013-07-04 Diamond Innovations, Inc. Near-Net Cutting Tool Insert
WO2013160388A1 (en) * 2012-04-26 2013-10-31 Heraeus Quarzglas Gmbh & Co. Kg Process for producing sio2 granules

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005030518A1 (en) * 2005-06-29 2007-01-04 Universität Bremen Process for mullite production by suspension of Al powder in an aqueous silica-sol suspension used in building ceramics and fire resistant materials in which silica particles have a specified diameter,
DE102008000100A1 (en) * 2008-01-18 2009-07-23 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Lightweight green and molded body of a ceramic and / or powder metallurgical material and method for its preparation
US20130167447A1 (en) * 2011-12-30 2013-07-04 Diamond Innovations, Inc. Near-Net Cutting Tool Insert
WO2013160388A1 (en) * 2012-04-26 2013-10-31 Heraeus Quarzglas Gmbh & Co. Kg Process for producing sio2 granules

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