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WO1996003355A1 - Procede de production de microstructures ceramiques - Google Patents

Procede de production de microstructures ceramiques Download PDF

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Publication number
WO1996003355A1
WO1996003355A1 PCT/EP1995/002242 EP9502242W WO9603355A1 WO 1996003355 A1 WO1996003355 A1 WO 1996003355A1 EP 9502242 W EP9502242 W EP 9502242W WO 9603355 A1 WO9603355 A1 WO 9603355A1
Authority
WO
WIPO (PCT)
Prior art keywords
sol
gel
ceramic
microstructures
electrically conductive
Prior art date
Application number
PCT/EP1995/002242
Other languages
German (de)
English (en)
Inventor
Hans-Joachim Ritzhaupt-Kleissl
Jürgen Laubersheimer
Original Assignee
Forschungszentrum Karlsruhe Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Forschungszentrum Karlsruhe Gmbh filed Critical Forschungszentrum Karlsruhe Gmbh
Publication of WO1996003355A1 publication Critical patent/WO1996003355A1/fr

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Classifications

    • 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
    • C04B35/624—Sol-gel processing

Definitions

  • the invention relates to a method for producing ceramic microstructures according to claim 1.
  • DE 43 10 068 C1 discloses a process for producing a plate-shaped microstructure body made of ceramic, in which a film produced according to the "Doctor-Blade M process is provided with a microstructured embossing tool with the complementary structures of the embossing tool The embossed film is sintered and transferred into a ceramic microstructure body.
  • Electrophoresis and its use in shaping ceramics are described in the "Handbook of Ceramics", edited by Dr.-Ing. Wilhelm Büke, Verlag Schmid GmbH, Freiburg i. Brg. , treated. Electrophoresis using "lyophobic" brine (eg iron (II hydroxide, clay, quartz, sulfur in water) is explained on page 16. On page 20, the use of electrophoresis for the production of articles of daily use is reported Manufacture is based, inter alia, on a slip of 50% quartz and 59% clay, and the electrophoretic deposition is carried out on a porous sintered bronze or a porous graphite or graphite cement.
  • lyophobic brine eg iron (II hydroxide, clay, quartz, sulfur in water
  • the object of the invention is, in addition to the above-mentioned impression of a film produced by the "doctor blade” process, to provide a further process by means of which ceramic microstructures can be produced.
  • the starting point of the process are liquid organometallic compounds from which a gellable sol is formed. Usually alcoholates are used for the production of sol.
  • a sol for example, the precursor for a ceramic made of lead zirconium titanium oxide [PZT ceramic, Pb (Zrn 52 ⁇ i 0 48 ) ° 3 3 can be used.
  • organic auxiliaries for example formamide, can be added to the sol.
  • the microstructure in the finished ceramic microstructures can be adjusted by adding binders and plasticizers.
  • a "lost" shape which can either consist of a metal that can be selectively dissolved with respect to the ceramic, or of a plastic that can be burned or that can be selectively dissolved by chemical means.
  • a suitable material for the shape is poly methyl methacrylate (PMMA), which can be burned without residue.
  • PMMA poly methyl methacrylate
  • the form contains the complementary structures of the microstructures to be produced from ceramic.
  • the complementary structures can in turn be obtained by deep X-ray lithography, mechanical microfabrication or by molding an embossing tool.
  • a metal mold can be produced by galvanic molding of a plastic mold.
  • the complementary structures must be provided with an electrically conductive surface, provided that the material of the mold is not electrically conductive per se.
  • the conductive surface is preferably by dusting a metal (sputtering), e.g. B. made of gold.
  • the electrically conductive surface of the complementary structures is switched as an electrode during the subsequent electrophoresis step.
  • Any inert electrode e.g. B. a platinum sheet can be used.
  • the gel particles are preferably deposited on the electrically conductive surface at constant current, preferably at 30 to 100 mA, with voltages of up to 250 V being established. Typical and particularly preferred values for current and voltage in the PZT deposition are 30 mA and 80 V.
  • the deposition rate of the PZT sol in this case is approximately 20 ⁇ m / min.
  • the components of the sol are deposited homogeneously in accordance with the stoichiometric composition of the sol.
  • the auxiliaries, binders and plasticizers are deposited in the mold together with the components.
  • the sol gels during the electrophoretic deposition.
  • the gel filling the mold is dried. Drying is preferably carried out in several steps, each lasting a few hours: B. Lucas ⁇ drying, drying at 50 to 100 ° C in air and finally at 50 to 100 ° C in a vacuum. If drying cracks cannot be completely ruled out, in this case again gel of the same composition can be deposited electrophoretically. Since the deposition preferably begins at the points closest to the electrode, drying cracks are filled in from the bottom of the crack.
  • the complementary structure of the mold can first be filled in only partially, after which it is dried and then a further electrophoresis step takes place. These steps can be repeated several times.
  • the subsequent electrophoresis step the cracks which have arisen in the layer produced by the previous electrophoresis step during drying are automatically filled in, so that finally a gel is obtained which at most shows surface cracks.
  • the shape is removed.
  • plastic molds this can be done without residue by thermal pyrolysis.
  • the plastic form can be selectively removed using chemical solvents.
  • a form made of PMMA can be detached, for example, by acetonitrile or hot ethyl acetate.
  • Metal molds with a low melting point can be removed by selective melting. Since shrinkage occurs during drying, the dried gel can in many cases be easily removed from the metal mold anyway without destroying the mold.
  • the gel is then ceramized and densely sintered in a known manner by using high temperatures.
  • the ceramization is preferably carried out at temperatures of 500 to 800 ° C.
  • the sealing sintering takes place by increasing the temperature, for example to temperatures between 1000 and 1500 ° C. at PZT ceramics, the optimal temperature is 1150 ⁇ C with a holding time of 90 to 150 min.
  • the gold layer was about 30 n thick.
  • the microstructures formed a pattern of free-standing hexagonal columns with a height of 250 ⁇ m and a thickness of 50 ⁇ m, the distances between which corresponded to the column thickness. Each column was surrounded by six neighboring columns.
  • the gelled sol produced was placed in a thermostated electrophoresis cell.
  • the electrically conductive surface of the mold (2 x 2 cm) was switched as an anode.
  • a platinum sheet (2 x 2 cm) was used as the cathode, and its distance from the mold was at least 3 cm.
  • the electrophoresis was carried out at a constant current of 30 mA and approx. 80 V. After a deposition time of approx. 2 hours, a layer thickness of 2 mm was obtained, so that the microstructures were completely covered by the gel.
  • Drying was carried out in three steps: one day in air, then several hours at 80 ° C and finally at 80 ° C in a vacuum. Drying cracks were filled in by repeating the electrophoresis step.
  • both the organic constituents in the dried gel and the PMMA-For were burned off in a suitable oven, with continuous heating from 200 ° C. to 500 ° C. slowly (1.5 ° C./min). After that there was a ceramic microstructure.
  • the ceramic structure was densely sintered by sintering at a temperature of 1150 ° C. for 90 minutes.
  • a ceramic microstructure was obtained in the form of a plate which had a hexagonal pattern of hexagonal openings. The diameter of the openings was approximately 40 ⁇ m because of the shrinkage.

Landscapes

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

Abstract

L'invention vise à mettre au point un procédé de production de microstructures céramiques. Ce procédé comprend les étapes suivantes: a) un sol gélifiable est réalisé à partir de plusieurs constituants liquides organo-métalliques, b) un moule est préparé qui porte des structures complémentaires des microstructures qui sont munies de surfaces électroconductrices, c) les structures complémentaires du moule sont remplies de manière homogène de sol par électrophorèse, la surface électroconductice faisant office d'électrode et le sol étant transformé en gel, d) le gel est séché, e)le moule est enlevé et f) le gel est transformé en céramique par combustion des constituants organiques.
PCT/EP1995/002242 1994-07-22 1995-06-10 Procede de production de microstructures ceramiques WO1996003355A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP4425978.6 1994-07-22
DE19944425978 DE4425978C1 (de) 1994-07-22 1994-07-22 Verfahren zur Herstellung keramischer Mikrostrukturen

Publications (1)

Publication Number Publication Date
WO1996003355A1 true WO1996003355A1 (fr) 1996-02-08

Family

ID=6523869

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1995/002242 WO1996003355A1 (fr) 1994-07-22 1995-06-10 Procede de production de microstructures ceramiques

Country Status (2)

Country Link
DE (1) DE4425978C1 (fr)
WO (1) WO1996003355A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2342373C2 (ru) * 2003-09-19 2008-12-27 Авентис Фарма С.А. Ацетоновый сольват диметоксидоцетаксела и способ его получения

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10357540B4 (de) * 2003-12-10 2007-08-16 Deutsches Zentrum für Luft- und Raumfahrt e.V. Verfahren zur elektrochemischen Abscheidung von Aerogelen auf metallischen Oberflächen, anisotrope Beschichtung und deren Verwendung
DE102006005474A1 (de) * 2006-01-27 2007-08-02 Michael Loos Verfahren zur Herstellung dünnwandiger Lautsprechermembrane aus einem keramischen Material und durch das Verfahren erhaltene Membran für Lautsprecher bevorzugt im Tief- und Mitteltonbereich

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0535854A1 (fr) * 1991-10-04 1993-04-07 Foseco International Limited Moules
US5302319A (en) * 1991-01-07 1994-04-12 United Technologies Corporation Preparation of sol gel composition for electrophoresis

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4310068C1 (de) * 1993-03-27 1994-06-16 Kernforschungsz Karlsruhe Verfahren zur Herstellung eines plattenförmigen Mikrostrukturkörpers aus Keramik

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5302319A (en) * 1991-01-07 1994-04-12 United Technologies Corporation Preparation of sol gel composition for electrophoresis
EP0535854A1 (fr) * 1991-10-04 1993-04-07 Foseco International Limited Moules

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HIROSHI HISASHIMA ET AL.: "PREPARATION OF SOL-GEL COATINGS BY ELECTROPHORETIC DEPOSITION", MATER-RES.SOC.SYMP.PROC. 346 (BETTER CERAMICS THROUGH CHEMISTRY VI), vol. 346, 4 April 1994 (1994-04-04) - 8 April 1994 (1994-04-08), PITTSBURGH PENNSYLVANIA, USA, pages 95 - 100 *
YINING ZHANG ET AL.: "ELECTROPHORETIC DEPOSITION OF SOL-GEL DERIVED CERAMIC COATINGS", MATER.RES.SOC.SYMP.PROC. 271 (BETTER CERAMICS THROUGH CHEMISTRY V), vol. 271, 27 April 1992 (1992-04-27) - 1 May 1992 (1992-05-01), pages 465 - 470 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2342373C2 (ru) * 2003-09-19 2008-12-27 Авентис Фарма С.А. Ацетоновый сольват диметоксидоцетаксела и способ его получения

Also Published As

Publication number Publication date
DE4425978C1 (de) 1995-11-23

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