DE10232791A1 - Production of barium or strontium titanate useful as dielectrics in capacitors comprises reacting a titanium alkoxide with barium or strontium hydroxide hydrate in an alcohol or glycol ether - Google Patents

Production of barium or strontium titanate useful as dielectrics in capacitors comprises reacting a titanium alkoxide with barium or strontium hydroxide hydrate in an alcohol or glycol ether Download PDF

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DE10232791A1
DE10232791A1 DE2002132791 DE10232791A DE10232791A1 DE 10232791 A1 DE10232791 A1 DE 10232791A1 DE 2002132791 DE2002132791 DE 2002132791 DE 10232791 A DE10232791 A DE 10232791A DE 10232791 A1 DE10232791 A1 DE 10232791A1
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barium
strontium
glycol mono
strontium titanate
ether
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Hans-Josef Dr. Sterzel
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BASF SE
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Priority to AT03008675T priority patent/ATE346825T1/en
Priority to EP03008675A priority patent/EP1362830B1/en
Priority to DE50305808T priority patent/DE50305808D1/en
Priority to ES03008675T priority patent/ES2276994T3/en
Priority to US10/435,457 priority patent/US7223378B2/en
Priority to JP2003133887A priority patent/JP2004131364A/en
Publication of DE10232791A1 publication Critical patent/DE10232791A1/en
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    • C—CHEMISTRY; METALLURGY
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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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6264—Mixing media, e.g. organic solvents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/006—Alkaline earth titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3215—Barium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/441—Alkoxides, e.g. methoxide, tert-butoxide

Abstract

Production of barium or strontium titanate comprises reacting a titanium alkoxide with barium or strontium hydroxide hydrate in a C1-C8 alcohol or glycol ether at 50-150degreesC. An Independent claim is also included for barium or strontium titanate produced as above and having an average particle diameter below 10 nm.

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Barium- oder Strontiumtitanat durch Umsetzung von Titanalkoholaten mit Barium- oder Strontiumhydroxid-hydrat in einem Alkohol oder einem Glykolether bei erhöhter Temperatur.The present invention relates to a process for the production of barium or strontium titanate by reacting titanium alcoholates with barium or strontium hydroxide hydrate in an alcohol or a glycol ether at elevated temperature.

Aus J. Am. Ceram. Soc., Vol 52, No. 10, Seite 523 bis 526 (1969) ist die Herstellung von Bariumtitanat-Pulvern aus Bariumisopropoxid und Titantetra-tert.-amyloxid in einem Lösungsmittel unter Rückfluss und anschließende tropfenweise Wasserzugabe bekannt. Die Korngröße des kristallinen Materials nach Trocknung bei 50°C beträgt 5 bis 15 nm. Zur Entfernung organischer Reste ist eine Erhitzung auf mindestens 900°C erforderlich, wobei Kohlenstoff im Titanat verbleibt, das Ursache für hohe Leckströme ist und bei der Verwendung als Kondensatormaterial nachteilig ist.From J. Am. Ceram. Soc., Vol 52, No. 10, pages 523 to 526 (1969) is the production of barium titanate powders from barium isopropoxide and titanium tetra-tert-amyl oxide in a solvent under reflux and subsequent dropwise water addition known. The grain size of the crystalline material after Drying at 50 ° C is 5 to 15 nm. To remove organic residues, heating is necessary to at least 900 ° C required, with carbon remaining in the titanate, the cause for high Leakage current is and is disadvantageous when used as a capacitor material.

Aus High Tech Ceramics, 1987, Seite 1459 bis 1468 ist ein Verfahren zur Herstellung kohlenstofffreier Bariumtitanate durch Einbringen einer wässrigen Bariumhydroxid-octahydrat-Lösung in eine Lösung von Titantetra-n-butylat in Butanol bekannt, wobei ein Gel entsteht, das bei 100°C getrocknet und bei 1350°C gesintert wird. Die Korngröße beträgt ca. 1 μm.From High Tech Ceramics, 1987, page 1459 to 1468 is a process for making carbon-free Barium titanates by introducing an aqueous barium hydroxide octahydrate solution into a solution known from titanium tetra-n-butoxide in butanol, forming a gel, that at 100 ° C dried and at 1350 ° C is sintered. The grain size is approx. 1 μm.

Nachteilig an diesen Verfahren sind die Größe der erhaltenen Körner bzw. der verbleibende Kohlenstoffgehalt.These processes are disadvantageous the size of the received grains or the remaining carbon content.

Der vorliegenden Erfindung lag daher die Aufgabe zugrunde, den zuvor genannten Nachteilen abzuhelfen.The present invention was therefore based on the task of remedying the disadvantages mentioned above.

Demgemäß wurde ein neues und verbessertes Verfahren zur Herstellung von Barium- oder Strontiumtitanat gefunden, welches dadurch gekennzeichnet ist, dass man Titanalkoholate mit Barium- oder Strontiumhydroxid-hydrat in einem C1- bis C8-Alkohol oder einem Glykolether bei einer Temperatur von 50 bis 150°C umsetzt.Accordingly, a new and improved process for the preparation of barium or strontium titanate has been found, which is characterized in that titanium alcoholates with barium or strontium hydroxide hydrate in a C 1 - to C 8 -alcohol or a glycol ether at a temperature of 50 to 150 ° C implemented.

Das erfindungsgemäße Verfahren lässt sich wie folgt durchführen:
Man kann Titanalkoholate in einem C1- bis C8-Alkanol, in einem Glykolether oder deren Gemischen vorlegen und bei einer Temperatur von 50 bis 150°C, bevorzugt 60 bis 120°C, besonders bevorzugt 70 bis 110°C, insbesondere bei Rückflusstemperatur und einem Druck von 0,1 bis 3 bar, bevorzugt 0,5 bis 2 bar, besonders bevorzugt bei Atmosphärendruck (Normaldruck) mit Barium- oder Strontiumhydroxid-hydrat umsetzen.The method according to the invention can be carried out as follows:
Titanium alcoholates can be initially introduced in a C 1 to C 8 alkanol, in a glycol ether or mixtures thereof and at a temperature of 50 to 150 ° C, preferably 60 to 120 ° C, particularly preferably 70 to 110 ° C, in particular at the reflux temperature and a pressure of 0.1 to 3 bar, preferably 0.5 to 2 bar, particularly preferably at atmospheric pressure (normal pressure) with barium or strontium hydroxide hydrate.

Die Konzentration der alkoholischen Titanalkoholat-Lösung kann in weiten Grenzen variiert werden. Bevorzugt liegt die Konzentration bei 50 bis 800 g/Liter, besonders bevorzugt bei 100 bis 600 g/Liter, besonders bevorzugt bei 200 bis 400 g/Liter.The concentration of alcoholic Titanium alkoxide solution can be varied within wide limits. The concentration is preferably at 50 to 800 g / liter, particularly preferably at 100 to 600 g / liter, particularly preferably at 200 to 400 g / liter.

Als Barium- oder Strontiumhydroxid-hydrate eignen sich die bekannten Hydroxid-hydrate, z.B. Barium- oder Strontiumhydroxid-octahydrat.Suitable as barium or strontium hydroxide hydrates the known hydroxide hydrates, e.g. Barium or strontium hydroxide octahydrate.

Als Titanalkoholate eignen sich beispielsweise Titantetramethanolat, Titantetraethanolat, Titantetra-n-propanolat, Titantetra-iso-propanolat, Titantetra-n-butanolat, Titantetra-iso-butanolat, Titantetra-sec.-butanolat, Titantetra-tert.-butanolat, Titantetra-n-pentanolat und Titantetra-iso-pentanolat, bevorzugt Titantetraethanolat, Titantetra-n-propanolat, Titantetra-iso-propanolat, Titantetra-n-butanolat, Titantetra-isobutanolat, Titantetra-sec.-butanolat und Titantetra-tert.-butanolat, besonders bevorzugt Titantetra-n-propanolat, Titantetra-iso-propanolat, Titantetra-n-butanolat und Titantetra-iso-butanolat oder deren Gemische.Suitable as titanium alcoholates, for example Titanium tetramethanolate, titanium tetraethanolate, titanium tetra-n-propanolate, Titanium tetra-iso-propanolate, titanium tetra-n-butanolate, titanium tetra-iso-butanolate, titanium tetra-sec-butanolate, Titanium tetra-tert-butanolate, titanium tetra-n-pentanolate and titanium tetra-isopentanolate, preferably titanium tetraethanolate, titanium tetra-n-propanolate, titanium tetra-iso-propanolate, Titanium tetra-n-butanolate, titanium tetra-isobutanolate, titanium tetra-sec-butanolate and titanium tetra-tert-butanolate, particularly preferably titanium tetra-n-propanolate, titanium tetra-iso-propanolate, Titanium tetra-n-butanolate and titanium tetra-iso-butanolate or mixtures thereof.

Als Alkohole eignen sich C1- bis C8-Alkanole, bevorzugt C1- bis C4-Alkanole wie Methanol, Ethanol, n-Propanol, Iso-propanol, n-Butanol, iso-Butanol, sec.-Butanol oder tert.-Butanol, besonders bevorzugt C1- bis C3-Alkanol wie Methanol, Ethanol, n-Propanol oder Iso-propanol, insbesondere Methanol oder Ethanol.Suitable alcohols are C 1 -C 8 -alkanols, preferably C 1 -C 4 -alkanols such as methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-butanol, sec-butanol or tert. -Butanol, particularly preferably C 1 -C 3 -alkanol such as methanol, ethanol, n-propanol or iso-propanol, in particular methanol or ethanol.

Als Glykolether eignen sich alle bekannten Glykolether wie beispielsweise Ethylenglykol-mono-methylether, Ethylenglykol-mono-ethylether, Ethylenglykol-mono-n-propylether, Ethylenglykol-mono-iso-propylether, Ethylenglykol-mono-n-butylether, Ethylenglykol-mono-iso-butylether, Ethylenglykol-mono-sec.-butylether, Ethylenglykol-tert.-butylether, Diethylenglykol-mono-methylether, Diethylenglykol-mono-ethylether, Diethylenglykol-mono-n-propylether, Diethylenglykol-mono-iso-propylether, Diethylenglykol-mono-n-butylether, Diethylenglykol-mono-iso-butylether, Diethylenglykol-mono-sec.-butylether, Diethylenglykol-tert.-butylether, bevorzugt Ethylenglykol-mono-ethylether, Ethylenglykol-mono-n-propylether, Ethylenglykol-mono-iso-propylether, Ethylenglykol-mono-n-butylether, Ethylenglykol-mono-iso-butylether, Ethylenglykol-mono-sec.-butylether, Ethylenglykol-tert.- butylether, Diethylenglykol-mono-euhylether, Diethylenglykol-mono-n-propylether, Diethylenglykol-mono-iso-propylether, Diethylenglykol-mono-n-butylether, Diethylenglykol-mono-iso-butylether, Diethylenglykol-mono-sec.-butylether und Diethylenglykol-tert.-butylether, besonders bevorzugt Ethylenglykol-mono-n-propylether, Ethylenglykol-mono-iso-propylether, Ethylenglykol-mono-n-butylether, Ethylenglykol-mono-iso-butylether, Ethylenglykol-mono-sec.-butylether, Ethylenglykol-tert.-butylether, Diethylenglykol-mono-n-propylether, Diethylenglykol-mono-iso-propylether, Diethylenglykol-mono-n-butylether, Diethylenglykol-mono-iso-butylether, Diethylenglykol-mono-sec.-butylether und Diethylenglykol-tert.-butylether, insbesondere Ethylenglykol-mono-iso-propylether, Ethylenglykol-mono-iso-butylether, Ethylenglykol-tert.-butylether, Diethylenglykol-mono-iso-propylether, Diethylenglykol-mono-iso-butylether und Diethylenglykol-tert.-butylether.All are suitable as glycol ethers known glycol ethers such as ethylene glycol monomethyl ether, Ethylene glycol mono ethyl ether, ethylene glycol mono n-propyl ether, Ethylene glycol mono-iso-propyl ether, Ethylene glycol mono-n-butyl ether, ethylene glycol mono-iso-butyl ether, Ethylene glycol mono-sec-butyl ether, ethylene glycol tert-butyl ether, Diethylene glycol mono methyl ether, diethylene glycol mono ethyl ether, Diethylene glycol mono-n-propyl ether, Diethylene glycol mono-iso-propyl ether, diethylene glycol mono-n-butyl ether, Diethylene glycol mono-iso-butyl ether, diethylene glycol mono-sec-butyl ether, Diethylene glycol tert-butyl ether, preferably ethylene glycol monoethyl ether, ethylene glycol mono n-propyl ether, Ethylene glycol mono-iso-propyl ether, ethylene glycol mono-n-butyl ether, Ethylene glycol mono-isobutyl ether, ethylene glycol mono-sec-butyl ether, Ethylene glycol tert-butyl ether, Diethylene glycol mono-euhyl ether, diethylene glycol mono-n-propyl ether, diethylene glycol mono-iso-propyl ether, Diethylene glycol mono-n-butyl ether, diethylene glycol mono-iso-butyl ether, diethylene glycol mono-sec-butyl ether and diethylene glycol tert-butyl ether, particularly preferably ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, Ethylene glycol mono-n-butyl ether, ethylene glycol mono-iso-butyl ether, Ethylene glycol mono-sec-butyl ether, ethylene glycol tert-butyl ether, Diethylene glycol mono-n-propyl ether, diethylene glycol mono-iso-propyl ether, Diethylene glycol mono-n-butyl ether, diethylene glycol mono-iso-butyl ether, Diethylene glycol mono-sec-butyl ether and diethylene glycol tert-butyl ether, in particular ethylene glycol mono-iso-propyl ether, ethylene glycol mono-iso-butyl ether, Ethylene glycol tert-butyl ether, diethylene glycol mono-iso-propyl ether, Diethylene glycol mono-iso-butyl ether and diethylene glycol tert-butyl ether.

Es kann vorteilhaft sein das Eintragen des Barium- oder Strontiumhydroxid-octahydrat durch kräftiges Rühren zu unterstützen.It may be advantageous to enter it the barium or strontium hydroxide octahydrate by stirring vigorously support.

Eine vorteilhafte Ausführungsform besteht darin, dass kein zusätzliches Wasser außer dem Wasser aus dem Hydroxid-hydrat in die Umsetzung eingetragen wird.An advantageous embodiment is that no additional Water except the water from the hydroxide hydrate entered in the reaction becomes.

Eine bevorzugte Ausführungsform besteht darin, dass einen Teil des Barium- oder Strontiumhydroxidoctahydrats durch wasserfreies Barium- oder Strontiumhydroxid zu ersetzen und über das Kristallwasser nur insgesamt 2 bis 4 Mole Wasser pro Mol Titanat einzubringen. Diese Vorgehensweise führt zu einer gießfähigen, stabilen Suspension der Titanatteilchen im Alkohol oder Glykolether.A preferred embodiment is that part of the barium or strontium hydroxide octahydrate to be replaced by anhydrous barium or strontium hydroxide and over the Crystal water only 2 to 4 moles of water per mole of titanate contribute. This procedure leads to a pourable, stable Suspension of the titanate particles in alcohol or glycol ether.

Gegebenenfalls können Dotierelemente wie Mg, Ca, Zn, Zr, V, Nb, Ta, Bi, Cr, Mo, W, Mn, Fe, Co, Ni, Pb, Ce oder deren Gemische, bevorzugt Mg, Ca, Cr, Fe, Co, Ni, Pb oder deren Gemische, beispielsweise in Form ihrer Hydroxide, Oxide, Carbonate, Carboxylate oder Nitrate eingebracht werden.If necessary, doping elements such as Mg, Ca, Zn, Zr, V, Nb, Ta, Bi, Cr, Mo, W, Mn, Fe, Co, Ni, Pb, Ce or their mixtures, preferably Mg, Ca, Cr, Fe, Co, Ni, Pb or their Mixtures, for example in the form of their hydroxides, oxides, carbonates, carboxylates or nitrates.

Die erfindungsgemäß hergestellten Barium- und Strontiumtitanate haben einen mittleren Teilchendurchmesser von kleiner als 10 nm, bevorzugt 0,5 bis 9,9 nm, besonders bevorzugt 0,6 bis 9 nm, insbesondere 1 bis 8 nm.The barium and Strontium titanates have an average particle diameter of smaller than 10 nm, preferably 0.5 to 9.9 nm, particularly preferred 0.6 to 9 nm, in particular 1 to 8 nm.

Barium- und Strontiumtitanat oder deren Gemische eignen sich als Dielektrika und haben relative Dielektrizitätskonstanten bis 5.000. Sie eignen sich als Dielektrika in Kondensatoren, insbesondere in keramischen Kondensatoren.Barium and strontium titanate or their mixtures are suitable as dielectrics and have relative dielectric constants up to 5,000. They are particularly suitable as dielectrics in capacitors in ceramic capacitors.

Es ist möglich, kommerzielle Metallfolien wie Nickelfolien mit den erfindungsgemäßen Dispersionen in Schichtdicken unterhalb 0,5 μm zu beschichten, den Alkohol oder Glykolether zu verdampfen und bevorzugt unter Sauerstoffausschluss eine entsprechend dünne Titanatschicht auf der Metallfolie zu erzeugen und damit einen Wickelkondensator herzustellen.It is possible to use commercial metal foils like nickel foils with the dispersions according to the invention in layer thicknesses below 0.5 μm to coat, evaporate the alcohol or glycol ether and preferred with exclusion of oxygen, a correspondingly thin titanate layer on the To produce metal foil and thus produce a winding capacitor.

BeispieleExamples

Beispiel 1example 1

Unter Stickstoffatmosphäre wurden 716 g wasserfreies Ethanol und 284 g (1 Mol) Titantetraisopropoxid (Titantetra-iso-propanolat) unter Rückfluss erhitzt und eine Mischung aus 107,1 g (5/8 Mol) wasserfreiem Bariumhydroxid und 118,3 g (3/8 Mol) Bariumhydroxid-octahydrat zugegeben. Nach 10 h kochen unter Rückfluss wurde die fließfähige Suspension abgekühlt.Under a nitrogen atmosphere 716 g of anhydrous ethanol and 284 g (1 mole) of titanium tetraisopropoxide (Titanium tetra-iso-propanolate) heated under reflux and a mixture from 107.1 g (5/8 mol) of anhydrous barium hydroxide and 118.3 g (3/8 Mol) barium hydroxide octahydrate added. After 10 h cook under backflow became the flowable suspension cooled.

Die Untersuchung der Probe mittels Elektronenmikroskopie ergab sehr regelmäßige Bariumtitanatteilchen von ca. 2 nm Durchmesser. Das Bariumtitanat wies eine kubische Kristallstruktur auf, die Gitterkonstante ao betrug 0,4054 nm.Examination of the sample by means of electron microscopy showed very regular barium titanate particles with a diameter of approx. 2 nm. The barium titanate had a cubic crystal structure, the lattice constant a o was 0.4054 nm.

Ein Teil der Suspension wurde bei einer Temperatur von ca. 180°C sprühgetrocknet. Man erhielt ein sehr feines Bariumtitanat-Pulver mit einem Ba/TiO-Verhältnis von 0,139.Part of the suspension was added a temperature of approx. 180 ° C spray dried. A very fine barium titanate powder with a Ba / TiO ratio of 0.139.

Aus dem getrockneten Pulver wurde durch Verpressen ein Grünkörper mit der Dichte 2,12 g/cm3 hergestellt. Die Probe wurde unter Luft bei 1000°C innerhalb von 5 h zu einem dichten Formkörper mit der Dichte 5,92 g/cm3 gesintert.A green body with a density of 2.12 g / cm 3 was produced from the dried powder by pressing. The sample was sintered in air at 1000 ° C. within 5 h to form a dense shaped body with a density of 5.92 g / cm 3 .

Beispiel 2Example 2

Analog Beispiel 1 wurden 203,8 g Ethylenglykol-mono-n-butylbutylether und 71 g (250 mmol) Titantetraisopropoxid (Titantetra-iso-propanolat) auf 100°C erhitzt und eine Mischung aus 27,9 g (156 mmol) wasserfreiem Bariumhydroxid und 29,6 g (94 mmol) Bariumhydroxid-octahydrat zugegeben. Nach 21 h bei 100°C wurde die fließfähige Suspension abgekühlt.Analogously to Example 1, 203.8 g Ethylene glycol mono-n-butyl butyl ether and 71 g (250 mmol) titanium tetraisopropoxide (Titanium tetra-iso-propanolate) heated to 100 ° C and a mixture from 27.9 g (156 mmol) of anhydrous barium hydroxide and 29.6 g (94 mmol) Barium hydroxide octahydrate added. After 21 h at 100 ° C flowable suspension cooled.

Die Untersuchung der Probe mittels Elektronenmikroskopie ergab Bariumtitanatteilchen von ca. 3 bis 10 nm Durchmesser.Examination of the sample using Electron microscopy showed barium titanate particles from about 3 to 10 nm diameter.

Claims (7)

Verfahren zur Herstellung von Barium- oder Strontiumtitanat, dadurch gekennzeichnet, dass man Titanalkoholate mit Barium- oder Strontiumhydroxid-hydrat in einem C1- bis C8-Alkohol oder einem Glykolether bei einer Temperatur von 50 bis 150°C umsetzt.Process for the preparation of barium or strontium titanate, characterized in that titanium alcoholates are reacted with barium or strontium hydroxide hydrate in a C 1 to C 8 alcohol or a glycol ether at a temperature of 50 to 150 ° C. Verfahren zur Herstellung von Barium- oder Strontiumtitanat nach Anspruch 1, dadurch gekennzeichnet, dass der mittlere Durchmesser der Barium- oder Strontiumtitanat-Teilchen kleiner als 10 nm ist.Process for the production of barium or strontium titanate according to claim 1, characterized in that the average diameter the barium or strontium titanate particle is less than 10 nm. Verfahren zur Herstellung von Barium- oder Strontiumtitanat nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass man als Barium- oder Strontiumhydroxid-hydrat das Octahydrat einsetzt.Process for the production of barium or strontium titanate according to one of the claims 1 or 2, characterized in that as a barium or strontium hydroxide hydrate the octahydrate starts. Verfahren zur Herstellung von Barium- oder Strontiumtitanat nach einem der Ansprüche 1, 2 oder 3, dadurch gekennzeichnet, dass man Gemische aus Barium- oder Strontiumhydroxid und deren Octahydrat einsetzt.Process for the production of barium or strontium titanate according to one of the claims 1, 2 or 3, characterized in that mixtures of barium or strontium hydroxide and its octahydrate. Barium- oder Strontiumtitanat hergestellt nach einem der Ansprüche 1, 2, 3 oder 4, dadurch gekennzeichnet, dass die Barium- oder Strontiumtitanat-Teilchen einen mittleren Durchmesser kleiner als 10 nm aufweisen.Barium or strontium titanate produced according to one of claims 1, 2, 3 or 4, characterized in that the barium or strontium titanate particles have an average diameter of less than 10 nm. Verwendung der Barium- oder Strontiumtitanate nach einem der Ansprüche 1, 2, 3 oder 4 als Dielektrika.Use of the barium or strontium titanates according to one of the Expectations 1, 2, 3 or 4 as dielectrics. Verwendung der Barium- oder Strontiumtitanate nach einem der Ansprüche 1, 2, 3 oder 4 als Dielektrika in Kondensatoren.Use of the barium or strontium titanates according to one of the Expectations 1, 2, 3 or 4 as dielectrics in capacitors.
DE2002132791 2002-05-14 2002-07-18 Production of barium or strontium titanate useful as dielectrics in capacitors comprises reacting a titanium alkoxide with barium or strontium hydroxide hydrate in an alcohol or glycol ether Withdrawn DE10232791A1 (en)

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DE2002132791 DE10232791A1 (en) 2002-07-18 2002-07-18 Production of barium or strontium titanate useful as dielectrics in capacitors comprises reacting a titanium alkoxide with barium or strontium hydroxide hydrate in an alcohol or glycol ether
AT03008675T ATE346825T1 (en) 2002-05-14 2003-04-16 METHOD FOR PRODUCING BARIUM OR STRONTIUM TITANATE WITH AVERAGE DIAMETERS SMALLER THAN 10 NANOMETERS
EP03008675A EP1362830B1 (en) 2002-05-14 2003-04-16 Method for producing barium- or strontium titanate with average diameters lower than 10 nanometer
DE50305808T DE50305808D1 (en) 2002-05-14 2003-04-16 Process for the preparation of barium or strontium titanate with mean diameters less than 10 nanometers
ES03008675T ES2276994T3 (en) 2002-05-14 2003-04-16 PROCEDURE FOR THE PREPARATION OF BARIUM TITANIATE OR STRONTIUM WITH AVERAGE DIAMETERS UNDER 10 NANOMETERS.
US10/435,457 US7223378B2 (en) 2002-05-14 2003-05-12 Preparation of barium titanate or strontium titanate having a mean diameter of less than 10 nanometers
JP2003133887A JP2004131364A (en) 2002-05-14 2003-05-13 Method of manufacturing barium titanate or strontium titanate with mean particle diameter of less than 10 nm

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103359778A (en) * 2013-07-19 2013-10-23 福建中烟工业有限责任公司 Strontium titanate nanotube, its preparation method and application
DE102013000118A1 (en) 2013-01-04 2014-07-10 Hans-Josef Sterzel Electrolytic capacitor has current collectors, open porous electrodes made of n-type semiconductor and metallic conductor, liquid electrolyte and porous spacer for separating electrodes

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013000118A1 (en) 2013-01-04 2014-07-10 Hans-Josef Sterzel Electrolytic capacitor has current collectors, open porous electrodes made of n-type semiconductor and metallic conductor, liquid electrolyte and porous spacer for separating electrodes
CN103359778A (en) * 2013-07-19 2013-10-23 福建中烟工业有限责任公司 Strontium titanate nanotube, its preparation method and application
CN103359778B (en) * 2013-07-19 2015-12-02 福建中烟工业有限责任公司 A kind of strontium titanates nanotube and preparation method and purposes

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