DE10244285A1 - Process for coating a substrate used in the production of dielectrics or ferroelectrics in the manufacture of memory chips in microelectronics comprises applying a suspension onto a substrate, vaporizing the substrate, and sintering - Google Patents

Process for coating a substrate used in the production of dielectrics or ferroelectrics in the manufacture of memory chips in microelectronics comprises applying a suspension onto a substrate, vaporizing the substrate, and sintering Download PDF

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DE10244285A1
DE10244285A1 DE10244285A DE10244285A DE10244285A1 DE 10244285 A1 DE10244285 A1 DE 10244285A1 DE 10244285 A DE10244285 A DE 10244285A DE 10244285 A DE10244285 A DE 10244285A DE 10244285 A1 DE10244285 A1 DE 10244285A1
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substrate
coating
glycol mono
suspension
iso
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BASF SE
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Priority to DE10244285A priority Critical patent/DE10244285A1/en
Priority to KR1020057004899A priority patent/KR20050057540A/en
Priority to PCT/EP2003/009945 priority patent/WO2004028999A2/en
Priority to CNB038226170A priority patent/CN100471996C/en
Priority to JP2004538872A priority patent/JP4183681B2/en
Priority to AU2003273836A priority patent/AU2003273836A1/en
Priority to US10/527,548 priority patent/US20050220993A1/en
Priority to EP03757799A priority patent/EP1546437A2/en
Priority to TW092124896A priority patent/TWI291903B/en
Publication of DE10244285A1 publication Critical patent/DE10244285A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
    • 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
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5042—Zirconium oxides or zirconates; Hafnium oxides or hafnates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
    • H01L21/02197—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides the material having a perovskite structure, e.g. BaTiO3
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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
    • C04B2235/3231—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
    • C04B2235/32—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
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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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
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
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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
    • C04B2235/441—Alkoxides, e.g. methoxide, tert-butoxide

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Abstract

Process for coating a substrate comprises: applying a finely divided suspension having crystalline oxide particles onto a substrate; vaporizing the substrate; and sintering the coating on the substrate.

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Beschichtung eines Substrats durch Beschichten einer feinteiligen, stabilen Suspension kristalliner Oxidteilchen auf das ggf. zu temperierte Substrat, Verdampfen des Suspensionsmittel und Sintern bei erhöhter Temperatur.The present invention relates to a method for coating a substrate by coating a finely divided, stable suspension of crystalline oxide particles on the substrate, if necessary to be tempered, evaporating the suspension medium and sintering at increased Temperature.

Oxidische Materialien hoher Dielektrizitätskonstante wie Bariumtitanat, Strontiumtitanat, Mischtitanate aus Barium und Strontium, Bleizirkontitanate oder Strontiumwismuttantalat werden als Dielektrika bzw. Ferroelektrika für Speicherchips in der Mikroelektronik eingesetzt.Oxidic materials with high dielectric constant such as barium titanate, strontium titanate, mixed titanates of barium and Strontium, lead zirconium titanates or strontium bismuth tantalate as dielectrics or ferroelectrics for memory chips in microelectronics used.

Diese Materialien wirken auf einem Substrat als Dielektrikum, wenn diese als Film in Schichtdicken von ca. 100 nm in kristalliner Form aufgebracht sind. Zur Erzeugung eines Films muss eine Temperaturbehandlung bei 300 bis 1000°C erfolgen.These materials work on you Substrate as a dielectric, if this as a film in layer thicknesses of about 100 nm are applied in crystalline form. For generation a film must be heat treated at 300 to 1000 ° C.

Aus Appl. Phys. A 69, 55–61 (1999) ist bekannt, daß derartige Filme für das ferroelektrische Material SrBi2Ta2O9 nach Mischen und Calcinieren von SrCO3 mit Bi2O3 und Ta2O5 und anschließende Sinterung verpreßter Pellets mittels Laserbestrahlung (Sputtern) auf einem Substrat erhalten werden können. Nachteilig an diesem Verfahren ist, daß sich beim Sputtervorgang die Stöchiometrie des Materials ändern kann und daß damit die Dielektrizitätskonstante oder die permanente Polarisierbarkeit negativ beeinflusst werden.From appl. Phys. A 69, 55-61 (1999) discloses that such films for the ferroelectric material SrBi 2 Ta 2 O 9 after mixing and calcining SrCO 3 with Bi 2 O 3 and Ta 2 O 5 and subsequent sintering of pressed pellets by means of laser radiation ( Sputtering) can be obtained on a substrate. A disadvantage of this method is that the stoichiometry of the material can change during the sputtering process and that the dielectric constant or the permanent polarizability are thereby adversely affected.

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 Beschichtung eines Substrats gefunden, welches dadurch gekennzeichnet ist, daß man durch Beschichten eine feinteilige Suspension kristalliner Oxidteilchen auf ein Substrat aufgringt, das Suspensionsmittel verdampft und die Beschichtung auf dem Substrat sintert.Accordingly, a new and improved one Process for coating a substrate found, which thereby is characterized in that one by coating a finely divided suspension of crystalline oxide particles on a substrate, the suspending agent evaporates and the coating sinters on the substrate.

Das erfindungsgemäße Verfahren kann wie folgt durchgeführt werden:
Die Oxid-Suspensionen können durch geeigneten Vorrichtung wie Sprühdüsen auf ein Substrat versprüht werden, das man gegebenenfalls so hoch temperiert, dass das Suspensionsmittel verdampft. Die Verdampfung kann auch in einem separaten Schritt durch anschließende Erwärmung erfolgen. Ein homogener Sprühkegel kann erreicht werden, indem man die Sprühdüse(n) an einen Ultraschallschwinger ankoppelt oder bei der Dosierung eine Ultraschallschwingung überlagert oder die Suspension auf eine geeignet geformten Ultraschallschwinger dosiert. Das Versprühen der ggf. mäßig temperierten (Temperatur von Raumtemperatur bis unterhalb des Siedepunkts des Suspensionsmittels) Suspension kann in einer Zweistoffdüse durch ein Hilfsgas (wie beispielsweise Stickstoff oder Argon) erreicht werden und/oder indem man den Sprühvorgang beispielsweise durch überlagerte Ultraschallschwingungen unterstützt.The method according to the invention can be carried out as follows:
The oxide suspensions can be sprayed onto a substrate by means of a suitable device, such as spray nozzles, which is optionally heated to such a high temperature that the suspension medium evaporates. Evaporation can also be carried out in a separate step by subsequent heating. A homogeneous spray cone can be achieved by coupling the spray nozzle (s) to an ultrasonic oscillator or by superimposing an ultrasonic oscillation during dosing or by metering the suspension onto a suitably shaped ultrasonic oscillator. The spraying of the optionally moderately tempered (temperature from room temperature to below the boiling point of the suspension medium) suspension can be achieved in a two-component nozzle by means of an auxiliary gas (such as nitrogen or argon) and / or by supporting the spraying process, for example, by superimposed ultrasonic vibrations.

Das Beschichten kann durch Aufsprühen oder durch einen Spin-On-Prozess, bei welchem eine bestimmte Menge fließfähiger Suspensionan einer beliebigen Stelle, beispielsweise in Zentrum, eines rotierenden Substrats dosiert wird und die Suspension sich aufgrund der Fliehkraft über das Substrat gleichmäßig verteilt.The coating can be by spraying or through a spin-on process, in which a certain amount of flowable suspension on any one Place metered, for example in the center, of a rotating substrate is and the suspension due to the centrifugal force over the Evenly distributed substrate.

Nach erfolgter Abscheidung der Oxid-Suspension auf dem Substrat kann das System auf die dem Oxid adäquate Kristallisationstemperatur erhitzt und durch Zusammensintern der Nano-Teilchen der erwünschte zusammenhängende Film erzeugt werden.After the oxide suspension has been separated on the substrate the system can reach the crystallization temperature adequate for the oxide heated and by sintering together the nano-particles the desired coherent film be generated.

Die Sintertemperaturen für Nanoteilchen liegen in der Regel deutlich unterhalb der Sintertemperatur für Teilchen im Mikrometermaßstab. So liegt beispielsweise für BaTiO3-Teilchen die Sintertemperatur bei Nanoteilchen (Korngrößen von 2 bis 5 nm) bei ca. 750°C im Gegensatz zu Mikrometerteilchen (Korngrößen von 2 bis 5 μm) bei ca. 1350°C.The sintering temperatures for nanoparticles are generally well below the sintering temperature for particles on the micrometer scale. For example, for BaTiO 3 particles, the sintering temperature for nanoparticles (grain sizes from 2 to 5 nm) is approx. 750 ° C in contrast to micrometer particles (grain sizes of 2 to 5 μm) at approx. 1350 ° C.

Eine Änderung der Stöchiometrie der aufgebrachten Oxide wie bei anderen Verfahren erfolgt nicht. Damit werden Filme mit überlegenen dielektrischen bzw. ferroelektrischen Eigenschaften erhalten.A change in stoichiometry the oxides applied, as in other processes, do not take place. This makes films with superior obtained dielectric or ferroelectric properties.

Bei den Suspensionen feinteiliger, kristalliner Oxidteilchen werden in der Regel Wasser oder organische Suspensionsmittel eingesetzt, die die Oxidteilchen mit einer mittleren Teilchengrößen von 0,5 bis 9,9 nm, vorzugsweise von 0,6 bis 9 nm, besonders bevorzugt von 1 bis 8 nm enthalten. Die Oxidteilchen sind beispielsweise BaTiO3, SrTiO3, Bax Sr1_x TiO3 mit x = 0,01 bis 0,99, Pb (ZrxTi1_x) O3 mit x = 0,01 bis 0, 99 oder Sr Bi2Ta2O9.In the suspensions of finely divided, crystalline oxide particles, water or organic suspension media are generally used, which give the oxide particles an average particle size of 0.5 to 9.9 nm, preferably 0.6 to 9 nm, particularly preferably 1 to 8 nm contain. The oxide particles are, for example, BaTiO 3 , SrTiO 3 , Ba x Sr 1 _ x TiO 3 with x = 0.01 to 0.99, Pb (Zr x Ti 1 _ x ) O 3 with x = 0.01 to 0.99 or Sr Bi 2 Ta 2 O 9 .

Als Substrate eignen sich in der Regel Wafer aus Reinstsilizium, die bereits strukturiert sind, wobei die Strukturierung nach dem bekannten "Damascene"-Verfahren erfolgt. Die eigentlichen Substratschichten sind elektrisch leitende Schichten, die im Rahmen des Damascene-Prozesses erzeugt werden.Suitable substrates are in the Rule of ultra-pure silicon, which are already structured, the Structuring takes place according to the well-known "Damascene" process. The real ones Substrate layers are electrically conductive layers that are in the frame of the Damascene process.

Als organische Suspensionsmittel eignen sich in der Regel polare organische Suspensionsmittel, besonders aliphatische Alkohole, Etheralkohole oder deren Gemische mit einem Siedepunkt unterhalb von ca. 300°C unter Normaldruck. Diese können wasserfrei oder bevorzugt in handelsüblicher wäßriger Form eingesetzt werden.As an organic suspending agent As a rule, polar organic suspending agents are particularly suitable aliphatic alcohols, ether alcohols or mixtures thereof with one Boiling point below approx. 300 ° C under normal pressure. These can be anhydrous or preferably in commercial aqueous form be used.

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, especially methanol or ethanol.

Als Etheralkohole eignen sich alle bekannten Glykolether wie beispielsweise Ethylenglykol-mono-methylether, Ethylenglykol-mono-ethylether, Ethylenglykol-mono-n-propylether, Ethylenglykol-mono-iso-propylether, Ethylenglykol-mino-n-butylether, Ethylenglykol-mono-iso-butylether, Ethylenglykol-mono-sec.-butylether, Ethylenglykol-tert.-butylether, Diethylenglykolmino-methylether, Diethylenglykol-mono-ethylether, Diethylenglykol-mono-n-propylether, Diethylenglykol-mono-iso-propylether, Diethylenglykol-mono-n-butylether, Diethylenglykol-mono-iso-butylether, Diethlyenglykol-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-ethylether, Diethylenglykol-mono-n-propylether, Diethlyenglykol-mono-iso-propylether, Diethylenglykol-mono-n-butylether, Diethylenglykol-mono-iso-butylether, Diethylengykol-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.Suitable ether alcohols are all known glycol ethers such as, for example, ethylene glycol mono-methyl ether, ethylene glycol mono-ethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mino-n-bu tyl ether, ethylene glycol mono-iso-butyl ether, ethylene glycol mono-sec-butyl ether, ethylene glycol tert-butyl ether, diethylene glycol amino 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 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-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 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.

Der Feststoffgehalt der Suspensionen kann in weiten Grenzen variiert werden, beträgt in der Regel 1 bis 35 Gew.-%, bevorzugt 5 bis 25 Gew.-%, und kann in der Synthese der Suspensionen oder nachträglich durch Verdünnen oder Aufkonzentrieren eingestellt werden.The solids content of the suspensions can be varied within wide limits, is usually 1 to 35% by weight, preferably 5 to 25 wt .-%, and can in the synthesis of the suspensions or later by dilution or concentrate.

Die nanokristallinen Oxid-Suspensionen können wie folgt hergestellt werden:
Man kann Titanalkoholate in einem Alkanol, 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 nanocrystalline oxide suspensions can be produced as follows:
Titanium alcoholates can be introduced in an alkanol, 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 React 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, ganz 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, entirely particularly preferably at 200 to 400 g / liter.

Als Barium- oder Strontiumhydroxidhydrate 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, Titan-butanolat, Titantetra-sec.-butanolat und Titantetra-tert.-butanolat, besonders bevorzugt Titan-tetra-n-propanolat, Titan-tetra-iso-propanolat, Titantetra-n-butanolat und Titrantetra-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-iso-pentanolate, preferably titanium tetraethanolate, titanium tetra-n-propanolate, titanium butanolate, titanium tetra-sec-butanolate and titanium tetra-tert-butanolate, particularly preferably titanium tetra-n-propanolate, Titanium tetra-iso-propanolate, titanium tetra-n-butanolate and titrantetra-iso-butanolate or their mixtures.

Zur Herstellung von Ba(Zrx Ti1_x)O3 oder Sr (Zrx Ti1_x) O3-Oxide werden anstelle des reinen Titanalkoxids die Mischungen mit Zirkonalkoxiden eingesetzt und die bereits beschriebenen Bedingungen verwendet.In order to produce Ba (Zr x Ti 1 _ x ) O 3 or Sr (Zr x Ti 1 _ x ) O 3 oxides, the mixtures with zirconium alkoxides are used instead of the pure titanium alkoxide and the conditions already described are used.

Als Zirkonalkoxide werden die kommerziell zugänglichen Alkoxide, bevorzugt Zirkontetraisobutylat und/oder Zirkontetra-n-butylat eingesetzt.The commercially available zirconium alkoxides Alkoxides, preferably zirconium tetraisobutylate and / or zirconium tetra-n-butoxide used.

Zur Herstellung der Pb(Zrx T1_x)O3-Oxide setzt man in der Regel als Bleikomponente Bleiacetattrihydrat oder in Mischung das basische Bleiacetat [Pb(OAc)2·Pb(OH)2] ein. Durch das Mischungsverhältnis von Bleiacetattrihydrat und basischem Bleiacetat kann der Anteil des Reaktionswassers vorgegeben werden, wobei die Acetat-Reste als Essigsäure abgespalten werden und diese mit dem im Suspensionsmittel als Komponente vorhandenen Alkohol unter Esterbildung weiteres Wasser liefert. Die Zugabe von geringen Mengen zusätzlicher Essigsäure zur Bildung von Reaktionswasser kann gegebenenfalls vorteilhaft sein.To produce the Pb (Zr x T 1 _ x ) O 3 oxides, lead acetate trihydrate is generally used as the lead component or, in a mixture, the basic lead acetate [Pb (OAc) 2 .Pb (OH) 2 ]. The proportion of the water of reaction can be predetermined by the mixing ratio of lead acetate trihydrate and basic lead acetate, the acetate residues being split off as acetic acid and this, together with the alcohol present as a component in the suspension medium, providing further water with ester formation. The addition of small amounts of additional acetic acid to form water of reaction may be advantageous.

Zur Herstellung von SrBi2Ta2O9 setzt man in der Regel als Alkoxid das kommerziell erhältliche Tantalpentaethoxid Ta(OC2H5)5 ein, als Sr-Komponente vorzugsweise Sr(OH)2·8H2O, gegebenenfalls in Mischung mit wasserfreiem Sr(OH)2, und als Wismutkomponente Bi(OCOCH3)3 oder Wismuthydroxid Bi(OH)3.To produce SrBi 2 Ta 2 O 9 , the commercially available tantalum pentaethoxide Ta (OC 2 H 5 ) 5 is generally used as the alkoxide, preferably Sr (OH) 2 .8H 2 O as the Sr component, optionally in a mixture with anhydrous Sr (OH) 2 , and as bismuth component Bi (OCOCH 3 ) 3 or bismuth hydroxide Bi (OH) 3 .

Es kann vorteilhaft sein, das Eintragen der Feststoffe durch kräftiges Rühren zu unterstützen.It may be advantageous to register the solids by vigorous stir to support.

Eine vorteilhafte Ausführungsform besteht darin, dass in die Oxid-Suspensionen kein zusätzliches Wasser außer dem Wasser aus den Komponenten und dem Suspensionsmittel in die Umsetzung eingetragen wird.An advantageous embodiment is that there is no additional in the oxide suspensions Water except the water from the components and the suspending agent into the Implementation is entered.

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 Mischoxide haben in der Regel einen mittleren Teilchendurchmesser von kleiner als 10 nm, bevorzugt, 5 bis 9,9 nm, besonders bevorzugt 0,6 bis 9 nm, insbesondere 1 bis 8 nm.The mixed oxides produced according to the invention usually have an average particle diameter of smaller than 10 nm, preferably 5 to 9.9 nm, particularly preferably 0.6 to 9 nm, in particular 1 to 8 nm.

Mit dem erfindungsgemäße Verfahren kann man zu dielektrischen Schichten für DRAMs (Dynamic Random Access Memories), beispielsweise Titanate, BaTiO3, SrTiO3 sowie Ba1_x Srx TiO3 (x = 0,01 bis 0,99) bzw. ferroelektrischen Schichten für FeRAMs, beispielsweise Pb (Zr1_x Tix) O3 mit x = 0,01 bis 0,99 oder SrBi2Ta2O9 gelangen, die ohne Änderung der Stöchiometrie zu überlegenen dielektrischen bzw. ferroelektrischen Eigenschaften führen.The method according to the invention can be used to form dielectric layers for DRAMs (Dynamic Random Access Memories), for example titanates, BaTiO 3 , SrTiO 3 and Ba 1 _ x Sr x TiO 3 (x = 0.01 to 0.99) or ferroelectric layers for Fe RAMs, for example Pb (Zr 1 _ x Ti x ) O 3 with x = 0.01 to 0.99 or SrBi 2 Ta 2 O 9 , which lead to superior dielectric or ferroelectric properties without changing the stoichiometry.

BeispieleExamples

Beispiel 1example 1

Herstellung einer nanoteiligen Ba-Titanat-Suspensionmanufacturing a nanopartic Ba titanate suspension

Zu 844 g Butylglykol wurden nacheinander 335,6 g Titantetrabutylat und 79,6 g Ba(OH)2 × 8 H2O mit 128,4 g Ba(OH)2 schnell zugegeben und 48 h bei 120°C gerührt. Man erhielt eine Ba-Titanat-Suspensionen hochkristalline Teilchen mit einer mittleren Teilchengröße von 4 bis 6 nm.335.6 g of titanium tetrabutylate and 79.6 g of Ba (OH) 2 × 8 H 2 O with 128.4 g of Ba (OH) 2 were rapidly added to 844 g of butyl glycol and the mixture was stirred at 120 ° C. for 48 h. A Ba titanate suspension of highly crystalline particles with an average particle size of 4 to 6 nm was obtained.

Beispiel 2Example 2

Herstellung einer nanoteiligen SrBi2Ta2O9-Suspension von < 10 nmProduction of a nanoparticle SrBi 2 Ta 2 O 9 suspension of <10 nm

Zu 110 g Butylglykol wurden nacheinander 40,6 g Tantal-ethylat, 4,6 g Sr(OH)2 (Sr-Gehalt: 70,4 Gew.-%), 3,35 g Sr(OH)2 × H2O und 26 g Bi(OH)3 zugegeben, 48 h unter Rückfluss (104°C) gerührt. Man erhielt eine kristalline SrBi2Ta2O9-Suspension mit einer mittleren Teilchengröße von 5 nm.40.6 g of tantalum ethylate, 4.6 g of Sr (OH) 2 (Sr content: 70.4% by weight), 3.35 g of Sr (OH) 2 × H 2 O were added to 110 g of butyl glycol and 26 g of Bi (OH) 3 were added, the mixture was stirred under reflux (104 ° C.) for 48 h. A crystalline SrBi 2 Ta 2 O 9 suspension with an average particle size of 5 nm was obtained.

Beispiel 3Example 3

Herstellung einer nanaoteiligen SrBi2Ta2O9-Suspension von < 10 nmPreparation of a nanoparticle SrBi 2 Ta 2 O 9 suspension of <10 nm

Zu 110 g Butylglykol wurden nacheinander 40,6 g Tantal-ethylat, 1,55 g Sr(OH)2 (Sr-Gehalt: 70,4 Gew.-%), 10 g Sr(OH)2 × H2O und 26 g Bi(OH)3 zugegeben, 48 h unter Rückfluss (104°C) gerührt.40.6 g of tantalum ethylate, 1.55 g of Sr (OH) 2 (Sr content: 70.4% by weight), 10 g of Sr (OH) 2 × H 2 O and 26 were successively added to 110 g of butyl glycol g Bi (OH) 3 added, stirred under reflux (104 ° C.) for 48 h.

Man erhielt eine kristalline SrBi2Ta2O9-Suspension mit einer mittleren Teilchengröße von 8 nm.A crystalline SrBi 2 Ta 2 O 9 suspension with an average particle size of 8 nm was obtained.

Beispiel 4Example 4

Herstellung einer nanoteiligen Pb(Zr0,53Ti0,47)O3-SuspensionProduction of a nanoparticulate Pb (Zr 0.53 Ti 0.47 ) O 3 suspension

Zu 211 g Butylglykol wurden nacheinander 49,6 g Zr(OC3H7)4, 31,5 g Ti(OC4H9)4 und 75,8 g Pb(OCOCH3)2 × 3 H2O zugegeben und 24 h bei 80°C und 24 h bei 120°C gerührt. Man erhielt eine kristalline Pb(Zr0,53Ti0,47)O3-Suspension mit einer mittleren Teilchengröße von 2 bis 3 nm.49.6 g of Zr (OC 3 H 7 ) 4 , 31.5 g of Ti (OC 4 H 9 ) 4 and 75.8 g of Pb (OCOCH 3 ) 2 × 3 H 2 O were successively added to 211 g of butyl glycol and 24 h at 80 ° C and 24 h at 120 ° C. A crystalline Pb (Zr 0.53 Ti 0.47 ) O 3 suspension with an average particle size of 2 to 3 nm was obtained.

Beispiel 5Example 5

Herstellung einer nanoteiligen Pb(Zr0,53Ti0,47)O3-SuspensionProduction of a nanoparticulate Pb (Zr 0.53 Ti 0.47 ) O 3 suspension

Zu 211 g Butylglykol wurden nacheinander 49,6 g Zr(OC3H7)4, 31,5 g Ti(OC4H9)4, 24 g Essigsäure (100%-ig) und 75,8 g Pb(OCOCH3)2 × 3 H2O zugegeben und 24 h bei 80°C und 24 h bei 120°C gerührt . Man erhielt eine kristalline Pb (Zr0,53,Ti0,47)O3-Suspension mit einer mittleren Teilchengröße von 3 bis 4 nm.49.6 g of Zr (OC 3 H 7 ) 4 , 31.5 g of Ti (OC 4 H 9 ) 4 , 24 g of acetic acid (100%) and 75.8 g of Pb (OCOCH 3 ) 2 × 3 H 2 O and stirred for 24 h at 80 ° C and 24 h at 120 ° C. A crystalline Pb (Zr 0.53 , Ti 0.47 ) O 3 suspension with an average particle size of 3 to 4 nm was obtained.

Beispiel 6Example 6

Herstellung einer nanoteiligen Pb(Zr0,53Ti0,47)O3-SuspensionProduction of a nanoparticulate Pb (Zr 0.53 Ti 0.47 ) O 3 suspension

Zu 211 g Butylglykol wurden nacheinander 48,5 g Zr(OC4H9)4, 31,5 g Ti(OC4H9)4 und 75,8 g Pb(OCOCH3)2 × 3 H2O zugegeben und 72 h bei 120°C gerührt. Man erhielt eine kristalline Pb (Zr0,53,Ti0,47)O3-Suspension mit einer mittleren Teilchengröße von 2 bis 3 nm.48.5 g of Zr (OC 4 H 9 ) 4 , 31.5 g of Ti (OC 4 H 9 ) 4 and 75.8 g of Pb (OCOCH 3 ) 2 × 3 H 2 O were added in succession to 211 g of butyl glycol and 72 h at 120 ° C stirred. A crystalline Pb (Zr 0.53 , Ti 0.47 ) O 3 suspension with an average particle size of 2 to 3 nm was obtained.

Claims (4)

Verfahren zur Beschichtung eines Substrats, dadurch gekennzeichnet, daß man durch Beschichtung eine feinteilige Suspension kristalliner Oxidteilchen auf ein Substrat aufbringt, das Suspensionsmittel verdampft und die Beschichtung auf dem Substrat sintert.A method of coating a substrate, characterized in that a finely divided suspension of crystalline oxide particles is applied to a substrate by coating, the suspension medium evaporates and the coating is sintered on the substrate. Verfahren zur Beschichtung eines Substrats nach Anspruch 1, dadurch gekennzeichnet, daß man Oxidteilchen mit einer mittleren Teichengröße von 0,5 bis 9,9 nm einsetzt.A method of coating a substrate according to claim 1, characterized in that oxide particles with an average pond size of 0.5 to 9.9 nm. Verfahren zur Beschichtung eines Substrats einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß man als Oxidteilchen BaTiO3, SrTiO3, Bax Sr1_x TiO3 mit x = 0,01 bis 0,99, Pb (ZrxTi1_x) 03 mit x = 0,01 bis 0,99 oder Sr Bi2Ta2O9 einsetzt.Process for coating a substrate according to one of claims 1 or 2, characterized in that BaTiO 3 , SrTiO 3 , Ba x Sr 1 _ x TiO 3 with x = 0.01 to 0.99, Pb (Zr x Ti 1 _ x ) 03 with x = 0.01 to 0.99 or Sr Bi 2 Ta 2 O 9 . Verfahren zur Beschichtung eines Substrats einem der Ansprüche 1, 2 oder 3, dadurch gekennzeichnet, daß man als Suspensionsmittel Alkohole oder Glykolether einsetzt.Process for coating a substrate of claims 1, 2 or 3, characterized in that one as a suspending agent Alcohols or glycol ethers are used.
DE10244285A 2002-09-23 2002-09-23 Process for coating a substrate used in the production of dielectrics or ferroelectrics in the manufacture of memory chips in microelectronics comprises applying a suspension onto a substrate, vaporizing the substrate, and sintering Withdrawn DE10244285A1 (en)

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DE10244285A DE10244285A1 (en) 2002-09-23 2002-09-23 Process for coating a substrate used in the production of dielectrics or ferroelectrics in the manufacture of memory chips in microelectronics comprises applying a suspension onto a substrate, vaporizing the substrate, and sintering
KR1020057004899A KR20050057540A (en) 2002-09-23 2003-09-08 Thin films of oxidic materials having a high dielectric constant
PCT/EP2003/009945 WO2004028999A2 (en) 2002-09-23 2003-09-08 Thin films of oxidic materials having a high dielectric constant
CNB038226170A CN100471996C (en) 2002-09-23 2003-09-08 Thin film of oxidic materials having a high dielectric constant
JP2004538872A JP4183681B2 (en) 2002-09-23 2003-09-08 Thin film of oxide material with high dielectric constant
AU2003273836A AU2003273836A1 (en) 2002-09-23 2003-09-08 Thin films of oxidic materials having a high dielectric constant
US10/527,548 US20050220993A1 (en) 2002-09-23 2003-09-08 Thin film of oxidic materials having a high dielectric constant
EP03757799A EP1546437A2 (en) 2002-09-23 2003-09-08 Thin films of oxidic materials having a high dielectric constant
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102482114A (en) * 2009-04-08 2012-05-30 利物浦大学 Mixed metal oxides

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