WO2002016508A2 - Sphärische metalloxidpartikel mit partikulären oberflächenerhebungen und verfahren zu dessen herstellung sowie deren verwendung - Google Patents
Sphärische metalloxidpartikel mit partikulären oberflächenerhebungen und verfahren zu dessen herstellung sowie deren verwendung Download PDFInfo
- Publication number
- WO2002016508A2 WO2002016508A2 PCT/EP2001/009608 EP0109608W WO0216508A2 WO 2002016508 A2 WO2002016508 A2 WO 2002016508A2 EP 0109608 W EP0109608 W EP 0109608W WO 0216508 A2 WO0216508 A2 WO 0216508A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- metal oxide
- particles
- oxide particles
- spherical
- compounds
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3045—Treatment with inorganic compounds
- C09C1/3054—Coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
Definitions
- the object with respect to the spherical particles is achieved by the characterizing features of claim 1 and in relation to the method for production by the features of claim 7 and in terms of use by the features of claim 19.
- metal oxide particles according to the invention have the particular structure on the surface described in more detail above.
- the particles according to the invention prove to be particularly advantageous when they are used in a composite.
- the integration of the particles is apparently significantly improved by the physical effect (push button effect) compared to the known particles without surveys.
- the elevations on the surface thus obviously lead to interlocking and / or interlocking with the matrix of the composite. It should also be emphasized that this surprising effect occurs in addition to the chemical bonding known from the prior art.
- the surface modification is preferably obtained by partial or complete hydrolytic condensation of one or more hydrolytically condensable compounds of silicon and possibly other elements from the group boron, aluminum, phosphorus, tin, lead, the transition metals, the lanthanides and the actinides and / or Pre-condensates derived from the abovementioned compounds, if appropriate in the presence of a catalyst and / or a solvent by the action of water or moisture.
- connection of the connections to the party kel which are obtained by the condensation described above, takes place via reactive groups, such as OH groups on the surface.
- reactive groups such as OH groups on the surface.
- This surface modification is already known from DE 196 43 781.4 AI. The content of the disclosure of this document is therefore referred to in full.
- R alkyl, alkenyl, aryl, alkylaryl, or
- Arylalkyl R '' alkylene, or alkenylene, these radicals
- R alkyl, alkenyl, aryl, alkylaryl, or arylalkyl
- R '' alkylene or alkenylene, where these radicals can contain oxygen, sulfur atoms and / or amino groups,
- Z ' halogen or an optionally substituted amino, amide, aldehyde, alkylcarbonyl, carboxy, mercapto, Cyano, alkoxy, alkoxycarbonyl, sulfonic acid, phosphoric acid, acryloxy, methacryloxy, epoxy or vinyl group,
- a 0, 1, 2, or 3
- c 2, 4.
- R alkyl, alkenyl, aryl, alkylaryl, or
- Arylalkyl R '' alkylene, or alkenylene, where these radicals can contain oxygen, sulfur atoms and / or amino groups
- Z ' halogen or an optionally sub- substituted amino, amide, aldehyde, alkylcarbonyl, carboxy, mercapto, cyano, alkoxy, alkoxycarbonyl, sulfonic acid, phosphoric acid, acryloxy, methacryloxy, epoxy or vinyl group
- a 0 , 1, 2, or 3
- R alkyl, alkenyl, aryl, alkylaryl or arylalkyl
- R ' alkylene, arylene or alkylenearylene
- R' ' hydrogen, alkyl or aryl
- X hydrogen, halogen, hydroxy, alkoxy
- alkyl or alkenyl radicals are optionally substituted straight-chain, branched or cyclic radicals having 1 to 20 carbon atoms and may contain oxygen, sulfur atoms and / or amino groups
- aryl for optionally substituted phenyl, naphthyl or biphenyl and the above alkoxy, acyloxy, alkylcarbonyl, alkoxycarbonyl, alkylaryl, arylalkyl, arylene, alkylene and alkylenearyl radicals are derived from the alkyl and aryl radicals defined above.
- radicals and indices may be the same or different and have the following meaning:
- X hydrogen, halogen, hydroxy, alkoxy,
- R alkyl, alkenyl, aryl, alkylaryl or arylalkyl;
- R ' alkylene, arylene, arylene alkylene or alkylene arylene each having 0 to 10 carbon atoms, these radicals being able to contain oxygen, sulfur atoms and / or amino groups;
- R 2 H or COOH
- R optionally alkylene, arylene or alkylene arylene containing oxygen, sulfur atoms and / or amino groups, each having 1 to 10 carbon atoms and
- radicals and indices here may be the same or different and have the following meaning:
- X hydrogen, halogen, hydroxy, alkoxy,
- R alkyl, alkenyl, aryl, alkylaryl or arylalkyl
- R ' alkylene, arylene, arylene alkylene or alkylene arylene each having 0 to 10 carbon atoms, where these radicals can contain oxygen, sulfur atoms and / or amino groups
- R ′′ alkylene, arylene, arylene alkylene or alkylene arylene and in each case 1 to 10 c atoms, it being possible for these radicals to contain oxygen, sulfur atoms and / or amino groups.
- R alkyl, alkenyl, aryl, alkylaryl or
- Arylalkyl, X hydrogen, halogen, hydroxy, alkoxy,
- radicals and indices can be the same or different and have the following meaning:
- R hydrogen, R ⁇ -R ⁇ R ⁇ SiXxR 3 ⁇ x 1 / Carboxyl, alkyl, alkenyl, aryl, alkylaryl or arylalkyl each having 1 to 15 hydrocarbon atoms, where these radicals can contain oxygen or sulfur atoms, ester, carbonyl, amide or amino groups;
- R alkylene, arylene, arylene alkylene or alkylene, each having 0 to 15 carbon atoms, where these radicals can contain oxygen or sulfur atoms, ester, carbonyl, amide or amino groups;
- R alkylene, arylene, arylene alkylene or alkyl arylene each having 0 to 15 carbon atoms, where these radicals can contain oxygen or sulfur atoms, ester, carbonyl, amide or amino groups;
- R 3 alkyl, alkenyl, aryl, alkylaryl or
- Arylalkyl each having 1 to 15 carbon atoms, where these radicals can contain oxygen or sulfur atoms, ester, carbonyl, amide or amino groups;
- R alkylene, arylene, arylene alkylene or alkyl arylene each having 1 to 15 carbon atoms, these radicals being oxygen or May contain sulfur atoms, ester, carbonyl, amide or amino groups;
- R hydrogen, alkyl or aryl with 1 to 10 carbon atoms
- R 9 hydrogen, alkyl, alkenyl, aryl, alkylaryl or arylalkyl each having 1 to 15 carbon atoms, where these radicals can contain oxygen or sulfur atoms, ester, carbonyl, amide or amino groups;
- X hydrogen, halogen, hydroxy, alkoxy,
- R' hydrogen, alkyl or aryl
- the Si compounds used allow great variability in the targeted influencing of the properties. In addition to the proportion of solids, they can influence the mechanical properties, such as the impact strength of the composite.
- the functional groups eg polymerizable double bonds which are present in relatively large numbers ensure a good one Integration of the filler in the resin or composite.
- Method acrylate groups have a larger elasticity module (modulus of elasticity) and a smaller coefficient of thermal expansion. With a larger number of alkoxy groups, a greater modulus of elasticity and a smaller thermal expansion coefficient can also be achieved.
- the monomers mentioned in Examples 1 and 2 which are derived from the general formulas I and II, can also be used for a desired modification in the interior of the spherical particles according to the invention, where a + b can also be 0 here.
- Water glass solutions can also be used for modification inside.
- the invention further relates to a method for producing spherical particles with a particulate surface.
- the procedure is such that in a first step the metal oxide particles are used according to methods known per se, such as e.g. the sol-gel process, especially the Stöber, the emulsion or Aerosol processes (e.g. spray drying) are produced and then in a subsequent one
- the metal oxide particles are used according to methods known per se, such as e.g. the sol-gel process, especially the Stöber, the emulsion or Aerosol processes (e.g. spray drying) are produced and then in a subsequent one
- Step the particles thus produced are treated energetically.
- the corresponding particulate structures in the form of an "hedgehog-like" formation result from the energetic treatment, for example tempering, laser beam treatment and / or electron beam treatment (see FIG. 2).
- the annealing can preferably be carried out by a temperature treatment in the range from 600 ° C. to 1000 ° C. over a period of 10 minutes to 90 minutes.
- the metal oxide particles themselves are produced by previously known processes. For this purpose, DE 42 19 287 AI, EP 0 391 447 B1 and CO co F * c ⁇ o c ⁇ o c ⁇ o C ⁇
- Salting of long-chain organic acids of selected compounds is effected before, during or after the formation of the emulsion, the compound in question either already being in the OH or H form or being generated in situ, whereupon the water is removed by distillation.
- small particles can be embedded in larger particles, the matrix of which consists of the same or a different oxide, in order to obtain a composite structure of the particles.
- Such a structure can also be achieved if small particles grow on large ones.
- Particles with a homogeneous distribution of different oxides in the respective particle can be obtained by joint hydrolysis and condensation with different metal oxide precursors (e.g. metal alcoholates, alkyl carbonyls).
- metal oxide precursors e.g. metal alcoholates, alkyl carbonyls.
- Metal oxide particles are preferably produced which contain an oxide of the metals Si, Sn, Ti, Zr, Al or Sr or a mixture thereof.
- a metal oxide particle is shown schematically, the heterogeneous areas i.e. Contains nanoparticles.
- the surface formation corresponds to the type in Fig. A.
- FIG. 1c shows a particle which has a homogeneous distribution in the interior and the exterior again has the particulate surface design which is already known from FIGS.
- a 10% by weight alcoholic solution of tin (IV) tert-butoxide is added all at once to an alcoholic dispersion containing 1% by weight of SiO 2 cores and heated to boiling over a period of 4 hours. After cooling to RT, a 1% water-containing, alcoholic solution is metered in at a rate of 0.02 ml / min. The dispersion is slowly stirred within the next 3 hours. The particles are then isolated by centrifugation and washed twice with alcohol using redispersion / centrifugation cycles.
- the Sn0 2 -coated Si0 2 particles are thermally treated in the oven at 700 ° C. for 60 minutes.
- the images obtained in the transmission electron microscope are shown in FIG. 2 as a function of the treatment time.
- Sn0 2 coated Si0 2 particles from Example 1 are focused in the transmission electron microscope. Pictures are taken at intervals of approx. 15 seconds over a period of a few minutes. The images obtained correspond to those from Example 2, with the difference that the treatment times between the individual photos are only about 15 seconds.
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2001295493A AU2001295493A1 (en) | 2000-08-22 | 2001-08-21 | Spherical metal oxide particles comprising particulate surface prominences, a method for producing the same and the use thereof |
US10/362,299 US20040023040A1 (en) | 2000-08-22 | 2001-08-21 | Spherical metal oxide particles comprising particulate surface prominences, a method for producing the same and the use thereof |
EP01976121A EP1311626A2 (de) | 2000-08-22 | 2001-08-21 | Sphärische metalloxidpartikel mit partikulären oberflächenerhebungen und verfahren zu dessen herstellung sowie deren verwendung |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10041038A DE10041038B4 (de) | 2000-08-22 | 2000-08-22 | Sphärische Metalloxidpartikel mit partikulären Oberflächenerhebungen und Verfahren zu dessen Herstellung sowie deren Verwendung |
DE10041038.3 | 2000-08-22 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2002016508A2 true WO2002016508A2 (de) | 2002-02-28 |
WO2002016508A3 WO2002016508A3 (de) | 2002-05-23 |
Family
ID=7653289
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2001/009608 WO2002016508A2 (de) | 2000-08-22 | 2001-08-21 | Sphärische metalloxidpartikel mit partikulären oberflächenerhebungen und verfahren zu dessen herstellung sowie deren verwendung |
Country Status (5)
Country | Link |
---|---|
US (1) | US20040023040A1 (de) |
EP (1) | EP1311626A2 (de) |
AU (1) | AU2001295493A1 (de) |
DE (1) | DE10041038B4 (de) |
WO (1) | WO2002016508A2 (de) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004065495A3 (en) * | 2003-01-24 | 2006-01-19 | Showa Denko Kk | Surface modification method for inorganic oxide powder, powder produced by the method and use of the powder |
RU2599668C2 (ru) * | 2012-02-09 | 2016-10-10 | Омиа Интернэшнл Аг | Композиция и способ для регулирования смачиваемости поверхностей |
CN114634801A (zh) * | 2022-03-10 | 2022-06-17 | 中国石油大学(华东) | 一种油基钻井液用两亲纳米二氧化硅固体乳化剂及其制备方法与应用 |
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DE102005018059A1 (de) | 2003-10-24 | 2006-10-26 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zum Verbrücken von Hydroxy- oder Carbonsäuregruppen enthaltenden, organisch polymerisierbaren Silanen oder Silanharzeinheiten, sowie Produkte dieses Verfahrens |
DE10353555A1 (de) | 2003-11-14 | 2005-06-30 | Carl Freudenberg Kg | Teilchenverbund, Verfahren zu deren Herstellung und deren Verwendung |
US20060189707A1 (en) * | 2005-02-24 | 2006-08-24 | Norbert Abels | Kits and methods for coating a dental filling material to increase wear resistance and durability |
CN101146880B (zh) * | 2005-03-31 | 2011-02-16 | 亚都玛科技株式会社 | 水系涂料组合物及热屏蔽涂料 |
DE102005018351B4 (de) * | 2005-04-20 | 2008-05-29 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verwendung widerstandsfähiger, langlebiger Komposite im Dentalbereich |
KR20080033280A (ko) * | 2005-07-18 | 2008-04-16 | 신젠타 파티서페이션즈 아게 | 살미생물제로서의 피라졸-4-카복스아미드 유도체 |
DE102005050094A1 (de) * | 2005-10-18 | 2007-04-19 | Identif Gmbh | Farbiges Effektpigment mit Schicht aus diskreten Metallteilchen, Verfahren zu dessen Herstellung und dessen Verwendung |
CA2668410C (en) * | 2006-11-02 | 2017-05-16 | Mitchell A. Winnik | Particles containing detectable elemental code |
DE102008023444A1 (de) | 2008-05-14 | 2009-11-19 | Basf Coatings Ag | Elektrotauchlackzusammensetzung |
DE102011054440A1 (de) | 2011-10-12 | 2013-04-18 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Kieselsäurepolykondensate mit cyclischen olefinhaltigen Strukturen, Verfahren zu deren Herstellung sowie deren Verwendung |
DE102012202005A1 (de) | 2011-10-12 | 2013-04-18 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Gefüllte und ungefüllte, organisch modifizierte, gegebenenfalls organisch vernetzte Kieselsäure(hetero)polysilikate als Dentalmaterialien für die "Chairside"-Behandlung |
DE102012104139A1 (de) | 2012-05-11 | 2013-11-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verwendung eines ungefüllten oder mit Füllstoff gefüllten, organisch modifizierten Kieselsäure(hetero)polykondensats in medizinischen und nichtmedizinischen Verfahren zum Verändern der Oberfläche eines Körpers aus einem bereits ausgehärteten, ungefüllten oder mit Füllstoff gefüllten Kieselsäure(hetero)polykondensat, insbesondere für die zahnmedizinische "Chairside"-Behandlung |
DE102013108594A1 (de) | 2013-08-08 | 2015-02-12 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Silane und Kieselsäure(hetero)polykondensate mit über Kupplungsgruppen angebundenen Aromaten, die sich als oder für Matrixsysteme mit hoher Transluzenz und guter Mechanik eignen |
DE102015114397A1 (de) | 2015-08-28 | 2017-03-02 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Misch- und Formverfahren für gefüllte Duromere aus organisch vernetzbaren Kompositmassen, insbesondere für dentale Zwecke |
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-
2001
- 2001-08-21 US US10/362,299 patent/US20040023040A1/en not_active Abandoned
- 2001-08-21 EP EP01976121A patent/EP1311626A2/de not_active Withdrawn
- 2001-08-21 AU AU2001295493A patent/AU2001295493A1/en not_active Abandoned
- 2001-08-21 WO PCT/EP2001/009608 patent/WO2002016508A2/de not_active Application Discontinuation
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EP0391447B1 (de) | 1989-04-07 | 1994-11-30 | Nippon Shokubai Kagaku Kogyo Co. Ltd. | Verfahren zur Herstellung von anorganischen Oxydteilchen |
DE4219287A1 (de) | 1992-06-12 | 1993-12-16 | Merck Patent Gmbh | Anorganische Füllstoffe und organische Matrixmaterialien mit Brechungsindex-Anpassung |
DE19643781A1 (de) | 1996-10-29 | 1998-04-30 | Fraunhofer Ges Forschung | Sphärische Partikel auf der Basis von Metalloxiden, Verfahren zu deren Herstellung und deren Verwendung |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004065495A3 (en) * | 2003-01-24 | 2006-01-19 | Showa Denko Kk | Surface modification method for inorganic oxide powder, powder produced by the method and use of the powder |
RU2599668C2 (ru) * | 2012-02-09 | 2016-10-10 | Омиа Интернэшнл Аг | Композиция и способ для регулирования смачиваемости поверхностей |
CN114634801A (zh) * | 2022-03-10 | 2022-06-17 | 中国石油大学(华东) | 一种油基钻井液用两亲纳米二氧化硅固体乳化剂及其制备方法与应用 |
Also Published As
Publication number | Publication date |
---|---|
US20040023040A1 (en) | 2004-02-05 |
WO2002016508A3 (de) | 2002-05-23 |
DE10041038A1 (de) | 2002-03-14 |
EP1311626A2 (de) | 2003-05-21 |
DE10041038B4 (de) | 2005-05-04 |
AU2001295493A1 (en) | 2002-03-04 |
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