AU2264600A - Solicon-aluminium mixed oxide - Google Patents

Solicon-aluminium mixed oxide Download PDF

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Publication number
AU2264600A
AU2264600A AU22646/00A AU2264600A AU2264600A AU 2264600 A AU2264600 A AU 2264600A AU 22646/00 A AU22646/00 A AU 22646/00A AU 2264600 A AU2264600 A AU 2264600A AU 2264600 A AU2264600 A AU 2264600A
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AU
Australia
Prior art keywords
silicon
mixed oxide
industry
produced
flame hydrolysis
Prior art date
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Abandoned
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AU22646/00A
Inventor
Klaus Deller
Rainer Golchert
Dieter Kerner
Helmut Mangold
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Evonik Operations GmbH
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Degussa GmbH
Degussa Huels AG
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Publication date
Application filed by Degussa GmbH, Degussa Huels AG filed Critical Degussa GmbH
Publication of AU2264600A publication Critical patent/AU2264600A/en
Abandoned legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/26Aluminium-containing silicates, i.e. silico-aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C01F7/302Hydrolysis or oxidation of gaseous aluminium compounds in the gaseous phase
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/02Amorphous compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/60Compounds characterised by their crystallite size
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/50Agglomerated particles
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/11Powder tap density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Physics & Mathematics (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Silicon Compounds (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Filtering Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Catalysts (AREA)

Abstract

A mixed silicon-aluminum oxide powder, produced by flame hydrolysis and having an amorphous structure with primary particles containing nano-crystallites, is new. A mixed silicon-aluminum oxide powder, having the composition 1-99.999 wt.% Al2O3 and balance SiO2 and produced by flame hydrolysis, has an amorphous structure (as shown by x-ray diffraction), consists of co-grown primary particles containing crystallites of 1-200 nm size and has a specific surface of 5-300 m<2>/g. An Independent claim is also included for production of the mixed oxide by evaporating silicon and aluminum halides in a specific ratio, uniformly mixing with a carrier gas of air, oxygen and hydrogen, combusting the mixture in a burner and, after separating solids from the gas phase, removing any halide residues adhering to the product by treating with moist air at elevated temperatu

Description

S&F Ref: 499340
AUSTRALIA
PATENTS ACT 1990 COMPLETE SPECIFICATION FOR A STANDARD PATENT
ORIGINAL
a. a a Name and Address of Applicant: Actual Inventor(s): Address for Service: Degussa-Huls Aktiengesellschaft D-60287 Frankfurt am Main Germany Klaus Deller, Rainer Golchert, Dieter Kerner, Helmut Mangold Spruson Ferguson St Martins Tower 31 Market Street Sydney NSW 2000 Silicon-aluminium Mixed Oxide description of this invention, including the best method of Invention Title: The following statement is a full performing it known to me/us:- 5845c >l 990033 FH 1 Silicon-aluminium mixed oxide This invention relates to a silicon-aluminium mixed oxide, a process for the production thereof as well as the use as a polishing agent in dispersions which are used, for example, for polishing electronic components, in particular for CMP applications.
The patent specification EP-0 585 544 discloses pulverulent silicon-aluminium mixed oxides produced by flame hydrolysis which are of amorphous structure and have a composition of 1 0 from 65 to 72.1 wt.% A1 2 0 3 and from 27.9 to 35 wt.% SiO 2 and a BET surface area of between 20 and 200 m 2 /g.
The invention provides a silicon-aluminium mixed oxide powder produced by flame hydrolysis and having a composition of from 1 to 99.999 wt.% A1 2 0 3 preferably 15 to 80 wt.% A1 2 0 3 the remainder being SiO 2 wherein the powder exhibits an amorphous structure in the X-ray diffraction pattern and consists of intergrown primary particles, and in these primary particles crystallites are present, and these crystallites have sizes of between one and 200 nanometres and the specific surface of the powder is between 5 and 300 m 2 preferably between 50 and 150 m 2 /g.
The invention also provides a process for the production of the silicon-aluminium oxide powder produced by flame hydrolysis according to the invention, wherein silicon halide and aluminium halide are vaporised in a particular ratio to one another and are homogeneously mixed with air, oxygen and hydrogen in a mixing unit by means of a carrier gas, this mixture undergoes combustion in a burner of known construction and, after the separation of the solids from the vapour phase, any traces of halide possibly adhering to the product are separated off in a further processing step by means of moist air at elevated temperature.
990033 FH 2 It has now been found that silicon-aluminium mixed oxides according to the invention which are made into a dispersion exhibit outstanding properties as polishing agents.
These dispersions can be used in particular for polishing in the electronics industry (CMP).
The silicon-aluminium mixed oxide according to the invention can also be used as filler, as supporting material, as a catalytically active substance, as ceramic raw material, in the electronics industry, as filler for polymers, as starting material for the production of glass or glass coatings or glass fibres, as auxiliary separating agents, in the cosmetics industry, as absorbent material, as an additive in the silicone and rubber industry, for adjusting the rheology of liquid systems, for heat- 15 protective stabilisation, as heat-insulating material, as flow-control agents, in the dental industry, as auxiliary agents in the pharmaceutical industry, in the paint industry, in PET-film applications, in fluorescent tubes, as starting material for the production of filter ceramics 20 or filters, in powders for toners, as rust inhibitors, as agents for the film-coating of polyethylene (PET) and polyvinyl acetate, in inks and in battery separators.
Examples Corresponding to the known burner arrangement described in Example 1 of EP-0 585 544, the following quantities are specified for the production of the mixed oxide.
Example 1: 1.6 Nm 3 /h hydrogen from the burner or from the reaction together with 5 Nm3/h air and 1.70 kg/h of previously vaporised SiCl, are mixed together. Into this mixture, which is at a temperature of about 200 is fed in addition 2.5 kg/h gaseous AlCl 3 (which has previously been vaporised at about 300 0 This mixture undergoes 990033 FH 3 combustion in a flame tube, while in addition 12 Nm 3 /h air is fed into this flame tube.
After the material has passed through the flame tube, the resulting powder is separated, in a filter or cyclone, from the gases containing hydrochloric acid, and adhering traces of hydrochloric acid are separated from the resulting mixed oxide by treatment at elevated temperature.
The analytical data for the mixed oxide is as follows: Specific BET surface area 56 m2/g, pH of a 4 per cent 10 dispersion 4.52, bulk density 49 g/l, tamped density 59 g/l. Composition of the powder: 63.6 wt.% A1 2 36.3 wt.% SiO 2 Example 2: 1.2 Nm3/h hydrogen from the burner or from the reaction together with 6 Nm3/h air and 1.70 kg/h of previously vaporised SiC14 are mixed together. Into this mixture, which is at a temperature of about 200 is fed in addition 2.5 kg/h gaseous AlCl 3 (which has previously been vaporised at about 300 0 This mixture undergoes 20 combustion in a flame tube, while in addition 12 Nm 3 /h air is fed into this flame tube.
After the material has passed through the flame tube, the resulting powder is separated, in a filter or cyclone, from the gases containing hydrochloric acid, and adhering traces of hydrochloric acid are separated from the resulting mixed oxide by treatment at elevated temperature.
The analytical data for the mixed oxide is as follows: Specific BET surface area 99 m 2 pH of a 4 per cent dispersion 3.9, bulk density 39 g/l, tamped density 48 g/.
Composition of the powder: 64.3 wt.% A1 2 0 3 35.52 wt.% SiO,.
Additional characterisation of the powders: 990033 FH 4 The powders have the following special feature: The X-ray diffraction patterns of these powders (Figure 1 of Example 1) show that there are virtually no crystalline phases in the powder.
But at the same time a high-resolution electron micrograph shows that the primary particles of the powders contain partially crystalline regions, which are probably responsible for the good polishing performance of the dispersions prepared from these mixed oxides (Figure 2).
*e e e* eo e

Claims (6)

1.A silicon-aluminium mixed oxide powder produced by flame hydrolysis and having a composition of from 1 to 99.999 wt.% A1 2 0 3 the remainder being SiO 2 wherein the powder exhibits an amorphous structure in the X-ray diffraction pattern and consists of intergrown primary particles, and in these primary particles crystallites are present, and these crystallites have sizes of between one and 200 nanometres and the specific surface of the powder is between 5 and 300 m 2 /g.
2.A process for the production of the silicon-aluminium mixed oxide produced by flame hydrolysis as claimed in claim 1, wherein silicon halide and aluminium halide are vaporised in a particular ratio to one another and are 15 homogeneously mixed with air, oxygen and hydrogen in a mixing unit by means of a carrier gas, this mixture g undergoes combustion in a burner of known construction and, after the separation of the solids from the vapour phase, any traces of halide possibly adhering to the 20 product are separated off in a further processing step by means of moist air at elevated temperature.
3.The use of the silicon-aluminium mixed oxide produced by flame hydrolysis as claimed in claim 1 for the production of dispersions which are used for polishing, in particular in the electronics industry (CMP).
4.The use of the silicon-aluminium mixed oxide produced by flame hydrolysis as claimed in claim 1 as filler, as supporting material, as a catalytically active substance, as ceramic raw material, in the electronics industry, as filler for polymers, as starting material for the production of glass or glass coatings or glass fibres, as auxiliary separating agents, in the cosmetics industry, as absorbent material, as an additive in the silicone and rubber industry, for adjusting the rheology of liquid systems, for heat-protective stabilisation, as 6 heat-insulating material, as flow-control agents, in the dental industry, as auxiliary agents in the pharmaceutical industry, in the paint industry, in PET-film applications, in fluoroescent tubes, as starting material for the production of filter ceramics or filters, in powders for toners, as rust inhibitors, as agents for the film-coating of polyethylene (PET) and polyvinyl acetate, in inks and in battery separators.
A silicon-aluminium mixed oxide powder, substantially as hereinbefore described with reference to any one of the examples.
6. Silicon-aluminium mixed oxide, produced by the process according to claim 2. Dated 27 March, 2000 1 0 Degussa-Huls Aktiengesellshaft Patent Attorneys for the Applicant/Nominated Person SPRUSON FERGUSON e* *o •o* o* o* IR:\LIBUUjO2O82.doc. NCN
AU22646/00A 1999-04-30 2000-03-29 Solicon-aluminium mixed oxide Abandoned AU2264600A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19919635A DE19919635A1 (en) 1999-04-30 1999-04-30 Silicon-aluminum mixed oxide
DE199196354 1999-04-30

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EP (1) EP1048617B1 (en)
JP (2) JP2001010811A (en)
KR (1) KR100669833B1 (en)
CN (1) CN1272455A (en)
AT (1) ATE312056T1 (en)
AU (1) AU2264600A (en)
BR (1) BR0002102A (en)
CA (1) CA2307057A1 (en)
DE (2) DE19919635A1 (en)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10049971A1 (en) * 2000-10-06 2002-04-11 Wieland Edelmetalle Ceramic dental articles such as crowns are made by electrophoretic deposition of a particle dispersion onto a shaped electrode and are strengthened by inclusion of ceramic fibers and/or nanocrystalline particles
EP1234800A1 (en) 2001-02-22 2002-08-28 Degussa Aktiengesellschaft Aqueous dispersion, process for its production and use thereof
DE10135452A1 (en) 2001-07-20 2003-02-06 Degussa Pyrogenically produced aluminum-silicon mixed oxides
DE50104223D1 (en) 2001-08-08 2004-11-25 Degussa Metal oxide particles coated with silicon dioxide
DE10149130A1 (en) * 2001-10-05 2003-04-10 Degussa Flame hydrolytic alumina doped with divalent metal oxide is used in aqueous dispersion for chemical-mechanical polishing of metallic and nonmetallic surfaces, coating paper or producing special glass
DE10205280C1 (en) * 2002-02-07 2003-07-03 Degussa Aqueous dispersion used for chemical-mechanical polishing of oxide surface, preferably silica, contains pyrogenic silica powder doped with alumina from aerosol with specified particle size
US20030162398A1 (en) 2002-02-11 2003-08-28 Small Robert J. Catalytic composition for chemical-mechanical polishing, method of using same, and substrate treated with same
DE10360087A1 (en) * 2003-12-20 2005-07-21 Degussa Ag Flame hydrolysis produced, hochoberflächiges alumina powder
EP1805255A1 (en) 2004-10-25 2007-07-11 Ciba Specialty Chemicals Holding Inc. Functionalized nanoparticles
CN100369803C (en) * 2005-05-31 2008-02-20 昆明理工大学 Method and apparatus for preparing fumed nano oxide
JP5345787B2 (en) * 2008-02-04 2013-11-20 電気化学工業株式会社 Method for producing silica-alumina composite oxide ultrafine powder for semiconductor encapsulant
JP5553749B2 (en) * 2008-05-16 2014-07-16 電気化学工業株式会社 Amorphous siliceous powder, production method and use thereof
DE102010002356A1 (en) 2010-02-25 2011-08-25 Evonik Degussa GmbH, 45128 Compositions of metal oxides functionalized with oligomeric siloxanols and their use
CN112028097B (en) * 2020-08-19 2023-10-17 南通江山农药化工股份有限公司 Method for preparing nano alumina-silicon dioxide composite powder and product thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2931585A1 (en) * 1979-08-03 1981-02-12 Degussa TEMPERATURE-STABILIZED, PYROGEN-PRODUCED ALUMINUM OXIDE MIXED OXIDE, THE METHOD FOR THE PRODUCTION AND USE THEREOF
JPH01119559A (en) * 1987-11-02 1989-05-11 Kureha Chem Ind Co Ltd Mullite-alumina composite sintered compact and its production
AU650382B2 (en) * 1992-02-05 1994-06-16 Norton Company Nano-sized alpha alumina particles
DE4214724C2 (en) * 1992-05-04 1995-05-18 Starck H C Gmbh Co Kg Fine-particle oxide ceramic powder
DE4228711A1 (en) * 1992-08-28 1994-03-03 Degussa Silicon-aluminum mixed oxide

Also Published As

Publication number Publication date
EP1048617B1 (en) 2005-12-07
JP2001010811A (en) 2001-01-16
DE50011789D1 (en) 2006-01-12
KR20010049302A (en) 2001-06-15
CA2307057A1 (en) 2000-10-30
BR0002102A (en) 2000-10-31
EP1048617A1 (en) 2000-11-02
CN1272455A (en) 2000-11-08
JP2009196891A (en) 2009-09-03
KR100669833B1 (en) 2007-01-18
ATE312056T1 (en) 2005-12-15
DE19919635A1 (en) 2000-11-23

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