WO2000020519A2 - Preparations contenant des oxydes inorganiques a fines particules - Google Patents

Preparations contenant des oxydes inorganiques a fines particules Download PDF

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Publication number
WO2000020519A2
WO2000020519A2 PCT/EP1999/007116 EP9907116W WO0020519A2 WO 2000020519 A2 WO2000020519 A2 WO 2000020519A2 EP 9907116 W EP9907116 W EP 9907116W WO 0020519 A2 WO0020519 A2 WO 0020519A2
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WO
WIPO (PCT)
Prior art keywords
preparations
oxide
preparation
preparations according
printing inks
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PCT/EP1999/007116
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German (de)
English (en)
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WO2000020519A3 (fr
Inventor
Juan GONZÁLEZ-BLANCO
Werner Hoheisel
Jens Sicking
Original Assignee
Bayer Aktiengesellschaft
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Filing date
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Application filed by Bayer Aktiengesellschaft filed Critical Bayer Aktiengesellschaft
Priority to KR1020017004458A priority Critical patent/KR20010080059A/ko
Priority to AU61962/99A priority patent/AU6196299A/en
Priority to EP99948855A priority patent/EP1144523A2/fr
Priority to JP2000574623A priority patent/JP2002526630A/ja
Publication of WO2000020519A2 publication Critical patent/WO2000020519A2/fr
Publication of WO2000020519A3 publication Critical patent/WO2000020519A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
    • C09D17/007—Metal oxide
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/017—Mixtures of compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/16—Amines or polyamines
    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
    • H01L21/4814—Conductive parts
    • H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
    • H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
    • H01L23/49883—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials the conductive materials containing organic materials or pastes, e.g. for thick films
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1343—Electrodes
    • G02F1/13439—Electrodes characterised by their electrical, optical, physical properties; materials therefor; method of making
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the invention relates to finely particulate inorganic oxide-containing preparations, a process for their preparation, their use for the production of printing inks and the use of the printing inks for the production of transparent, electrically conductive, structured surfaces on transparent carrier materials.
  • the object of the present invention is to produce preparations which are transparent, structured surfaces, e.g. can be applied to substrates in the form of conductor tracks with little outlay in terms of process technology.
  • the object of the present invention is to produce the electrical conductivity within these structured surfaces by sintering in a reducing atmosphere.
  • electrically conductive structured surfaces can be converted.
  • electrically conductive structured surface structures for example conductor tracks
  • the invention relates to preparations containing a) at least one oxide with an average primary particle size of 1 to 100 nm, b) at least one dispersant with an average molecular weight of M w greater than 1000 g / mol and c) at least one solvent.
  • A means Sn, In or Zn and
  • B is Sb, Sn, F, P, Al or Cd and X is O, S. Se or Te, preferably O and
  • A forms the host lattice and B represents the dopings in the host lattice, i.e. part of A is substituted by B, the
  • tungsten and molybdenum bronzes the composition Z WO 3 , or Z x MoO 3 with 0 ⁇ x ⁇ 1 and Z being an element of the first and / or second main group of
  • Periodic table of the elements is iii) tungsten and molybdenum oxides, the composition WO 3 . x , or MoO 3 . x with x ⁇ 0.1,
  • At least one dispersant with an average molecular weight M w of greater than 1,000 g / mol, preferably greater than 1,000 to 500,000 g / mol and c) at least one solvent.
  • the oxides a) contained in the preparations according to the invention can be present either in the form of their primary particles, agglomerates or aggregates of primary particles or mixtures of the two.
  • Agglomerates or aggregates are understood to mean particles in which several primary particles interact with one another via van der Waals forces, or in which the primary particles are connected to one another by surface reaction or "sintering" during the production process.
  • the average primary particle size of the oxides is usually 1 to 100 nm, preferably 1 to 50 nm. It can be determined with the aid of electron micrographs.
  • the primary particles of the oxides preferably have a spherical structure.
  • the oxides a) contained in the preparations according to the invention are in the form of their agglomerates or aggregates, the average particle size of these agglomerates or aggregates is less than 500 nm, preferably less than 150 nm.
  • the oxides a) contained in the preparations according to the invention can be crystalline or amorphous, preferably crystalline.
  • the oxides a) can, for example, by the sol-gel method, chemical vapor reaction method (CVR), chemical vapor condensation method or by
  • Plasma desorption can be produced.
  • the oxides a) contained in the preparations according to the invention are preferably present in an amount of from 0.05 to 80% by weight, in particular from 0J to 30% by weight, particularly preferably from 0.5 to 20% by weight, based on the
  • Molecules with a molecular weight of greater than 1,000 to 500,000 g / mol, preferably greater than 1,000 to 100,000 g / mol and in particular larger, are used as dispersants
  • the dispersants can be nonionic, anionic, cationic or amphoteric compounds.
  • Polymeric dispersants are particularly preferred.
  • polymeric dispersants are, for example, the compounds mentioned in the directory “Water-Soluble Synthetic Polymers: Properties and Behavior” (Volume I + II, Philip Molyneux, CRC Press, Florida 1983/84).
  • Other polymeric dispersants are, for example, water-soluble and water-emulsifiable compounds, for example homopolymers and copolymers, graft and graft copolymers and statistical block copolymers.
  • Particularly preferred polymeric dispersants are, for example, AB, BAB and
  • the A segment is a hydrophobic homopolymer or copolymer which, when used in the preparations according to the invention, ensures a connection to the oxide.
  • the B block is a hydrophilic homopolymer or copolymer or a salt thereof which, when used in the preparations according to the invention, ensures the dispersion of the oxide in the solvent in the preparation according to the invention.
  • Such polymeric dispersants and their synthesis are known for example from EP-A-518 225 and EP-A-556 649.
  • Suitable polymeric dispersants are:
  • Polyethylene oxides Polypropylene oxides, polyoxymethylenes, polytrimethylene oxides, polyvinyl methyl ethers, polyethyleneimines, polyacrylic acids, polyarylamides, polymethacrylic acids, polymethacrylamides, poly-N, N-dimethylacrylamides, poly-N-isopropylacrylamides, poly-N-acrylglycinamides, poly-N-methacrylacrylglycinamides, poly Copolymers of polyvinyl alcohol and
  • Suitable natural polymeric dispersants are: cellulose, starch, gelatin or their derivatives.
  • nonionic dispersants examples include alkoxylates, alkylolamides, esters, amine oxides, silanes such as 3-glycidyloxypropyltrimethoxysilane and alkylpolyglycosides.
  • Other suitable nonionic dispersants are: reaction products of alkylene oxides with alkoxylatable compounds, such as, for example, fatty alcohols, fatty amines, fatty acids, phenols, alkylphenols, arylalkylphenols, such as styrene-phenol condensates, carboxamides and resin acids. These reaction products are preferably ethylene oxide
  • alkylphenols with 4 to 12 carbon atoms in the alkyl radical or 3) saturated and / or unsaturated fatty amines with 14 to 20 carbon atoms or
  • Suitable ethylene oxide adducts are, in particular, the alkoxylable compounds mentioned under 1) to 5) with 5 to 120, preferably 5 to 60, in particular 5 to 30, ethylene oxide units per molecule.
  • Nonionic polymeric dispersants such as, for example, polyethylene oxides, polypropylene oxides, polyoxymethylenes, polytrimethylene oxides, polyvinyl methyl ether, polyethyleneimines, polyacrylic acids are particularly preferred.
  • Polyarylamides polymethacrylic acids, polymethacrylamides, poly-N, N-dimethylacrylamides, poly-N-isopropylacrylamides, poly-N-acrylglycinamides, poly-N-methacrylglycinamides, polyvinyl alcohols, polyvinyl pyrrolidone, polyvinyl oxazolidones, polyvinylmethyloxazolidones.
  • anionic dispersants are: alkyl sulfates, ether sulfates, ether carboxylates, phosphate esters, sulfosuccinates, sulfosuccinatamides, paraffin sulfonates, olefin sulfonates, sarcosinates, isothionates, taurates and lignin compounds.
  • Anionic, polymeric dispersants are particularly preferred.
  • Preferred anionic polymeric dispersants are condensation products of aromatic sulfonic acids with formaldehyde, such as, for example, condensation products from formaldehyde and alkylnaphthalenesulfonic acids, condensation products from formaldehyde and naphthalenesulfonic acids and / or benzenesulfonic acids or condensation products from optionally substituted phenol with formaldehyde and sodium bisulfite.
  • Naphthols with alkanols, addition of alkylene oxide and at least partial conversion of the terminal hydroxy groups into sulfo groups or half esters of maleic acid, phthalic acid or succinic acid are available.
  • preferred anionic dispersants are compounds from the
  • Alkoxylated fatty acid alcohols are understood to mean in particular those with 5 to 120, preferably 5 to 60, in particular 5 to 30, ethylene oxide units per molecule of C 6 -C 22 fatty acid alcohols which are saturated or unsaturated, in particular stearyl alcohol.
  • a stearyl alcohol alkoxylated with 8 to 10 ethylene oxide units is particularly preferred.
  • the sulfated alkoxylated fatty acid alcohols are preferably present as a salt, in particular as an alkali or ammonium salt, preferably as a diethylammonium salt.
  • anionic, polymeric dispersants are the salts of polyacrylic acids, polyethylene sulfonic acids, polystyrene sulfonic acid, polymethacrylic acids, polyphosphoric acids and polyaspartic acids.
  • anionic, polymeric dispersants which are copolymers of acrylic monomers. These copolymers are exemplified by Combinations of the following monomers are available, which are synthesized to random or alternating copolymers or graft copolymers:
  • N-acrylglycinamide N-isopropylacrylamide
  • Methacrylamide methacrylic acid
  • Methacrylic acid diphenylmethyl methacrylate
  • Methacrylic acid methyl methacrylate
  • Methacrylic acid styrene
  • lignin sulfonates for example those obtained by the sulfite or kraft process (sulfite and kraft lignin sulfonates). These are preferably products which are partially hydrolyzed, oxidized, propoxylated, sulfonated, sulfomethylated or disulfonated and are fractionated by known processes, for example by the molecular weight or by the degree of sulfonation. Mixtures of sulfite and kraft lignin sulfonates are also suitable.
  • Lignin sulfonates with an average molecular weight of greater than 1,000 to 100,000 g / mol, a content of active lignin sulfonate of at least 80% and preferably with a low content of polyvalent cations are particularly suitable.
  • the degree of sulfonation can vary within wide limits.
  • Examples of cationic dispersants are: alkylammonium compounds and imidazoles.
  • Cationic, polymeric dispersants are particularly preferred.
  • cationic, polymeric dispersants are the salts of polyethyleneimines, polyvinylamines, poly (2-vinylpyridines), poly (4-vinylpyridines), poly (diallyldimethylammonium) chloride, poly (4-vinylbenzyltrimethylammonium) salts, poly (2- vinylpiperidine) and polylysine.
  • amphoteric dispersants are: betaines, glycinates, propionates and imidazolines.
  • Anionic and cationic polymers are summarized as polyelectrolytes and can be partially or completely dissociated in an aqueous and / or organic phase.
  • the dispersants used are preferably in an amount of 0J to 200% by weight, in particular 0.5 to 100% by weight, particularly preferably 1 to
  • B means Sb, Sn, F, P, AI or Cd and XO, S, Se or Te, preferably O
  • A forms the host lattice
  • Sulfosuccinic acid esters alkylbenzene sulfonates, sulfated, alkoxylated fatty acid alcohols or their salts, ether sulfates, ether carboxylates, phosphate esters, sulfosuccinatamides, paraffin sulfonates, olefin sulfonates, sarcosinates, isothionates, taurates, lignin compounds, condensation products with formaldehyde acids, from aromatic sulfonates, from aromatic sulfonates, from aromatic sulfonates Condensation products from formaldehyde and naphthalenesulfonic acids and / or benzenesulfonic acids or
  • Condensation products from optionally substituted phenol with formaldehyde and sodium bisulfite, condensation products of naphthols with alkanols, addition of alkylene oxide and at least partially Conversion of the terminal hydroxyl groups into sulfo groups or half esters of maleic acid, phthalic acid or succinic acid are available, as well as polymers of amino acid units, in particular polyaspartic acid, or
  • quaternary alkylammonium compounds and imidazoles from the group of the cationic dispersants: quaternary alkylammonium compounds and imidazoles, or
  • amphoteric dispersants glycinates, propionates and imidazolines, or
  • Alkoxylates alkylolamides, esters, amine oxides, silanes such as, for example, 3-glycidyloxypropyltrimethoxysilane, alkylpolyglycosides and reaction products of alkylene oxides with alkoxylable compounds, such as, for example, fatty alcohols, fatty amines, fatty acids, phenols, alkylphenols,
  • Arylalkylphenols such as styrene-phenol condensates, carboxamides and resin acids, preferably ethylene oxide adducts, which result from the reaction of ethylene oxide with
  • the solvents used in the inventive preparations c) are preferably water, ahphatician C, -C 4 alcohols such as methanol, ethanol, isopropanol, n-propanol, ahphatician n-butanol, isobutanol or tert-butanol,
  • Ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone or diacetone alcohol,
  • Polyols such as ethylene glycol, propylene glycol, butylene glycol, diethylene glycol, triethylene glycol, trimethylolpropane, polyethylene glycol with an average molecular weight of 100 to 4,000 g / mol, preferably 400 to 1,500 g / mol, glycerol, monohydroxy ether, preferably monohydroxyalkyl ether are particularly preferred
  • Mono-C, -C 4 -alkyl glycol ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, dipropylene glycol monoethyl ether, thiodiglycol, triethylene glycol monomethyl ether or triethylene glycol pyrrolidone-2-methylrolidone-nolonyl ether, methyl-2-pyrrolidone -pyrrolidone, 1.3-
  • Mixtures of solvents are preferably used, particularly preferably mixtures of polyethylene glycol / 2-pyrrolidone / water or polyethylene glycol / 2-pyrrolidone / ethanol.
  • the amount of the solvent used in the preparations according to the invention is preferably 10 to 99% by weight, particularly preferably 30 to 98% by weight, based on the solids content of oxide in the preparation according to the invention.
  • the preparations according to the invention may contain further cationic anionic, amophotere and / or nonionic surface-active compounds, for example those which are available in the directory "Surfactants Europe, A Directory of Surface Active Agents Europe "(Edited by Gordon L. Hollis, Royal Society of Chemistry), Cambridge (1995).
  • these surface-active compounds should preferably be non-ionic or of the same ionicity as the dispersant b).
  • the preparations according to the invention can furthermore contain additives in addition to the components a) -c) used.
  • Preferred additives are aromatic dicarboxylic acids and their esters.
  • Preferred aromatic dicarboxylic acids are phthalic acid, isophthalic acid and terephthalic acid.
  • Preferred esters are isophthalic diesters, phthalic diesters and
  • Terephthalic acid diester of the formula RCOO-C 6 H 4 -COOR ' where R, R' independently of one another are methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, phenyl or benzyl.
  • Diethyl phthalate is particularly preferred. Mixtures of the additives mentioned are also suitable.
  • Further preferred additives are compounds from the group of terpenes, terpenoids, fatty acids and fatty acid esters.
  • Preferred compounds are ocimen, myrcene, geraniol, nerol, linalool, citronellol, geranial, citronellal, neral, limonene, menthol, for example (-) - menthol, menthone or bicyclic monoterpenes, saturated and unsaturated fatty acids with 6 to 22 carbon atoms, for example Stearic acid, oleic acid, linoleic acid or linolenic acid. Mixtures of the additives mentioned also come in
  • the preparation of the preparations according to the invention comprises wet comminution and a dilution step.
  • the wet comminution optionally includes a pre-comminution, the production of a grinding suspension and the grinding.
  • the oxides a are generally in powder form or in the form of water-moist
  • Press cake together with a portion of the dispersant and polar organic solvent and / or water, preferably deionized water, are beaten to a homogeneous grinding suspension, i.e. introduced and homogenized.
  • the dispersants used adsorb to the oxides, which thereby deagglomerate or deaggregate.
  • This grinding suspension can be produced, for example, by means of a stirrer, dissolver and similar devices.
  • the grinding suspension can also contain fractions of low-boiling solvents (boiling point ⁇ 150 ° C), which are removed in the course of the subsequent fine grinding
  • Evaporation can be carried out. However, it can also contain proportions of higher-boiling solvents, surface-active compounds as mentioned above or other additives e.g. Grinding aids, defoaming agents or wetting agents.
  • the solids content of oxide a) in the grinding suspension is preferably above the desired solids content in the finished preparation.
  • the desired solids content in the finished preparation is preferably set after the wet comminution.
  • the grinding takes place to the desired particle size distribution.
  • the grinding is carried out, for example, in kneaders, roller mills, kneading screws, ball mills, rotor-stator mills, dissolvers, corundum disc mills or vibrating mills. Milling is preferably carried out in high-speed, continuously or discontinuously charged stirred ball mills
  • the grinding media can be made of glass, ceramic or metal, e.g. Be steel.
  • the grinding temperature is preferably in the range from 0 to 250 ° C., but as a rule at room temperature, particularly preferably below the cloud point of the dispersant b) used.
  • the grinding can be carried out partially or completely in a high-pressure homogenizer or in a so-called jet disperser (known from DE-A 19 536 845).
  • a so-called jet disperser known from DE-A 19 536 845.
  • the suspension obtained after grinding is mixed and homogenized in a manner known per se in solvent, preferably water, optionally with the remaining amounts of dispersant and, if appropriate, further additives, and adjusted to the desired solids content of the finished preparation.
  • solvent preferably water
  • dispersants can also be added here, for example in order to avoid reagglomeration of fine particles in the finished preparation.
  • Stabilization sufficient dispersants are provided. in the Following this or after the dilution step, dispersing agents and / or excess surface-active compounds which are not adsorbed on the oxides a) used are preferably removed and then the desired solids content in the finished preparation is adjusted.
  • One method for removing dispersants in solution is, for example, centrifuging the grinding suspension and then decanting off the supernatant.
  • Membrane or microfiltration processes can also be considered.
  • the preparations according to the invention are preferred for applying structured, conductive and transparent surfaces (for example for display applications), such as Conductor tracks are used on insulating, transparent substrates.
  • the preparations according to the invention can be applied to the substrates in the form of pastes or pourable compositions by knife coating or casting or in the form of printing inks by inkjet printing.
  • the preparations according to the invention are preferably applied to substrates in the form of printing inks by ink-jet printing.
  • the invention further relates to printing inks containing the preparations according to the invention.
  • the printing inks according to the invention can contain agents for adjusting the viscosity of the ink, such as, for example, polyvinyl alcohol, polyvinylpyrrolidone, methyl cellulose and others, agents known to the person skilled in the art, provided that they do not adversely affect the stability of the printing ink, the printing behavior and the drying behavior on a suitable surface.
  • the printing inks according to the invention can also contain preservatives, surfactants and pH regulators.
  • NaOH, ammonia, aminomethylpropanol N, N-dimethylaminoethanol are preferably used as pH regulators.
  • the printing inks according to the invention can be produced analogously to the production of the preparations according to the invention, the printing ink according to the invention being adjusted to the desired viscosity, density and
  • Surface tension is preferably carried out with the adjustment of the solids content of the printing ink according to the invention.
  • the physical ink properties are preferably adjusted for use in conventional inkjet printers, with the surface tension preferably
  • the viscosity should preferably be less than 20 mPa-s, preferably 0.5 to 10 mPa-s.
  • the printing inks according to the invention are preferably filtered before use, for example using 0.5 to 5 ⁇ m membrane or glass filters.
  • the printing inks according to the invention show excellent dispersion and
  • the invention further relates to a method for producing electrically conductive, structured, transparent surfaces (for example for display applications), such as Conductor tracks on insulating, transparent
  • Substrates such as glass or high-melting plastics by applying the printing inks according to the invention in the form of structured, transparent surfaces by ink-jet printing and then converting these structured, transparent surfaces into electrically conductive, structured transparent surfaces by sintering the printed substrates in reductive
  • Ink-jet printing or the ink-jet method is known per se.
  • the printing ink is filled into a receptacle of an ink jet printhead and sprayed onto the substrate in small droplets.
  • the ink ejection in droplets is preferably carried out via a piezoelectric crystal, a heated cannula (bubble or thermo-jet process) or mechanical pressure increase, pressure being exerted on the ink system and ink drops being thrown out in this way.
  • the droplets are shot from one or more small nozzles onto the substrate.
  • a method is also possible in which the smallest volumes, in the form of drops, are brought onto a substrate by means of electrostatic deflection from an ink jet.
  • the individual droplets on the substrate are combined into characters or graphic patterns such as structured surfaces by electronic control.
  • a reducing atmosphere e.g. Argon-hydrogen gas mixture
  • forming gas 5% hydrogen, 95% argon
  • the electrically conductive, structured, transparent surfaces produced by the method according to the invention have a specific resistance of 0.014 to 0.11 ohm * cm.
  • d 10 means that 10% of all particles are not larger than 17 nm
  • d 50 means that 50% of all particles are not larger than 43 nm
  • d 90 means that 90% of all particles are not larger than 87 nm.
  • particles are to be understood as primary particles as well as aggregates or agglomerates.
  • polyaspartic acid (molecular weight 3,000 g / mol) were dissolved in 247.5 ml of water.
  • d 10 means that 10% of all particles are not larger than 34 nm
  • d 50 means that 50% of all particles are not larger than 79 nm
  • d 90 means that 90% of all
  • particles that are not larger than 107 nm.
  • particles are to be understood as primary particles as well as aggregates or agglomerates.
  • d 0 means that 10% of all particles are not larger than 23 nm
  • d 50 means that 50% of all particles are not larger than 60 nm
  • d 90 means that 90% of all particles are not larger than 92 nm.
  • particles are to be understood as primary particles as well as aggregates or agglomerates.
  • d 10 means that 10% of all particles are not larger than 34 nm
  • d 50 means that 50% of all particles are not larger than 67 nm
  • d 90 means that 90% of all
  • Particles are not larger than 1 10 nm.
  • particles are to be understood as primary particles as well as aggregates or agglomerates.
  • Indium tin oxide particles determined by the method of dynamic light scattering (scattered light distribution). A particle diameter of 91 nm could be measured. The mass distribution was determined in the ultracentrifuge:
  • d 10 means that 10% of all particles are not larger than 31 nm
  • d 50 means that 50% of all particles are not larger than 64 nm and cL ,,, means that 90% of all particles are not larger than 117 nm .
  • particles are to be understood as primary particles as well as aggregates or agglomerates.
  • the preparations prepared in Examples 1 to 5 were used as printing inks. Structured areas and conductor tracks were printed on 1 to 2 mm thick glass plates using an ink jet printer.
  • the glass plates printed in this way were sintered for 6 hours under forming gas (5% hydrogen, 95% argon) at 400 ° C. and then in an oven sintered in air for 6 hours at 400 ° C.
  • the electrically conductive, structured surfaces produced in this way are transparent and have a specific resistance of 0.014 to OJ 1 ohm * cm.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Electromagnetism (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Conductive Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Laminated Bodies (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

L'invention concerne des préparations contenant a) au moins un oxyde de dimension particulaire primaire moyenne comprise entre 1 et 100 nm, de préférence entre 1 et 50 nm; b) au moins un agent de dispersion de poids moléculaire moyen MW supérieur à 1000g/mole et c) au moins un solvant. Ces préparations s'utilisent notamment pour produire des encres d'impression, appliquées comme surfaces structurées sur un substrat transparent à point de fusion élevé, selon le procédé d'impression par jet d'encre. Après frittage en atmosphère à action réductrice, on obtient des couches transparentes électroconductrices.
PCT/EP1999/007116 1998-10-07 1999-09-24 Preparations contenant des oxydes inorganiques a fines particules WO2000020519A2 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020017004458A KR20010080059A (ko) 1998-10-07 1999-09-24 미세 미립자 무기 옥사이드를 포함하는 제제
AU61962/99A AU6196299A (en) 1998-10-07 1999-09-24 Preparations containing fine-particulate inorganic oxides
EP99948855A EP1144523A2 (fr) 1998-10-07 1999-09-24 Preparations contenant des oxydes inorganiques a fines particules
JP2000574623A JP2002526630A (ja) 1998-10-07 1999-09-24 微粒子状無機酸化物を含有する配合物

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19846096.1 1998-10-07
DE19846096A DE19846096A1 (de) 1998-10-07 1998-10-07 Präparation von Suspensionen ternärer Oxide für Drucktinten

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WO2000020519A2 true WO2000020519A2 (fr) 2000-04-13
WO2000020519A3 WO2000020519A3 (fr) 2001-11-29

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DE (1) DE19846096A1 (fr)
WO (1) WO2000020519A2 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006016729A1 (fr) * 2004-08-13 2006-02-16 Hae-Wook Lee Composition pour revetements fonctionnels, film forme a partir de celle-ci et procede de formation de la composition et du film
WO2006112647A1 (fr) * 2005-04-21 2006-10-26 Samsung Corning Co., Ltd. Procede de preparation d'une suspension d'oxyde metallique
WO2007038950A1 (fr) 2005-09-28 2007-04-12 Stichting Dutch Polymer Institute Procede de production de structures de surfaces metalliques et dispositif correspondant
DE102019201792A1 (de) * 2019-02-12 2020-08-13 Evonik Operations Gmbh Halbleiter-Schaltungsanordnung und Verfahren zu deren Herstellung

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DE19940560C2 (de) * 1999-08-26 2001-09-13 Infineon Technologies Ag Verfahren zur Herstellung eines Halbleiterchips mit nach dem Siliziumprozess einstellbarer elektrischer Eigenschaft
US20050236603A1 (en) * 2002-05-07 2005-10-27 Faris Sadeg M Conductive ink
US7683107B2 (en) 2004-02-09 2010-03-23 E.I. Du Pont De Nemours And Company Ink jet printable thick film compositions and processes
US20050176246A1 (en) * 2004-02-09 2005-08-11 Haixin Yang Ink jet printable thick film ink compositions and processes
US20050173680A1 (en) * 2004-02-10 2005-08-11 Haixin Yang Ink jet printable thick film ink compositions and processes
DE102004020559A1 (de) 2004-04-27 2005-12-01 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Dispergierung und Passivierung von feinteiligen Pulvern in Wassern und wässrigen Medien
US20070078190A1 (en) * 2005-09-30 2007-04-05 Distefano Frank V Use of 2,3-dihydroxynaphthalene-6-sulfonic acid salts as dispersants
US20100096601A1 (en) * 2005-10-27 2010-04-22 Distefano Frank Vito Molecules with complexing groups for aqueous nanoparticle dispersions and uses thereof
DE102013100662B4 (de) 2013-01-23 2018-09-20 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Markierungszusammensetzung, deren Verwendung und diese enthaltende Gegenstände
EP2962993B1 (fr) * 2013-03-01 2019-06-12 Kyoto University Procédé de production d'une dispersion liquide de microparticules céramiques
CN103242695B (zh) * 2013-05-05 2015-07-29 浙江师范大学 一种ZnO半导体纳米材料墨水的制备方法
JP6877996B2 (ja) * 2016-12-27 2021-05-26 小林製薬株式会社 外用組成物
JP6877997B2 (ja) * 2016-12-27 2021-05-26 小林製薬株式会社 外用組成物
CN108441024B (zh) * 2018-04-24 2021-03-26 株洲科能新材料有限责任公司 一种印刷用ito薄膜油墨及其制备方法

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FR2523993A1 (fr) * 1982-03-24 1983-09-30 Cables De Lyon Geoffroy Delore Pate serigraphiable a oxydes metalliques et produit obtenu avec cette pate
DE4427931C1 (de) * 1994-08-06 1995-11-23 Goldschmidt Ag Th Pigmentkonzentrat und dessen Verwendung
WO1996003466A1 (fr) * 1994-07-27 1996-02-08 Cookson Matthey Ceramics & Materials Limited Compositions de pates ou d'encres d'imprimerie
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WO1997015382A1 (fr) * 1995-10-27 1997-05-01 E.I. Du Pont De Nemours And Company Dispersants de materiaux non organiques dans des systemes aqueux
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FR2523993A1 (fr) * 1982-03-24 1983-09-30 Cables De Lyon Geoffroy Delore Pate serigraphiable a oxydes metalliques et produit obtenu avec cette pate
WO1996003466A1 (fr) * 1994-07-27 1996-02-08 Cookson Matthey Ceramics & Materials Limited Compositions de pates ou d'encres d'imprimerie
DE4427931C1 (de) * 1994-08-06 1995-11-23 Goldschmidt Ag Th Pigmentkonzentrat und dessen Verwendung
DE4430285A1 (de) * 1994-08-26 1996-02-29 Basf Ag Hochreine ferromagnetische Eisenoxidpigmente
WO1997015382A1 (fr) * 1995-10-27 1997-05-01 E.I. Du Pont De Nemours And Company Dispersants de materiaux non organiques dans des systemes aqueux
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006016729A1 (fr) * 2004-08-13 2006-02-16 Hae-Wook Lee Composition pour revetements fonctionnels, film forme a partir de celle-ci et procede de formation de la composition et du film
WO2006112647A1 (fr) * 2005-04-21 2006-10-26 Samsung Corning Co., Ltd. Procede de preparation d'une suspension d'oxyde metallique
WO2007038950A1 (fr) 2005-09-28 2007-04-12 Stichting Dutch Polymer Institute Procede de production de structures de surfaces metalliques et dispositif correspondant
DE102019201792A1 (de) * 2019-02-12 2020-08-13 Evonik Operations Gmbh Halbleiter-Schaltungsanordnung und Verfahren zu deren Herstellung

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DE19846096A1 (de) 2000-04-13
KR20010080059A (ko) 2001-08-22
CN1411497A (zh) 2003-04-16
EP1144523A2 (fr) 2001-10-17
AU6196299A (en) 2000-04-26
WO2000020519A3 (fr) 2001-11-29
JP2002526630A (ja) 2002-08-20

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