EP1044178A1 - Ceramiques non oxydables enduites superficiellement - Google Patents

Ceramiques non oxydables enduites superficiellement

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Publication number
EP1044178A1
EP1044178A1 EP98966404A EP98966404A EP1044178A1 EP 1044178 A1 EP1044178 A1 EP 1044178A1 EP 98966404 A EP98966404 A EP 98966404A EP 98966404 A EP98966404 A EP 98966404A EP 1044178 A1 EP1044178 A1 EP 1044178A1
Authority
EP
European Patent Office
Prior art keywords
ceramic
oxide
ceramics
group
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP98966404A
Other languages
German (de)
English (en)
Inventor
Juan Gonzalez-Blanco
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HC Starck GmbH
Original Assignee
HC Starck GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HC Starck GmbH filed Critical HC Starck GmbH
Publication of EP1044178A1 publication Critical patent/EP1044178A1/fr
Withdrawn legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • 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
    • C04B35/10—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 aluminium oxide
    • C04B35/111—Fine ceramics
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
    • C04B35/58014—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
    • C04B35/58028—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on zirconium or hafnium nitrides
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/636—Polysaccharides or derivatives thereof
    • C04B35/6365—Cellulose or derivatives thereof
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3886—Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
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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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
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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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/549—Particle size related information the particle size being expressed by crystallite size or primary particle size

Definitions

  • the invention relates to non-oxide ceramics, the surface of which is coated with at least one ⁇ -amino acid, a process for their production and their use for the production of ceramic sintered bodies and layers.
  • Preferred non-oxide ceramics are TiN, ZrN, TiC or SiC, in particular TiN or TiC.
  • Aromatic ⁇ -amino acids such as tyrosine, in particular L-tyrosine and heterocyclic ⁇ -amino acids are also advantageous.
  • the average primary particle size of the non-oxide ceramic used in the method according to the invention can be determined with the aid of electron microscopic images. It is preferably 0.1 to 50 nm, in particular 0.5 to 30 nm.
  • the primary particles of the non-oxide ceramics preferably have a spherical structure. They can also be in the form of their agglomerates or aggregates, these having an average particle size of less than 500 nm, preferably less than 150 nm.
  • the non-oxide ceramics used can have extremely low oxygen contents of less than 10% by weight, based on the solid, preferably ⁇ 1%, particularly preferably ⁇ 0.1%.
  • non-oxide ceramics are used particularly preferably in the inventive process which have a content of NH 4 -O ⁇ ® groups from 50 to 1000, preferably from 50 to 500, in particular 100 to 500 .mu.eq / g of non-oxide ceramics.
  • the -O ⁇ NH4® groups can be produced, for example, by reacting -OH groups on the ceramic surface with aqueous ammonia.
  • the - OH groups in turn can be obtained, for example, by oxidation or passivation with oxygen-containing gases of the ceramic particles produced by the CVR process. This creates a monomolecular oxide layer on the
  • the invention therefore further relates to a process for the production of -O ⁇ NH ®- group-containing ceramics, which is characterized in that at least one non-oxide ceramic from BN and from the group of carbides, nitrides, borides and silicides of the elements Ti, Zr, Hf , Cr, Mo, W, V, Nb, Ta, Si, Ge and Sn with an average primary particle size of 0.1 to 50 nm, with an aqueous NH 3 solution at a temperature of 20 to 150 ° C, optionally under pressure , treated.
  • the ceramics used for this treatment are preferably after
  • the NH 3 treatment is preferably carried out in a 5-50% by weight aqueous NH 3 solution. It is particularly preferably carried out at a temperature of 40-120 ° C.
  • the treated ceramic is filtered off, optionally washed with water and then dried.
  • Water can be removed.
  • this is possible with the following equipment: fluidized bed dryer, paddle dryer, spray dryer, drying cabinet and vacuum dryer.
  • Normal pressure It is particularly preferred to work under reflux. At higher temperatures, the process can also be carried out with the application of an external pressure, in particular 2 to 10 bar.
  • the process according to the invention is particularly preferred in water or aqueous
  • the ceramic to be used can also be wet-ground together with at least part of the ⁇ -amino acid, for example on a 2-roller grinding device.
  • the ceramic to be used is in powder form or in the form of the water-moist press cake together with a portion of the ⁇ -amino acid and water, preferably deionized water, to form a homogeneous grinding suspension, for example by means of an agitator bucket, dissolver and similar units, if appropriate after a pre-comminution and homogenized).
  • the grinding suspension can also contain fractions of low-boiling solvents (boiling point ⁇ 150 ° C.), which can be removed by evaporation in the course of a subsequent fine grinding. However, it can also contain proportions of higher-boiling solvents or other additives, for example grinding aids, defoamers or wetting agents.
  • the wet comminution of the ceramics to be used includes both the pre-comminution and the fine grinding.
  • the suspension concentration is preferably above the desired concentration of the finished preparation.
  • the desired final solids concentration is preferably set after the wet comminution.
  • grinding is carried out to the desired particle size distribution. Units such as e.g. Kneaders, roller mills, kneading screws, ball mills, rotor-stator mills, dissolvers, corundum disc mills, vibrating mills and in particular high-speed, continuously or discontinuously charged agitator ball mills with grinding media with a diameter of 0.1 to 2 mm in question.
  • the grinding media can be made of glass, ceramic or metal, e.g. Be steel.
  • the grinding temperature is preferably in the range from 20 to 150 ° C., but generally at room temperature, if appropriate below the cloud point of the optionally additionally used surface-active compounds as dispersing agents (grinding aids).
  • the ⁇ -amino acid is preferably used in an amount of 0.1 to 20% by weight, based on the amount of ceramic used.
  • Amount from 1 to 10% by weight.
  • Any excess ⁇ -amino acid can, for example, be separated from the surface-coated ceramic by filtration using the process according to the invention. Excess ⁇ -amino acid can also be separated off, for example, by centrifuging the suspension and then decanting off the supernatant. Membrane or micro filtration processes are also suitable.
  • the ceramic according to the invention is preferably used in the form of its aqueous or solvent-containing suspension, for example for the production of ceramic composite materials from non-oxidic and / or oxidic components.
  • the suspensions can also be used to manufacture metallic composite materials.
  • the invention therefore furthermore relates to suspensions containing the surface-coated ceramic and water and / or an organic solvent according to the invention.
  • the suspensions according to the invention preferably contain 5 to 50% by weight, in particular 10 to 35% by weight, based on the suspension, of the ⁇ -
  • aqueous suspensions according to the invention can also be used to produce layers, for example by dipping or knife coating.
  • the layers produced in this way can, for example, protect the wear of metals, ceramics,
  • the solvent-containing suspensions are preferably used for pigmenting plastics.
  • the suspensions containing organic solvents are preferably prepared by adding the organic solvent to the aqueous suspensions and removing the water by suitable methods, for example by distillation.
  • the invention further relates to a process for the production of ceramic sintered bodies, which is characterized in that the suspensions according to the invention, if appropriate together with other ceramic powders or suspensions, are processed before or after removal of the dispersing medium from water and / or solvent to give green bodies or layers and then sinters.
  • further ceramics include, for example, those with particle sizes of up to several ⁇ m.
  • Al 2 O, TiC, SiC and Si 3 N4 are to be mentioned as ceramics. These ceramic blends are ideal for the production of ceramic sintered bodies or layers.
  • Green bodies or sintered bodies or layers can be processed in various ways.
  • extrusion masses can be produced, which can be sintered into finished moldings after extrusion.
  • 20 to 80, in particular 30 to 70 and particularly preferably 40 to 60 parts by weight of the ceramic powder according to the invention (either as such or in the form of a suspension as described above, for example) are usually used per 100 parts by weight of extrusion compositions.
  • sion, 10 to 70, in particular 20 to 60 and particularly preferably 30 to 50 parts by weight of dispersing medium and 0.5 to 20, in particular 2 to 15, particularly preferably 5 to 10 parts by weight of additives which consist of binders, plasticizers and Mixtures of these are used.
  • the binders and plasticizers mentioned are preferably made from modified celluloses (e.g. methyl cellulose, ethyl cellulose, propyl cellulose and carboxy-modified cellulose), polyalkylene glycols (in particular polyethylene glycol and polypropylene glycol, preferably with an average molecular weight of 400 to 50,000), dialkyl phthalates (e.g. dimethyl phthalate,
  • binders and plasticizers are required in order to ensure an extrudable mass and sufficient dimensional stability after shaping.
  • part of the dispersion medium can be removed (preferably under reduced pressure) until the extrusion masses have the desired solids content.
  • Preferred solids contents of the extrusion mass are at least 30 and in particular at least 40% by volume.
  • shaping processes are electrophoresis, slip casting, slip die casting and filter pressing as well as combinations of electrophoresis and slip casting, slip die casting or filter presses; furthermore injection molding, fiber spinning, gel casting and centrifuging. With these shaping processes, compact shaped bodies with high green densities are obtained. It is also possible to use the suspensions for coating purposes. Suitable
  • Coating processes are, for example, dipping, spin-coating, knife coating, brushing and the Electrophoresis.
  • Metals, ceramics, hard metals, glass and cermets are suitable as substrates.
  • the ceramic sintered bodies or layers obtained are characterized by a nanoscale structure with a grain size below 100 nm, a density> 95% of theory and high hardness.
  • the ceramic sintered moldings according to the invention find e.g. Application as
  • Al 2 O 3 , TiC, SiC and Si 3 N 4 are particularly suitable as the matrix phase.
  • Microporous layers for filtration purposes e.g. Micro ultra nano filtration and reverse osmosis.
  • Round filter made of cellulose acetate / cellulose nitrate with a pore size of 0.45 ⁇ m is suctioned off with a glass frit and washed with deionized water. The filter cake was then dried in a drying cabinet at 70 ° C. for 10 hours.
  • the Cl content on the particle surface of the pretreated TiN could be reduced from 2.9 to 0.8 atom%.
  • the analysis was carried out by ESCA (Electron Spectroscopy for Chemical Analysis), using the XPS (x-ray photoelectron spectroscopy) method.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Ceramic Products (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

L'invention concerne des céramiques non oxydables formés de BN ou d'un constituant du groupe des carbures, nitrures, borures et siliciures des éléments Ti, Zr, Hf, Cr, Mo, W, V, Nb, Ta, Si, Ge et Sn de granulométrie moyenne des particules primaires de 0,1 à 50 nm, dont la surface est enduite d'au moins un aminoacide alpha .
EP98966404A 1998-01-07 1998-12-24 Ceramiques non oxydables enduites superficiellement Withdrawn EP1044178A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19800310 1998-01-07
DE19800310A DE19800310A1 (de) 1998-01-07 1998-01-07 Oberflächenbelegte, nichtoxidische Keramiken
PCT/EP1998/008442 WO1999035105A1 (fr) 1998-01-07 1998-12-24 Ceramiques non oxydables enduites superficiellement

Publications (1)

Publication Number Publication Date
EP1044178A1 true EP1044178A1 (fr) 2000-10-18

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Application Number Title Priority Date Filing Date
EP98966404A Withdrawn EP1044178A1 (fr) 1998-01-07 1998-12-24 Ceramiques non oxydables enduites superficiellement

Country Status (6)

Country Link
EP (1) EP1044178A1 (fr)
JP (1) JP2002500157A (fr)
KR (1) KR20010033904A (fr)
DE (1) DE19800310A1 (fr)
TW (1) TW562787B (fr)
WO (1) WO1999035105A1 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19939686A1 (de) * 1999-08-20 2001-02-22 Dechema Verfahren zur Herstellung korrosionsschützender Überzüge auf metallischen Werkstoffen auf der Basis nanoteiliger Pulver
GB0112000D0 (en) * 2001-05-16 2001-07-11 Oxonica Ltd Comminution of coated metal oxides and hydroxides
GB2383534A (en) * 2001-12-28 2003-07-02 Psimei Pharmaceuticals Plc Delivery of neutron capture elements for neutron capture therapy
EP1745161A1 (fr) * 2004-01-22 2007-01-24 The University of Manchester Revetement de ceramique
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KR20010033904A (ko) 2001-04-25
DE19800310A1 (de) 1999-07-08

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