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WO2018138210A1 - Procédé de fabrication de produits résistant aux températures élevées présentant des propriétés thermomécaniques améliorées - Google Patents

Procédé de fabrication de produits résistant aux températures élevées présentant des propriétés thermomécaniques améliorées Download PDF

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Publication number
WO2018138210A1
WO2018138210A1 PCT/EP2018/051864 EP2018051864W WO2018138210A1 WO 2018138210 A1 WO2018138210 A1 WO 2018138210A1 EP 2018051864 W EP2018051864 W EP 2018051864W WO 2018138210 A1 WO2018138210 A1 WO 2018138210A1
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WO
WIPO (PCT)
Prior art keywords
temporary
temperature
coating
materials
mixtures
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.)
Ceased
Application number
PCT/EP2018/051864
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German (de)
English (en)
Inventor
Christos Aneziris
Patrick Gehre
Andreas HERDERING
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Bergakademie Freiberg
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Bergakademie Freiberg
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Application filed by Bergakademie Freiberg filed Critical Bergakademie Freiberg
Priority to DE112018000221.7T priority Critical patent/DE112018000221B4/de
Publication of WO2018138210A1 publication Critical patent/WO2018138210A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C9/00—Moulds or cores; Moulding processes
    • B22C9/08—Features with respect to supply of molten metal, e.g. ingates, circular gates, skim gates
    • B22C9/086—Filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C9/00—Moulds or cores; Moulding processes
    • B22C9/10—Cores; Manufacture or installation of cores
    • B22C9/105—Salt cores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
    • B22D41/50—Pouring-nozzles
    • B22D41/52—Manufacturing or repairing thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
    • B22D41/50—Pouring-nozzles
    • B22D41/52—Manufacturing or repairing thereof
    • B22D41/54—Manufacturing or repairing thereof characterised by the materials used therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/001—Joining burned ceramic articles with other burned ceramic articles or other articles by heating directly with other burned ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6028—Shaping around a core which is removed later

Definitions

  • the invention relates to a process for the production of high-temperature resistant products with improved thermomechanical properties.
  • High-temperature-resistant products are used in various industries, such as in the foundry industry, in the glass industry or in energy technology.
  • High-temperature resistant products are, for example, metallurgical vessels for melting or pouring metal or glass melts, such as crucibles, spout components.
  • products such as filters for molten metal filtration or catalyst carriers in the chemical industry.
  • High temperature products are used at temperatures above 600 ° C.
  • High temperature solid products are used, for example, as spout components in metallurgy, as core shells in metal foundries, as ceramic or metalloceramic filters for molten metal filtration, as heat shields for power engineering, as inlays in slide plates, as molds in the glass industry, as complex components e.g. Catalyst carriers in the chemical industry, used as mixing components in the homogenization of metal melts or as complex components in the automotive industry.
  • High-temperature-resistant products are produced from non-metallic ceramic materials or high-melting metallic materials.
  • the high-temperature-resistant products are generally produced by customary coarse or fine-grained processes, for example powder metallurgy or ceramic production processes via casting or press molding or via the melt.
  • customary coarse or fine-grained processes for example powder metallurgy or ceramic production processes via casting or press molding or via the melt.
  • these methods can not produce complex geometries.
  • water must be added to the raw material.
  • Complex component geometries can today be produced with the help of regenerative manufacturing processes of additive manufacturing using the example of ceramic or metallic products.
  • the example of the ceramic products is u.a. the SD laser printing technology is a promising method and the example of the metallic products u.a. the electron melting of high resolution of great interest.
  • US 3 090 094 A1 discloses a method for producing an open-cell, porous ceramic body, comprising the steps of: immersing an open-celled element of a polyurethane sponge material in a suspension containing a ceramic coating material around the cell-defining walls of the element to coat; Removal of the excess suspension from the element, and firing of the element to remove the sponge material and a cured structure of a to produce porous ceramic.
  • a disadvantage of this method is that the polyurethane sponge material must be burned out, which can cause cracks in the applied ceramic coating.
  • Another disadvantage is the low achievable form fidelity of the ceramic body.
  • DE 102009006778 B4 discloses a process for producing a flame or plasma sprayed thermoshock and corrosion resistant ceramic layer based on A 03-TiO 2 -ZrO 2.
  • an insert piece for flame or plasma spraying is produced from AI2O3, fully stabilized ZrCk and TiO2 powder.
  • a lost nucleus e.g. carbon-based or paper-based is applied by flame or plasma spraying the sintered insert workpiece a layer.
  • the thermal shock resistant layers have excellent thermomechanical properties. These properties are based on lamellar microstructures with corresponding in situ generated crack networks. In the flame-sprayed layers, a primary crack pattern is formed, while a secondary crack pattern during thermal shock loading is formed in the use of the refractory product.
  • EP 0807479 A1 discloses a method for producing a light metal casting, in particular a cylinder block for internal combustion engines with a coating of a wear and / or corrosion resistant material.
  • the coating is formed prior to casting by thermal spraying of the material onto a lost core of the casting, the lost core consisting of a foamed styrene polymer.
  • DE 197 16 524 C1 discloses a method for producing a body with at least one cavity, in which a body is produced with a water-soluble core of an aluminum or magnesium alloy, which is subsequently dissolved out.
  • the water-soluble core has a porosity of at least 1% by volume.
  • Such cores are used for producing a combustion chamber wall of an engine, wherein the water-soluble aluminum alloy is introduced by flame spraying between the ribs of an inner wall to form cores, which are subsequently dissolved out.
  • the outer wall is applied to the fins and the cores by thermal spraying and the cores are subsequently dissolved out to expose the cooling channels of the combustion chamber wall.
  • DE 691 25 064 T2 discloses a method of molding a product using a mold core.
  • the mold core comprises an inert particulate material, wherein the inert particulate material is bound by a binder and the binder contains a water-soluble carbohydrate.
  • the binder comprises a silicate salt, preferably a sodium silicate.
  • the water-soluble carbohydrate is selected from saccharides and starches. Saccharides are here dextrose and molasses and starch is a corn starch.
  • the inert particulate material is selected from the group: sand, metal scrap, plastic polymers, glass, alumina, clays or mixtures thereof.
  • the mixed core material is introduced into a core container and cured by heat, preferably microwave radiation, in the core container. Such cores are used in molds in which metal or plastic materials are injected in the liquid state to form the final product.
  • DE 29 17 208 A1 discloses a casting core for producing difficult to access cavities in castings made of aluminum and a method for producing the casting core.
  • the casting core consists of a base substance and a hardened organic binder, wherein the binder is sugar or a sugar derivative.
  • the basic substance is a water-soluble salt, quartz sand, metal granules or a mixture thereof.
  • the basic substance is mixed with the binder in aqueous or organic solution, pressed into molds and baked at elevated temperature.
  • DE 103 12 782 A1 discloses water-soluble salt cores for foundry purposes, which are produced under pressure and subsequent sintering, these containing a porosity-generating additive, such as sugar. Further, the document discloses a method for producing the salt cores by mixing water-soluble salts with sugar, pressing this mixture in a mold, and sintering the pressed salt core.
  • DD 151 047 A discloses protective layers on water-soluble cores for the production of cooling cavities, in particular in liquid-pressed pistons, which are thermally resistant and able to absorb the pressures occurring during liquid-pressing.
  • the water-soluble cores are coated with a metallic or non-metallic material as a protective layer.
  • the protective layer is 0.5 to 10 mm thick.
  • the object of the invention is to provide an improved process for the production of high-temperature resistant products, which are easier to produce and have improved thermal shock resistance.
  • the object is achieved by a method for the production of high-temperature-resistant products with the steps:
  • high-temperature-resistant products with improved thermal shock resistance can be produced by the method according to the invention. Furthermore, the inventive method allows the saving of process steps and process costs and the production of high temperature resistant products with improved tolerance and dimensional accuracy.
  • high temperature resistant products such as spout components in metallurgy, core shells in metal foundries, ceramic or metalloceramic filter for molten metal filtration, heat shields for power engineering, inlays in slide plates, forms in the glass industry, complex components such.
  • Catalyst carriers in the chemical industry, mixing components in the homogenization of metal melts or complex components in the automotive industry are produced.
  • Such high-temperature resistant products have a porosity of 5 to 90 vol .-%, wherein high-temperature-resistant products with a porosity of ⁇ 45 vol .-%, also referred to as dense high temperature resistant products, for example, used as spout components in metallurgy or as a delivery.
  • High-temperature resistant products with a porosity of> 45% by volume also referred to as porous high-temperature-resistant products, For example, they are used as filters for molten metal filtration or as catalyst supports.
  • step b) applied by thermal coating coating of high temperature resistant materials subject to any shrinkage, as in conventional coarse or fine powder metallurgy or ceramic processes, so that a better dimensional accuracy of the high temperature resistant products can be achieved.
  • lamellar structure of the applied by thermal coating coating of high temperature resistant materials better thermal shock resistance than conventional coarse or fine powder metallurgy or ceramic processes.
  • a temporary molding of salt and / or sugar in the context of the invention is a molding, hereinafter also referred to as the core, which is used for the production of the high-temperature resistant product and removed after application coating of high-temperature resistant materials.
  • the temporary molded body may have a cellular or a compact structure.
  • Cellular temporary shaped bodies also referred to as porous cores, have a porosity of> 45% by volume.
  • the cellular temporary shaped bodies there are combined a solid and a gaseous phase, wherein the gaseous phase is embedded within cells or pores of the cellular shaped body in the solid phase.
  • a temporary molded body with a cellular structure open-celled also referred to as open-pored.
  • the pores or cells may be interconnected, also referred to as open-celled, or isolated from each other, also referred to as closed-cell, present in the cellular shaped body.
  • Open-cell in the sense of the invention means that the pores of the cellular shaped body are interconnected by webs and accessible from the outside.
  • Examples of open-cell cellular, temporary shaped bodies are foam structures, honeycomb structures or complex 3-dimensional structures.
  • porous high-temperature-resistant products such as, for example, filters for molten metal filtration, which have a porosity of> 45% by volume.
  • Closed-cell in the sense of the invention means that the individual pores of the cellular shaped body are separated from each other by cell walls.
  • Compact temporary shaped bodies, also referred to as dense cores, have a porosity of less than 45% by volume.
  • dense, high-temperature-resistant products such as crucibles or pouring nozzles for metallurgy, which have a porosity of ⁇ 45% by volume, are preferably produced.
  • the temporary shaped body is manufactured by means of generative manufacturing processes so that it forms the mold for the high-temperature-resistant product produced by thermal coating and subsequent removal of the temporary shaped body.
  • the coating of high-temperature-resistant materials is applied by thermal coating method to the temporary shaped body that this forms after removal of the temporary molded body in step c) the high temperature resistant product.
  • the temporary shaped body is purposefully coated in such a way that the coating gives the high-temperature-resistant product in terms of thickness, structure and dimension.
  • the coating of high temperature resistant materials in step b) is applied to the compact temporary molded body so that the coating follows the contours of the compact temporary molded body.
  • near net shape high temperature products can be produced. This eliminates subsequent steps, such as sintering and the associated shrinkage, which occurs in conventional powder metallurgy or ceramic manufacturing process.
  • the coating in step b) is applied such that the coating is present on the webs of the open-cell cellular FK.
  • Porous high-temperature-resistant products whose pore structure and size almost correspond to the pore structure of the open-cell cellular temporary shaped body can advantageously be produced by the method according to the invention since subsequent steps such as sintering and the associated shrinkage are eliminated.
  • the temporary shaped bodies consist of salt and / or sugar, salt and / or sugar being present as fine and / or coarse solid grains.
  • Sugars are, chemically speaking, water-soluble carbohydrates. They include monosaccharides such as glucose or fructose, also referred to as fructose, oligosaccharides such as maltose, lactose and sucrose, also referred to as sugar or cane sugar or beet sugar, a disaccharide of glucose and fructose.
  • Salts are chemical compounds made up of positively charged ions, also cations, and negatively charged ions, also anions. The salts may be water-soluble or water-insoluble, preferably the salts are water-soluble.
  • Coarse solid grains in the sense of the invention means that the particle sizes of the individual salt and / or sugar particles are in the range from 40 ⁇ m to 500 ⁇ m, preferably in the range from 40 ⁇ m to 200 ⁇ m.
  • Fine solid grains in the sense of the invention means that the particle sizes of the individual salt and / or sugar particles are smaller than 40 ⁇ m.
  • the porous or dense cores consist of fine and / or coarse solid grains of water-soluble carbohydrates.
  • the porous or dense cores of fine and / or coarse solid grains consist of monosaccharides or oligosaccharides or mixtures thereof.
  • the porous or dense cores consist of fine and / or coarse solid granules of glucose or fructose or maltose or lactose or sucrose or mixtures thereof.
  • the porous or dense cores consist of fine and / or coarse solid granules of water-soluble salt or common salt.
  • the porous or dense cores of fine and / or coarse solid grains consist of mixtures of water-soluble carbohydrates with water-soluble salt or common salt.
  • Generative manufacturing processes are methods for the rapid and cost-effective production of models, moldings, samples, prototypes, tools and end products.
  • the production takes place in layers, additive, of materials which are present for example as a liquid, gel, paste, powder or as a band, wire or sheet-like material, which are solidified by means of chemical and / or physical processes.
  • generative manufacturing processes it is also possible to produce complex shaped bodies which can not be produced using conventional production methods or only with considerable effort.
  • the generative manufacturing processes include, for example, 3D printing processes, melt-coating processes (also known as fused filament fabrication) or electron beam melting.
  • the temporary shaped body of salt and / or sugar is preferably produced by means of an SD printing process.
  • 3D printing processes are understood to be processes in which a shaped body is built up in layers from superimposed cross sections.
  • complex shaped bodies can also be generated by means of 3D printing processes.
  • the temporary shaped body is produced by means of a powder-based SD printing method, an extrusion-based 3D printing method or a suspension-based 3D printing method, preferably a powder-based SD printing method.
  • Powder-based 3D printing processes work with powder beds, the so-called powder bed, which are consolidated in layers in accordance with the shaped body to be produced locally with the aid of a binder or by the action of energy.
  • Powder-based 3D printing processes which achieve solidification of the powder bed with the aid of binders, include binder jetting, 3D powder printing.
  • Powder-based 3D printing processes which achieve solidification of the powder bed by the action of energy, are, for example, selective laser sintering (also referred to as SLS), which generates 3D laser sintering technology by partial heating by means of a laser individual layers.
  • SLS selective laser sintering
  • Suspension-based 3D printing processes include stereolithography (also referred to as SLA), liquid composite molding (also referred to as LCM), layer-slurry deposition, lithography-based processes, 3D screen printing.
  • SLA stereolithography
  • LCM liquid composite molding
  • layer-slurry deposition lithography-based processes
  • 3D screen printing 3D screen printing.
  • Extrusion-based 3D printing processes include, for example, melt-coating processes such as Fused Filament Fabrication (FFF) or Fused Deposition Modeling (FDM).
  • FFF Fused Filament Fabrication
  • FDM Fused Deposition Modeling
  • the cores may be fabricated using additive manufacturing techniques based on powder-based or suspension-based methods, preferably by SD laser sintering, selective laser sintering, 3D powder printing, gas assisted powder deposition, 3D screen printing, lithography based processes, SD thermoplastic printing or coating Slicker deposition can be generated.
  • the porous or dense water-soluble cores consisting of fine or coarse solid grains based on water-soluble carbohydrates or based on salt, sodium chloride or mixtures thereof by means of additive manufacturing processes based on powder-based or suspension-based methods preferably by means of 3D laser sintering technology, Selective laser sintering , 3 D powder pressure, gas assisted powder deposition, 3D screen printing, lithography based process, 3D Thermoplastic printing process or layer slurry deposition.
  • 3D laser sintering technology Selective laser sintering
  • 3 D powder pressure gas assisted powder deposition
  • 3D screen printing 3D screen printing
  • lithography based process 3D Thermoplastic printing process or layer slurry deposition.
  • Fine solid grains of sugar and / or salt are used, for example, for extrusion-based 3D printing processes.
  • Coarse solid grains of sugar and / or salt are used, for example, for laser sintering processes.
  • the porous or dense water-soluble cores consisting of fine or coarse solid grains based on water-soluble carbohydrates or based on salt, sodium chloride or mixtures thereof by means of the press molding, the plastic molding preferably by means of extrusion molding or casting on aqueous or not produced aqueous base and optionally post-treated mechanically and / or thermally.
  • the water-soluble cores are produced by uniaxial pressing, extrusion, injection molding or slip casting with special dispersing media.
  • these can be mechanically removed, e.g. be reworked by drilling, milling.
  • the porous water-soluble cores are based on water-soluble carbohydrates or based on salt, sodium chloride or mixtures thereof via direct foaming of an aqueous slurry consisting of dissolved carbohydrates with or without dissolved salt and its stabilization with the aid of further additives containing the Surface tension of the bubbles change, generated.
  • the porous water-soluble cores are based on water-soluble carbohydrates or on the basis of salt, for example sodium chloride; or mixtures thereof can be generated by direct foaming of an aqueous slip consisting of dissolved carbohydrates with or without dissolved salt and stabilization thereof by means of further additives which change the surface tension of the bubbles.
  • salt for example sodium chloride
  • Additives which change the surface tension of the bubbles are, for example, alcohol alkoxylates, acrylate copolymers, polyether siloxanes, silicone surfactants.
  • High-temperature-resistant materials in the context of the invention are materials which can be used permanently at temperatures of more than 600 ° C. and have sufficient mechanical properties over a long period of use.
  • High-temperature resistant materials according to the invention are ceramic or metallic materials or combinations thereof.
  • Thermal coating method according to the invention means thermal spraying. According to DIN EN 657, thermal spraying involves processes in which spray additives inside or outside of sprayers are fused, melted or melted onto a surface. The spray additives represent the coating material. The coating is preferably applied from high-temperature-resistant materials by means of flame or plasma spraying.
  • Coatings applied by means of thermal coating processes have a lamellar layer structure, the coating consisting of several superimposed layers of the coating material.
  • the coating of high-temperature-resistant materials applied in step b) by means of thermal coating processes comprises at least one layer of high-temperature-resistant materials.
  • step b) the coating of high-temperature-resistant materials is applied to at least one side of the temporary molded body by means of thermal coating methods.
  • step b) the coating of high-temperature-resistant materials is applied to at least one side of the compact temporary molded body by means of thermal coating methods.
  • step b) the coating of high-temperature-resistant materials is applied on all sides to the temporary molded body by means of thermal coating methods.
  • step b) the coating of high-temperature-resistant materials is applied on all sides to the open-cell cellular temporary shaped body by means of thermal coating methods.
  • step b) the coating of high-temperature-resistant materials is applied by means of computer-controlled thermal coating methods.
  • step b) the coating of high-temperature-resistant materials is applied on all sides with robot support and / or rotation of the temporary shaped body.
  • An apparatus for applying a coating of high temperature resistant materials to an open-cell cellular temporary shaped body on all sides comprises a thermal coating apparatus, a robotic arm, a computer controller, an apparatus for rotating the open cell cellular temporary shaped body.
  • the temporary shaped body is removed in step c).
  • the removal of the temporary shaped body takes place by dissolving the temporary shaped body.
  • the dissolution of the temporary shaped body is preferably carried out by means of a solvent.
  • the solvent used is water.
  • the temporary molding is removed by immersing the coated temporary molding in water.
  • the temporary shaped article is dissolved by spraying the coated temporary shaped article with water.
  • the high-temperature-resistant products according to the invention can be dried and used directly.
  • the method according to the invention takes into account not only economic and qualitative aspects but also ecological aspects.
  • the inventive method allows the saving of process steps, so eliminates the known from the Schwartzwalder method burning out of the temporary shaped body.
  • the material of the temporary shaped body can be recovered after the dissolution of the temporary shaped body in water, so that advantageous material is saved.
  • the exposed, flame or plasma sprayed ceramic, metal or metalloceramic high temperature resistant products have excellent thermal shock properties.
  • porous or dense lost, water-soluble cores consisting of fine or coarse solid grains are generated, which are thermally coated and subsequently be removed with the help of water.
  • porous or dense ceramic, metallic or metalloceramic high temperature products are made by combination of a thermal coating process such as flame spraying or plasma spraying of ceramics, metals or mixtures of metals and ceramics on porous or dense sugar-based or salt-based cores or mixtures thereof, wherein the porous or dense cores consist of fine or coarse solid grains which are water-soluble and are subsequently removed with the aid of water as the solvent.
  • a thermal coating process such as flame spraying or plasma spraying of ceramics, metals or mixtures of metals and ceramics on porous or dense sugar-based or salt-based cores or mixtures thereof, wherein the porous or dense cores consist of fine or coarse solid grains which are water-soluble and are subsequently removed with the aid of water as the solvent.
  • the melting point of the salt eg of sodium chloride, also designated as common salt of about 801 ° C. for a flame or plasma sprayed product suffice Technology, but also that of sugar, in a temperature range of 150 ° C to 180 ° C.
  • coarse or fine crystalline sugars are converted via SD laser sintering printer technology into complex porous or dense cores, which are then thermally coated by flame spraying.
  • dense or porous ceramic or metallic or metalloceramic materials are prepared by thermally coating porous or dense water-soluble cores consisting of fine or coarse solid grains by flame spraying or plasma spraying, and then removing the cores in a water bath.
  • an intermediate layer of ceramic materials, of carbon or of salt is applied to the temporary shaped body before step b) by means of a cold coating method.
  • Ceramic materials include oxide or non-oxide ceramic materials. In one embodiment, an intermediate layer of non-oxide ceramic materials is applied. Non-oxide materials include boron nitride and silicon nitride.
  • an intermediate layer of salt is applied to the temporary shaped body.
  • Cold coating processes in the context of the invention are coating processes in which the material of the intermediate layer is present at a temperature of less than or equal to 50 ° C. and applied to the temporary shaped body.
  • Cold coating methods are, for example, spray methods, dipping methods, impregnation methods or deposition methods.
  • the intermediate layer is applied by spraying or dipping.
  • the intermediate layer is applied to a temporary shaped body of sugar and / or salt, preferably a temporary shaped body of sugar.
  • the intermediate layer serves for the thermal stabilization of the temporary shaped body for the subsequent thermal coating.
  • the intermediate layer applied before step b) is a temporary intermediate layer.
  • Temporary intermediate layer according to the invention means that the intermediate layer is removed in a subsequent process step, preferably the temporary intermediate layer is removed in step c).
  • the intermediate layer remains at least partially preserved after removal of the temporary shaped article in step c). In one embodiment, the intermediate layer is applied to the temporary shaped body with a layer thickness of 1 ⁇ m to 500 ⁇ m.
  • the sugar cores are coated prior to thermal coating with a boron nitride or silicon nitride slurry in the cold state at room temperature by means of spraying or impregnation.
  • an intermediate layer of carbon is deposited on the temporary shaped body after step a) and before step b).
  • the carbon can be advantageously adjusted based on the combustion of acetylene at the beginning of the flame spraying process.
  • carbon deposits are generated based on the combustion of acetylene on a water-soluble substrate.
  • the water-soluble cores are coated at room temperature with a boron nitride or silicon nitride-based impregnating or spraying film.
  • the coating of high-temperature-resistant materials having a layer thickness of 3 ⁇ m to 20 mm is applied in step b), preferably with a layer thickness of 40 ⁇ m to 10 mm.
  • step b) the coating of high-temperature-resistant materials having a locally varying layer thickness is applied to the temporary shaped body.
  • a local reinforcement of the high temperature resistant product can be achieved thereby.
  • a local reinforcement of the high temperature resistant product is used, for example, in crucibles to locally increase the mechanical stability of the high temperature resistant product.
  • the temporary shaped body has a porosity of 5 to 97% by volume.
  • Temporary moldings with a porosity of ⁇ 45% by volume are preferably used for the production of compact high-temperature-resistant products, such as, for example, spout components, such as spout nozzles or also crucibles for melting metals.
  • Temporary shaped articles with a porosity of> 45% by volume are preferably used for the production of porous high-temperature-resistant products, such as filters for molten metal filtration.
  • the high temperature resistant product after step c) is thermally treated at a temperature of 50 to 2000 ° C.
  • the thermal after-treatment of the high-temperature-resistant product increases the strength of the high-temperature-resistant products, reduces the porosity and / or achieves a phase transformation of the applied high-temperature-resistant materials.
  • the high temperature resistant product after step c) is thermally treated at a temperature of at most 150 ° C.
  • the drying of the high-temperature-resistant product is achieved after the release of the temporary molded body.
  • the high temperature resistant product after step c) is thermally treated at a temperature of 600 ° C to 1000 ° C.
  • this increases the strength of the high temperature resistant product, reduces porosity, and achieves phase transformation within the high temperature resistant materials.
  • the dense or porous ceramic or metallic or metalloceramic products are optionally thermally post-treated at a temperature of between 50 to 2000 ° C.
  • the applied by thermal coating method coating with ceramic materials, metallic materials or mixtures thereof.
  • metallic materials applied in step b) are selected from:
  • Metallic materials with a melting point greater than 1000 ° C are Cu, Fe, Si, Ni, Ti or mixtures thereof.
  • Intermetallic phases are known to the expert homogeneous mixtures of two or more metals, such as high temperature materials such as NiAl, TiCr2, TaFeAl or high-temperature lightweight materials such as Ti3AI, TiAl or the sigma phase FeCr.
  • the intermetallic phases are chemically resistant and have a high melting point.
  • Refractory metals in the context of the invention are refractory, base metals of the 4th, 5th, 6th or 7th subgroup of the periodic table with a melting point greater than 1600 ° C. or mixtures of these metals.
  • Base metals of the 4th subgroup are, for example, Ti, Zr, Hf.
  • Base metals of the 5th subgroup are, for example, V, Nb or Ta.
  • Common metals of the 6th subgroup are, for example, Cr, Mo or W.
  • Unwanted metals of the 7th subgroup are, for example Mn, Tc or Re.
  • grains used in flame spraying or plasma spraying are ceramic or metallic or intermetallic phases or mixtures thereof.
  • ceramic materials applied in step b) are selected from oxidic ceramic, non-oxidic ceramic materials or combinations thereof.
  • the oxide ceramic materials are selected from: calcium oxide, magnesium oxide, dolomite, chromium oxide, aluminum oxide, mullite, zirconium mullite, zirconium dioxide, magnesium aluminate spinel, bauxite, yttrium oxide, titanium dioxide, lanthana, lanthanum chromium or mixtures thereof.
  • Calcium oxide, magnesium oxide, dolomite, chromium oxide, aluminum oxide, mullite, zirconium matte, zirconium dioxide, magnesium aluminate spinel, bauxite, yttrium oxide, titanium dioxide, lanthanum oxide, lanthanum chromium or combinations or mixtures thereof are used as oxidic grains in flame spraying or plasma spraying.
  • oxidic grains used in flame spraying or plasma spraying are ceria oxide, magnesium oxide, dolomite, chromium oxide, aluminum oxide, mullite, zirconium mullite, zirconium dioxide, magnesium aluminate spinel, bauxite, yttrium oxide, titanium dioxide, lanthanum oxide, lanthanum chromium or combinations or mixtures.
  • the oxide, the carbides or the nitrides of the refractory metals can serve as oxidic or non-oxidic ceramic materials.
  • the non-oxide ceramic materials are selected from silicon carbide, silicon nitride, boron nitride, boron carbide, aluminum nitride and carbon or mixtures thereof.
  • the non-oxidic grains may be silicon carbide, silicon nitride, boron nitride, boron carbide, aluminum nitride and carbon, or combinations or mixtures thereof.
  • silicon carbide, silicon nitride, boron nitride, boron carbide, aluminum nitride and carbon or combinations or mixtures of these are used as non-oxidic grains in flame spraying or plasma spraying.
  • the metallic materials having a melting temperature greater than 1000 ° C are selected from: Cu, Fe, Si, Ni, Ti, or mixtures thereof.
  • metals for the thermal spraying with a melting point above 1000 ° C serve Cu, Fe, Si, Ni, Ti or mixtures thereof.
  • the refractory metals are selected from Zr, Hf, V, Nb, Ta, Cr, Mo, W, Tc, Re or mixtures thereof.
  • refractory metals are preferably Zr, Hf, V, Nb, Ta, Cr, Mo, W, Tc, Re or mixtures thereof.
  • the metal grains used in flame spraying or plasma spraying are Cu, Fe, Si, Ni, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Tc, Re or mixtures thereof.
  • the intermetallic phases having a melting temperature greater than 1000 ° C are selected from: NiAl, TiCr2, TaFeAI, T13AI, TiAl, FeCr, or mixtures thereof.
  • intermetallic phases such as e.g. NiAl, TiCr2, TaFeAI, TI3AI, TiAl, FeCr or mixtures thereof.
  • the grain sizes used in flame spraying or plasma spraying are intermetallic phases NiAl, TiCr, TaFeAl, TbAl, TiAl, FeCr or mixtures thereof.
  • the process of the present invention can advantageously produce high temperature products such as spouts for metallurgy, core shells for metal foundries, ceramic or metallo-ceramic filters for molten metal filtration, heat shields for power engineering, slide plate inlays, molds for the glass industry, complex components e.g. Catalyst supports for the chemical industry, mixing components for homogenizing molten metal or complex components for the automotive industry are produced.
  • high temperature products such as spouts for metallurgy, core shells for metal foundries, ceramic or metallo-ceramic filters for molten metal filtration, heat shields for power engineering, slide plate inlays, molds for the glass industry, complex components e.g. Catalyst supports for the chemical industry, mixing components for homogenizing molten metal or complex components for the automotive industry are produced.
  • crucibles for the melting of metals from ceramic materials such as Al 2 O 3, mullite, ZrO 2 or aluminum titanate, which have a better thermal shock resistance, can be produced by the method according to the invention.
  • Foam filters for molten metal filtration of ceramic materials such as Al 2 O 3, for example, which have better thermal shock resistance and dimensional stability than ceramic foam filters produced by the Schwartzwalder process, can preferably be produced by the process according to the invention.
  • the high-temperature-resistant products produced by the process according to the invention have a lamellar structure of the applied coating of high-temperature-resistant materials, so that advantageously the thermal shock resistance of the high-temperature resistant products is improved.
  • the high temperature resistant products made by the process of the invention have a porosity of from 5% to 90% by volume.
  • High-temperature-resistant products having a porosity of> 45% by volume, prepared by the process according to the invention, are used, for example, as filters for molten metal filtration.
  • High-temperature-resistant products having a porosity of ⁇ 45% by volume, produced by the process according to the invention, are preferably used, for example, as spout components or crucibles in metallurgy.
  • a plurality of high temperature resistant products will be joined together by thermal coating.
  • porous high-temperature-resistant products having complex structures and large dimensions can be produced by joining together a plurality of high-temperature-resistant products produced by the method according to the invention by means of thermal coating methods.
  • the coating of high-temperature-resistant materials is applied on all sides on the open-cell cellular shaped body used for the production of porous high-temperature resistant products.
  • porous high-temperature resistant products can be produced with enlarged dimensions.
  • Fig. 1 shows a cross-sectional view of a coated compact temporary shaped body for producing a high-temperature resistant nozzle for metallurgy.
  • Fig. 2 shows a cellular temporary molded body used to make a ceramic filter for molten metal filtration.
  • Fig. 3 shows a cross-sectional view of a coated compact temporary molded article for producing a crucible for melting metals.
  • Example 1 Hollow body of a spout nozzle for metallurgy
  • Fig. 1 shows the cross-sectional view of a coated compact temporary shaped body of sugar 1 for producing a high-temperature resistant pouring spout for metallurgy.
  • laser sintering the so-called laser sintering technology (laser sintering)
  • a water-soluble, wedge-shaped sugar core is produced as a compact, temporary shaped body 1 of a pouring nozzle.
  • a powder bed of 90 wt .-% maltose and 10 wt .-% impurities with particle sizes in the range of 40 to 60 ⁇ is used.
  • the powder bed of maltose is solidified by energy input by a laser, with a sintering temperature of 120 ° C with a 14 W C02 laser with a focus diameter of 100 ⁇ and 50% power throttling is achieved. Subsequently, the next layer of a powder bed of maltose is applied and solidified by the entry of laser energy.
  • the maltose sugar kernel 1 produced in this way has a height of 100 mm, an outer diameter of 20 mm at the inlet and 10 mm at the outlet. The nuclear production took about 4 hours.
  • Feed rate of spray material mm / min 50
  • the exposed spout nozzle has the dimensions: height of 120 mm, inner diameter at the inlet 20 mm and at the outlet 10 mm and a wall thickness of about 5 mm.
  • Example 2 ceramic filter for molten metal filtration
  • Fig. 2 shows a cellular temporary molded body 3 used for producing a ceramic filter for molten metal filtration.
  • a cellular temporary shaped body of salt 3 was produced.
  • layer by layer of common salt consisting of 90 wt .-% sodium chloride and 10 wt .-% impurities with particle sizes in the range of 40 to 80 ⁇ applied as a powder bed and solidified in layers by means of energy input by a laser.
  • a 1000 W C02 laser with a focus diameter of 100 ⁇ a sintering temperature of 780 ° C was achieved.
  • the cellular temporary shaped body 3 thus produced has an open-cell spongy structure of the pore class 10 ppi with a porosity of 95% by volume and has the dimensions 50 ⁇ 50 ⁇ 25 mm 3 .
  • the coating of the open-cell cellular temporary shaped body 3 takes place by means of flame spraying, wherein an acetylene-oxygen mixture is used as the fuel gas.
  • flame spraying a coating consisting of 99.7% by weight of Al 2 O 3 and 0.3% by weight of other oxides as impurities having a layer thickness of 500 ⁇ m is applied on all sides, rotating the open-cell cellular temporary shaped body 3.
  • Table 2 gives the parameters of flame spraying: Table 2: Parameters for flame spraying
  • the open cell cellular temporary shaped body is removed.
  • the coated temporary molded body is immersed in a water bath
  • the ceramic filter obtained after removal of the temporary molded body was dried at 150 ° C for 24 hours.
  • the ceramic filter produced in this way shows improved form retention compared with a ceramic Ab03 foam filter produced by the Schwartzwalder process.
  • Fig. 3 shows a cross-sectional view of a coated compact temporary molded article 1 for producing a crucible for melting metals.
  • the compact temporary shaped body 1 was produced by means of an extrusion-based 3 D printing process. For this purpose, a mixture of 70 wt .-% sodium chloride, 4 wt .-% sucrose with particle sizes less than 40 ⁇ was homogeneously dispersed with the addition of 24 wt .-% ethanol as a solvent and 2 wt .-% organic additives. The mass thus produced was heated in an extruder and the temporary molded body 1 was produced in layers therefrom.
  • the thus produced compact temporary molded body 1 has the dimensions: height 140 mm and outer diameter of 120 mm and a wall thickness of 5 mm and has a porosity of 25 vol .-%.
  • an intermediate layer of salt is applied by dipping the temporary shaped body in a dispersed salt solution.
  • the intermediate layer has a layer thickness of 500 ⁇ m.
  • the coating of the compact temporary molded body 1 by means of flame spraying wherein an acetylene-oxygen mixture is used as the fuel gas.
  • flame spraying is on one side of the temporary molded body 1, a coating consisting of 99.7 wt .-% Al2O3 and 0.3 wt .-% of other oxides applied as impurities with a layer thickness of 10 mm.
  • Table 3 gives the parameters of flame spraying:
  • an increased layer thickness of the Al 2 O 3 coating was locally applied in order to achieve a local reinforcement of the high-temperature-resistant crucible.
  • the coating is applied by means of flame spraying with a layer thickness of 15 mm.
  • the exposed crucible has a filling volume of 250 ml with the dimensions height 140 mm, outside diameter 1 10 mm and a wall thickness of 10 mm.
  • the ceramic crucible obtained after removal of the temporary molded body was dried at 150 ° C for 24 hours.

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Filtering Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention concerne un procédé de fabrication de produits résistant aux températures élevées, ce procédé comprenant les étapes suivantes : a) production d'un corps façonné temporaire en sel et/ou en sucre par un procédé de fabrication additive, b) application d'un revêtement constitué de matières résistant aux températures élevées sur le corps façonné temporaire par un procédé de revêtement thermique, c) élimination du corps façonné temporaire. Le revêtement constitué de matières résistant aux températures élevées est appliqué sur le corps façonné temporaire de telle sorte qu'il forme le produit résistant aux températures élevées après l'élimination du corps façonné temporaire à l'étape c).
PCT/EP2018/051864 2017-01-25 2018-01-25 Procédé de fabrication de produits résistant aux températures élevées présentant des propriétés thermomécaniques améliorées Ceased WO2018138210A1 (fr)

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WO2020127980A1 (fr) * 2018-12-20 2020-06-25 Proionic Gmbh Composition à mouler comprenant un composant à base de sucre
DE102019219132A1 (de) * 2019-12-09 2021-06-10 Volkswagen Aktiengesellschaft Verfahren und Vorrichtung zur Herstellung eines Gusskerns und ein Verfahren zur Herstellung eines Gussteils sowie ein Kraftfahrzeug
DE102020107742A1 (de) 2020-03-20 2021-09-23 Bayerische Motoren Werke Aktiengesellschaft Verfahren zur Herstellung eines Formkörpers
DE102022106739A1 (de) 2021-05-04 2022-11-10 GM Global Technology Operations LLC Verfahren zur herstellung eines keramikfilters für den metallguss
US11992874B2 (en) 2021-05-04 2024-05-28 GM Global Technology Operations LLC Process to make a ceramic filter for metal casting

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Publication number Priority date Publication date Assignee Title
WO2020127980A1 (fr) * 2018-12-20 2020-06-25 Proionic Gmbh Composition à mouler comprenant un composant à base de sucre
CN113195194A (zh) * 2018-12-20 2021-07-30 普罗奥尼克股份有限公司 包括糖组分的模塑组合物
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JP2024016091A (ja) * 2018-12-20 2024-02-06 プロイオニック ゲーエムベーハー 糖成分を含む成形用組成物
DE102019219132A1 (de) * 2019-12-09 2021-06-10 Volkswagen Aktiengesellschaft Verfahren und Vorrichtung zur Herstellung eines Gusskerns und ein Verfahren zur Herstellung eines Gussteils sowie ein Kraftfahrzeug
DE102020107742A1 (de) 2020-03-20 2021-09-23 Bayerische Motoren Werke Aktiengesellschaft Verfahren zur Herstellung eines Formkörpers
DE102022106739A1 (de) 2021-05-04 2022-11-10 GM Global Technology Operations LLC Verfahren zur herstellung eines keramikfilters für den metallguss
US11992874B2 (en) 2021-05-04 2024-05-28 GM Global Technology Operations LLC Process to make a ceramic filter for metal casting
DE102022106739B4 (de) 2021-05-04 2024-05-29 GM Global Technology Operations LLC Keramikschaumfilter

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