EP3063103A2 - Matériau à structure polyphasée - Google Patents

Matériau à structure polyphasée

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Publication number
EP3063103A2
EP3063103A2 EP14812120.5A EP14812120A EP3063103A2 EP 3063103 A2 EP3063103 A2 EP 3063103A2 EP 14812120 A EP14812120 A EP 14812120A EP 3063103 A2 EP3063103 A2 EP 3063103A2
Authority
EP
European Patent Office
Prior art keywords
phase
article
component
material according
mpa
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.)
Pending
Application number
EP14812120.5A
Other languages
German (de)
English (en)
Inventor
Erich Neubauer
Michael KITZMANTEL
Gottfried KLADLER
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Publication of EP3063103A2 publication Critical patent/EP3063103A2/fr
Pending 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/12—Metallic powder containing non-metallic particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/14—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by a layer differing constitutionally or physically in different parts, e.g. denser near its faces
    • 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
    • C04B35/01—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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486—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
    • C04B35/01—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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486—Fine ceramics
    • C04B35/488—Composites
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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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • 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
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    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • 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
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0466—Alloys based on noble metals
    • G—PHYSICS
    • G04—HOROLOGY
    • G04B—MECHANICALLY-DRIVEN CLOCKS OR WATCHES; MECHANICAL PARTS OF CLOCKS OR WATCHES IN GENERAL; TIME PIECES USING THE POSITION OF THE SUN, MOON OR STARS
    • G04B37/00—Cases
    • G04B37/22—Materials or processes of manufacturing pocket watch or wrist watch cases
    • A—HUMAN NECESSITIES
    • A44—HABERDASHERY; JEWELLERY
    • A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C1/00—Brooches or clips in their decorative or ornamental aspect
    • A—HUMAN NECESSITIES
    • A44—HABERDASHERY; JEWELLERY
    • A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C3/00—Medals; Badges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • 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
    • C04B2235/02—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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
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    • C04B2235/40—Metallic constituents or additives not added as binding phase
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Definitions

  • the invention relates to a material with a multi-phase structure comprising at least a first solid phase and at least one second solid phase, wherein the individual phases are characterized in that they are present in a macrostructure and are distinguishable from the naked eye.
  • the invention further relates to a method for producing this material and the use of the material.
  • components having a macrostructure e.g., watch cases, rings, pendants, etc.
  • These components are characterized by a visually striking and appealing, two- or multi-colored pattern.
  • the pattern is formed by an arrangement of two or more different metals in a periodic or irregular manner, wherein a plurality of process steps is required.
  • the process is limited to the use of ductile metals, i. on materials that can be reshaped especially at room temperature without the application of temperature.
  • the individual process steps of the above-mentioned method can basically be described as follows. First, (1) metal foils of two or more metals are stacked alternately and then together via a taking place under pressure and temperature (2) diffusion process to a multilayer semi-finished product connected. For example, one (3) rod is cut out of the multi-layer semifinished product and this one
  • the invention therefore aims to provide a material with a multi-phase structure and to provide a production method with which the abovementioned disadvantages can be avoided.
  • the invention is an extended material variety and allow a significant reduction of the process steps.
  • the invention provides a material with a multiphase structure comprising at least a first solid phase and at least one second solid phase,
  • first phase and the second phase are each a metal, a metal alloy, a ceramic material or combinations thereof in the form of a composite material
  • phase of the microstructure are macroscopically distinguishable from each other
  • multiphase microstructure is formed as an interstitial structure or as a three-dimensional interpenetration microstructure
  • the storage structure comprises the first phase and in three spatial dimensions continuously occurring matrix phase and the second phase as a discontinuous, randomly distributed interstitial phase, and - wherein the first phase is prepared from powders producible in the course of the process ⁇ by sintering.
  • the at least two phases are macroscopic, ie as far as visible to the naked eye, sharply delimited from one another. Only at the microscopic level can reaction products and intermediate phases of reactions at the interfaces between the phases be present in the interface region between two phases. Furthermore, reaction products of reactions of the phases with oxygen, carbon and / or nitrogen may be included. Based on the total volume of the workpiece, the described reaction products and intermediate phases are preferred but only in an amount of less than 10 vol. -% available.
  • the multiphase structure according to the invention is designed either as a bedding structure or as a penetration structure.
  • An intercalation structure is present if at least one phase (intercalation phase) is intermittently incorporated into at least one other, continuous phase (matrix phase).
  • the matrix phase occurs continuously in three spatial dimensions, and the particles of the intercalation phase are arranged distributed in three spatial dimensions in the matrix phase.
  • the embedded phase may well be present in higher concentration than the matrix phase.
  • a preferred orientation of the individual phases in one or two spatial directions may occur.
  • Penetration structures are given when all the phases represented in the material occur continuously. This is generally the case when the phases in the form of sponge-like three-dimensional network structures penetrate through ⁇ .
  • the phases of the microstructure are macroscopically, ie, recognizable with the naked eye, distinguishable from each other. This means that the microstructure is limited to the structures visible to the naked eye.
  • the second phase has discontinuous areas, each having an area of at least 0.2 mm 2, preferably at least 1 mm 2 in the projection. Towards the top, the discontinuous regions of the second phase are limited to a diameter of, for example, 10 mm.
  • the phases of the material can each be composed of atoms of a single chemical element, so that there is a pure phase. However, the phases can also exist as alloy or composite material (mixed phase). If a composite material is used for the first phase and / or the second phase, then this preferably consists of a matrix of a first substance into which fillers having a particle size of ⁇ 100 m are introduced. This substructure can not be resolved with the naked eye without the aid of optical aids.
  • the invention allows the use of a variety of different materials.
  • the first phase is preferably formed from a metal, a metal alloy, a metallic composite material, a ceramic material, a metal-ceramic composite material or a ceramic composite material.
  • the second phase is preferably of a metal, a metal alloy, a metallic composite material, a ceramic material, a metal-ceramic composite fabric, a ceramic composite material, plastic or a plastic composite material formed.
  • the material of the first phase and the material of the second phase during the manufacturing process do not form an alloy, but form separate, sharply demarcated phases. In each case, only similar particles agglomerate with each other to form the individual phases.
  • the microstructure of the material preferably results from a random arrangement or mixture of the powder, powder granular or particulate starting components "in situ" during its production. The large number of usable materials is made possible by the fact that the first phase is produced according to the invention by sintering.
  • a pulverulent or powder-granular component is used, which is sintered in a compression operation under temperature and pressure.
  • the compression process process parameters are preferably used here, which on the one hand prevent a significant diffusion / reaction for the respective material combination
  • the process must take long enough or the temperatures should be so high that, in the case of the use of powder granules, these become a dense body internally and there is a positive connection of the individual components, ideally with a very well controlled, low diffusion zone.
  • composition there is no limitation of the composition to metals with high ductility at room temperature or with good forming behavior at elevated temperature, or the production technology used does not require intermediate annealing in order to allow further forming steps.
  • the material according to the invention is produced by means of a compression process, in contrast to the repeated repetition of forming steps in the prior art.
  • the composites produced can be made using appropriate combinations of the starting powders and process engineering to be made with a random (non-deterministic) macrostructure.
  • the composite materials produced allow phases with very high hardness and wear resistance if the individual phases are made up of a substructure, ie a matrix in which hard-material particles in the micro-scale region are introduced.
  • the first phase is made of a material with a lower sintering or deformation temperature than the second phase.
  • a material with a lower sintering or deformation temperature than the second phase.
  • the sintering temperature is meant here the temperature at which the powdery starting components grow together via diffusion processes to form a solid. Depending on the material, this temperature is about 0.5-0.95% of the melting point (measured in Kelvin) of the starting component.
  • the forming temperature or deformation temperature is a temperature at which the material starts to flow when using pressure and temperature, or plastic deformation occurs.
  • the second phase can also be formed by sintering.
  • the second phase may be prepared by incorporating particles in the initial phase in their initial powdered state.
  • the storage takes place, for example, in that a mixture of the powder or powder granules of the first component with the particles of the second component is produced. Thereafter, the mixture is subjected to a densification process whereby the first phase is sintered and the particles of the second component are sintered in the sintered first phase, respectively be included.
  • the particles of the second component may be subjected to a forming process.
  • the particles have a length to diameter ratio of 1: 1 to 3: 1.
  • the particles are formed, for example, as spheres, ellipsoids, flakes, platelets, chips, sheets, pieces of sheet metal, wires, fragments or the like.
  • a preferred development further provides that the particles have a mean volume equivalent ball diameter of 0.3-lOmm, preferably 0, 5-3mm.
  • the particles of the second phase can be either identically oriented or randomly oriented.
  • both the first phase and the second phase is a metal.
  • the first and second phases are each a noble metal or a noble metal alloy, e.g. is a platinum group element or alloy.
  • ceramic particles may form the second phase, which are randomly distributed in a sintered metal phase.
  • the first phase consists of a material having a thermal conductivity of> 150 W / mK, such as Ag, Cu or Al, and the second phase of a material having a thermal expansion of ⁇ 8 ppm / K, such as W, Mo , TiB 2 , Zr (Wo 4 ) 2 ⁇
  • the first and / or the second phase is a composite material which has a continuous matrix in which at least one particulate filler is introduced.
  • the volume fraction of the first phase is preferably 10-95%, preferably 30-70%, preferably 40-60%.
  • the volume fraction of the second, in particular produced by sintering phase is 10-95%, preferably 30-70%, preferably 40-60%.
  • the second phase is not formed by sintering but by particles
  • a preferred development provides that the volume fraction of the second phase produced by incorporation of particles into the first phase is 10-60%, preferably 20-50%, preferably 30-50%. 40%.
  • the embedded particles with a size of preferably at least 300 ⁇ are present.
  • the invention relates to a method for producing the above-described material from at least one first powdered or powdered granular component and at least one second component, comprising the following steps:
  • the procedure is such that the second component is used in powder form or as powder granules and is sintered in the compacting step to form a second phase of the multiphase structure.
  • the powder of the first phase and possibly the second phase preferably has a particle size of ⁇ 300 pm, preferably ⁇ , preferably ⁇ 100 ⁇ m, preferably ⁇ 50 ⁇ m.
  • the densification step is designed as hot pressing, hot isostatic pressing, direct hot pressing, spark plasma sintering, pressing and sintering or extrusion, and their modified forms.
  • the densification step preferably comprises the application of pressure at a rate of> 0.001 MPa / s, preferably> 0.1 MPa / s and more preferably> 10 MPa / s.
  • the pressure application rate is preferably at most 10 6 MPa / s.
  • the densification step may include a heat input at a heating rate of> 10 K / min, preferably> 100 K / min, more preferably> 1000 K / min.
  • the densification step preferably comprises, after the application of pressure and the introduction of heat, a holding step in which the temperature and the pressure are maintained for a period of ⁇ 6 hours, preferably ⁇ 1 hour, more preferably 1-60 seconds.
  • the pressure during the holding step is preferably> 1 MPa, preferably> 10 MPa, particularly preferably> 100 MPa.
  • the compression step can be carried out in protective gas, vacuum or in air. According to another embodiment of the invention, the manufacturing process is carried out as follows.
  • Step 1 involves the preparation of the starting components.
  • the following starting components can be used:
  • the first component is in particular a powder of sinterable metallic or ceramic particles. These powders may have particle sizes of less than 300 ⁇ m, preferably less than 100 ⁇ m, particularly preferably less than 45 ⁇ m.
  • the first component can also consist of powder granules. These arise from the fact that sinterable metal or ceramic powder with water or by solvent addition (eg via spray drying, freeze drying ⁇ or the like.), Or with granulation aids (such as binder components, polymers, waxes) in granules having a size of 0.5 - 10mm preferably 1 to 5 mm transferred.
  • granulation aids such as binder components, polymers, waxes
  • the second component may consist of another powder of a sinterable metallic or ceramic particle. These powders may have particle sizes of less than 300 m, preferably less than ⁇ , more preferably less than 45 ⁇ ⁇ . Likewise, the second component may be made from powder granules (such as the first component). Another embodiment includes the possibility that the second component may be formed of particles having a one-dimensionally or two-dimensionally directed shape, such as wire pieces or wires having a diameter of 0.3 mm to 5 mm, preferably 0.5 mm to 2 mm or fibers with a diameter of 0.3mm to 5mm, preferably 0.5mm to 2mm, or flakes, flakes, chips, sheets or pieces of sheet metal.
  • the particles have characteristic dimensions with a length which is greater than the thickness, wherein the thickness of the particles is in a range of 0.1 mm to 5 mm, preferably 0.5 mm to 1 mm.
  • the particles must be distinguished by having ductile properties at room temperature and / or when applying pressure and temperature.
  • the second component may also be formed by particles having a regular (e.g., spheres) or irregular shape (e.g., fragments, chips ). These fillers may have an average diameter of 0.3 mm to 10 mm, preferably between 1 mm and 5 mm.
  • the particles of this type may, for example, be easily deformable bulk materials with the possibility of deformation under the action of pressure and temperature.
  • Step 2 may also be non-deformable or difficultly deformable materials which are substantially inert in a matrix: here, in particular ceramic fillers or carbon-based fillers, in particular diamond, which are not easy even when using very high temperatures and pressures could be deformed.
  • the shaping takes place.
  • the mixture is poured into a suitable mold and compressed at room temperature by applying pressure, so that a stable, handleable "green part" is produced.
  • a particular embodiment in this context includes the layer-by-layer filling of a mold, wherein layers of different concentrations of the individual phases are combined here.
  • a gradient material, a sandwich or multilayer material can be produced. It is likewise possible to selectively introduce the multiphase material locally or to press it directly onto a carrier body.
  • the mixture can also be filled directly into the mold and then subjected to the compression process at temperature and pressure.
  • the green compact - After the presence of the green body of this - if it contains a high proportion of plastic binder - in one optional debinding step to be freed from the binder. Subsequently, the green compact - provided with a release agent - used in a suitable mold and compacted using pressure and temperature to form a compact component.
  • the additional shaping step described here can also be dispensed with - depending on the compression method - and the compression of the starting material can be carried out directly in the mold.
  • the multiphase material of layers of different composition of the individual phases can be placed as a gradient material, in a sandwich design or else as an insert in a targeted manner. At the same time can be pressed directly onto a body.
  • process parameters are used which, on the one hand, prevent a significant diffusion / reaction between the individual components for the respective material combination, which would lead to an extinction of the desired multi-phase structure.
  • the process must take long enough or the temperatures should be so high that, in the case of the use of powder granules, these sinter into a dense body and there is a positive connection of the individual components, ideally with a very well controlled, low diffusion zone.
  • Step 5 in the process taking place in the air, in the course of production, in addition, a rapid ⁇ breckreckvorgang done and possibly also the reactions with the atmosphere can be exploited.
  • a rapid compaction process makes it possible to retain very fine-grained microstructures of the sintered phases, which has an advantageous effect on the material properties of the end product.
  • an additional heat treatment can optionally be used, in particular when very rapid compaction processes are used. This can be used for the controlled formation of a diffusion zone, or to relax tension in the material.
  • a forming process can optionally take place, which makes it possible, for example, to convert semifinished products into other geometries and also to produce a certain preferred orientation thereof.
  • Prerequisite for this forming Steps is the appropriate ductility of the materials.
  • Possible processes are forming processes, such as rolling, drawing, hammering, rolling, extruding, Severe Plastic Deformation.
  • processes such as turning, milling, grinding, wire eroding, die sinking, laser machining or the like. are used to influence the geometry of the semifinished product or to perform a surface finish.
  • ⁇ v / ground optional additional process for the surface treatment can be made ⁇ v / ground. These may have the task of changing the color of the component or influencing the material properties such as hardness or wear resistance.
  • the methods of surface treatment may include the following methods:
  • Thermodiffiffusion treatment The component is provided with powdery or paste-like sizes. By a heat treatment e s comes to the reaction of the
  • the heat treatment can lead to the formation of reactions that lead to a different visual appearance or change the functional properties of the component (s).
  • Oxygen and / or nitrogen, used to form reaction products on the surface of the component generate, for example, nitrides or oxides.
  • the heat treatment can also take place in air.
  • a chemical treatment using current / voltage can be used, for example, to anodize surfaces. It can be influenced by the selection of electrolytes and the voltage / current characteristic, the layer thicknesses of generated nitrides / oxides, etc.
  • a transparent wear resistant layer e.g. with diamond, DLC or lacquer / plastic layers.
  • Step 1 Preparation of the .usga ngsko m pon duck n
  • Step 2 Weigh in and mix the components
  • Step 3 Forming by pressure assist process (making a "green”) alternatively directly to step 4
  • Step 4 Compress the components by exposure to pressure and / or temperature (e.g., by hot pressing, spark plasma sintering, etc.).
  • Step 5 Optional: Heat Treatment
  • Step 6 Optional: Forming process (e.g., rolling, extruding, hammering, etc.)
  • Step 7 Finishing the over-aged texture
  • Step 8 Optional: Surface finish such as hardening, coating or etching
  • the invention makes it possible to produce objects whose multiphase structure gives a unique and individual macrostructure which can be used, for example, as an authentication feature or security element. Since the macrostructure obtained according to the invention is not reproducible, it can not be copied.
  • the inventive or inventively producible material is particularly suitable for the production of jewelry, luxury items and technical functional materials.
  • the non-determined macrostructure Of particular use, in particular in the jewelery and luxury goods sector, is the non-determined macrostructure. This gives the products uniqueness due to their aesthetic appearance, especially when it comes to precious metals or elements of the platinum group and their alloys, and also represents a security element at the same time.
  • the surface of an article having the macrostructure simultaneously has a copy protection function, since it is difficult to reproduce the non-deterministic macrostructure without a considerable effort.
  • the macro structure can be used with the possibility of unique identification to produce high-quality investment objects such as coins, medals and bars. This is particularly advantageous when materials are used with ductility, as they can be subsequently stamped. Also here is a combination with other materials possible, so for example bi-metal coins are made, which consist of a metal edge in which an insert of the composite material is embedded with macrostructure in the center or vice versa.
  • Security features based on numbers, image codes or holograms, such as those used in software, are only of limited use in the jewelry and luxury goods sector because they change the external appearance.
  • holograms and security features made of plastic with relief structure are used or pigments with special properties.
  • the present invention provides a solution by using the non-deterministic macrostructure characterized by bi- or multicolor.
  • these materials are visually appealing and can therefore be used for luxury items and jewelry, especially if they are composed of precious metals or elements of the platinum group and their alloys.
  • the two- or multi-color macrostructure not only satisfies the aesthetic appearance requirement, but at the same time makes it possible to use this hard-copy macro pattern as a security element.
  • a picture Identification software can be generated from the optical differences, for example, in terms of color or reflectance, emissivity or the like, a unique code.
  • a semifinished product consisting of two or more phases, which differ in their visual appearance, for example, in terms of color or reflectance, by processes of forming or mechanical processing, eg by milling, turning or the like.
  • a component transferred the following in the Schuck, luxury and premium product range is used, such as watch cases, rings, mobile phone cases, etc.
  • the procedure can be such that the manufacturer of a product consisting of the material or containing it creates an image of the macrostructure on the surface, wherein the image detail covers the entire product or only a defined area thereof. This image is uniquely assigned to the product as an authentication feature. If possible copies appear on the market, then the characteristic pattern can be determined via the image recognition and compared with the database of the manufacturer.
  • the macrostructure of the product can be converted into a binary pattern by means of image recognition and a numerical code can be generated by means of an algorithm. This number code can be used as a second security feature.
  • dendritic copper powder As the first component dendritic copper powder is used with a particle size ⁇ 45 ⁇ . This powder is added with the addition of a dissolved in alcohol granulation binder
  • the body is debindered in an oven at a temperature of 450 ° C, so that the wax components are removed.
  • the green compact is placed in a heated to 750 0 C mold and compressed by applying 100 MPa pressure in 30 seconds in air and then expelled from the mold.
  • the material can be quenched directly in water or oil. After compaction, the ring blank is turned and then finely polished. The relative density is 99.9% of the theoretically calculated density.
  • the blank is shown in FIG. 5 is shown.
  • Example 1 A similar procedure is chosen as in Example 1. Instead of copper, titanium powder with a particle size ⁇ 45 m is used. The powder granule mixture is in a Graphitpressform filled with a diameter of 38mm and compacted by means of directly heated hot presses at 50 MPa at 830 ° C and with a holding time of 3 minutes. The relative density achieved is 99.8% of the theoretically calculated density.
  • the blank is shown in FIG. 1, in which case a heat treatment has already been carried out as a test. The blank is transferred by milling in a watch case and polished. Subsequently, a heat treatment at 600 ° C in air, whereby only the titanium areas change color. The watch case is photographed and a binary image is generated, which clearly identifies the watch case due to the special macro structure. This is characterized by the fact that unidirectional application of the pressing force results in different macrostructures in the pressing direction and transversely thereto.
  • Silver powder with a particle size ⁇ 45 ⁇ is mixed with particles of boron carbide (B4C) in an etchant, wherein the proportion of B4C particles at 5 vol. -% is and the particles have a particle size below 10 ⁇ .
  • the composite powder of Ag and B4C is mixed with brass chips (in a ratio of 50:50 vol.%) Which have a size of about -6 mm in length and about 0, 5-lm in width and about. Have depth, the mixture in a mold (diameter 30mm) filled and compacted at 150 MPa.
  • the resulting green compact is placed in a permanently heated mold at 680 ° C and compacted at 120 MPa for 60 seconds. Thereafter, the blank is processed into a ring.
  • Silver powder granules as in Example 1 and gold chips with a length of about 3-5 mm and a thickness / width of about 0.5-2 mm are mixed (in the ratio 55:45 vol .-%) and the mixture is in a graphite form with a Dimension of about 27mm x 40mm filled.
  • the mixture is compressed in a direct hot press at 50 MPa and a temperature of 820 ° C over a period of 5 minutes. This vacuum is used.
  • the resulting blank with a dimension of 40x40x8mm has a relative density of 99.7%. Due to the lower pressing force, the differences in the macrostructure in the pressing direction and across are not so pronounced.
  • the block is milled and subsequently heat treated and transferred in a rolling process over several forming steps, wherein the rolling direction is changed, in a plate with a thickness of 2mm.
  • the density of the plate increases by this process to> 99, 9%.
  • Aluminum powder with a grain size ⁇ 63 ⁇ is converted by addition of a binder in a granulate with a granulate particle size of 3-5mm. Then the granules are mixed with titanium shavings, with a Ratio of aluminum powder to titanium chips of 70:30 vol .-% is used. The mixture is filled into a graphite mold (diameter 30 mm), which is provided with release agent. The compaction takes place in an inductively heated hot press at a temperature of 630 ° C and a pressure of 35 MPa. For the production, a high heating rate of 200 K / min is used and the holding time is 5 minutes. In the final product there are indications of TiAl phases, in particular at the transition zone between the Ti phase and the Al phase.
  • the TiAl phases are in volume with about 5 vo.l .-% before. After production, the material is ground and polished and subsequently surface-modified by glass bead blasting. It turns out that the phases have a different hardness and thus a different surface structure, the colors differ little in color. Only after performing a heat treatment at 550 ° C change the phases, in particular the titanium phase, the color. From the part of a trailer is made.
  • a powder of a titanium alloy (T16AI4V) with a grain size ⁇ 63 ⁇ is converted into a granulate with a granule particle size of 3 -6mm. This is mixed with spheres of glassy carbon with a diameter of 1.5 mm so that the proportion of titanium alloy matrix is 65 vol%.
  • the powder is hot-pressed in a graphite mold with a diameter of 76mm with a height of 8mm. Then rings and pendants are milled out. The rings are subjected to an additional heat treatment under nitrogen at 800 ° C for one hour. This results in a change in the color of the titanium component, with an improvement the surface hardness of more than 25% is accompanied and also increases the wear resistance.
  • ZrC> 2 powder with an 8 mol% Y 2 O 3 stabilization as the first component and ZrÜ 2 with an 8 mol .-% Y 2 O 3 stabilization and an addition of 3 wt .-% C0O 3 as second components are each using Attritor mixed and then transferred by adding binder (2 wt .-%) in two granular materials with a grain size of about 3-5mm. These are mixed and subsequently, at 300 MPa in a steel mold, a 30 mm diameter green compact is produced. After a debinding process at 450 ° C for 1 hour, the green compact is placed in a graphite mold and compacted by inductive hot press at -50 MPa and a temperature of 1350 ° C in less than 15 minutes.
  • a two-color ceramic is present. Due to a reducing environment in the hot pressing by the graphite mold, the component is subsequently oxidized again in air at 1000 ° C at a slow heating rate. This results in a change of colors. After renewed grinding and polishing, the part is fitted with a metal frame and serves as a pendant.
  • Granulated brass powder with a granule size of 4-5mm is mixed with stainless steel 316L powder granules with a granule size of 3-6mm in the ratio 60:40 vol. -% mixed.
  • the granulate mixture is cold pressed in a 39mm x 26mm steel tool at 80 MPa ⁇ and then provided with a release agent.
  • the green part is at 700 ° C and 100 MPa for 2 minutes in a steel mold hot-pressed and then ejected.
  • the component is then cleaned in a blasting process. Due to the low temperature selected, the second component is not sintered and can therefore be removed by blasting.
  • the result is a porous body with a macrostructure, which can be used because of its visual appearance for a jewelry item, such as a key chain or a brooch. Similarly, the 3-dimensional porosity can be highlighted by optical staining. Further fields of application of the body with macroporosity are filter elements in the technical plant sector.
  • Fig. 2 shows a two-phase structure of silver and brass in a ratio of 50:50 vol. -%.
  • Fig. 3 shows a two-phase structure of gold and silver in one. Ratio of 50:50 vol. -%.
  • Fig. Figure 4 shows a section of the macrostructure of a two-phase microstructure serving as an authentication feature for the article made therefrom.
  • the cutout can be converted to a black-and-white image to be better processed in this way, e.g. to be transformed into a binary code.
  • Powder granules as in example 1 are used and mixed with a powder granulate having a composition Cu: Ag of 40:60 vol.% Filled in a mold in the form of layers.
  • the layers of Cu: Ag with 40:60 vol.% Are outdoors and in the center is a layer with 60:40 vol.%.
  • the sandwich structure obtained consists of a 60:40 Cu: Ag 4 mm thick core surrounded by two layers of Cu: Ag of 40:60 vol.% Approximately 1.5 mm thick.
  • Fig. 6 shows a multi-phase material consisting of two layers with different concentrations of the individual phases.
  • Fig. 7 shows a multi-phase material consisting of three layers (sandwich arrangement) with different concentrations.
  • Fig. 8 shows a polyphase material consisting of a gradient structure.
  • Fig. 9 shows a multi-phase material which is pressed directly onto a carrier material.
  • Fig. 10 shows a combination of a multi-phase material with a carrier body.
  • FIG. 11 shows a multiphase material introduced locally into a carrier body.

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Abstract

Matériau à structure polyphasée comportant au moins une première phase solide et au moins une deuxième phase solide, caractérisé en ce que la première phase et la deuxième phase sont chacune un métal, un alliage métallique, un matériau céramique ou des combinaisons de ceux-ci sous forme de matériau composite, les phases de la structure peuvent être différenciées entre elles de manière macroscopique, la structure polyphasée est conçue comme une structure interstitielle ou comme une structure à interpénétration tridimensionnelle, la structure interstitielle comprend la première phase sous forme de phase matricielle présente en continu dans les trois dimensions et la deuxième phase sous forme de phase interstitielle discontinue à répartition statistique, la première phase étant obtenue par frittage.
EP14812120.5A 2013-10-28 2014-10-28 Matériau à structure polyphasée Pending EP3063103A2 (fr)

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ATA829/2013A AT515007B1 (de) 2013-10-28 2013-10-28 Werkstoff mit mehrphasigem Gefüge
PCT/AT2014/000197 WO2015061817A2 (fr) 2013-10-28 2014-10-28 Matériau à structure polyphasée

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WO2019018436A1 (fr) * 2017-07-17 2019-01-24 Desktop Metal, Inc. Fabrication additive à l'aide de débits d'alimentation de matériau de construction variables
CH713998B1 (fr) * 2017-07-18 2021-03-31 Hublot Sa Geneve Composant horloger en matériau composite et procédé de fabrication d'un tel composant.
EP4296796A3 (fr) * 2018-11-16 2024-01-17 The Swatch Group Research and Development Ltd Matériau composite à matrice métallique et procédé de fabrication d'un tel matériau
EP4389319A1 (fr) 2022-12-20 2024-06-26 Manufacture d'Horlogerie Audemars Piguet SA Procédé pour la fabrication d'un composant horloger à base d'alliage d'or et pièce résultante
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WO2015061817A3 (fr) 2015-07-02

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