Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
• • 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
  • B22F5/007—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of moulds
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
  • B22D33/00—Equipment for handling moulds
  • B22D33/04—Bringing together or separating moulds
• • 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
• • 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
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/12—Both compacting and sintering
  • B22F3/14—Both compacting and sintering simultaneously
  • B22F3/15—Hot isostatic pressing
• • 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
  • B22F7/062—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 involving the connection or repairing of preformed parts
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C24/00—Coating starting from inorganic powder
  • C23C24/02—Coating starting from inorganic powder by application of pressure only
  • C23C24/04—Impact or kinetic deposition of particles
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
  • C23C4/06—Metallic material
  • C23C4/08—Metallic material containing only metal elements
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
  • C23C4/126—Detonation spraying
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
  • C23C4/129—Flame spraying
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
  • C23C4/134—Plasma spraying
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/18—After-treatment
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
  • C30B29/10—Inorganic compounds or compositions
  • C30B29/16—Oxides
  • C30B29/20—Aluminium oxides
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
  • C30B35/002—Crucibles or containers
• • 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
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/02—Compacting only
• • 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
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/10—Sintering only

Definitions

• the invention relates to a container comprising at least two interconnected parts, wherein at least a part of refractory metal or a
• Refractory metal alloy with a refractory metal content> 80 Ma% Refractory metal alloy with a refractory metal content> 80 Ma%.
• the invention relates to a method for producing a container which at least partially consists of refractory metal or a refractory metal alloy with a refractory metal content> 80 Ma%.
• Invention summarized the materials of the 5th (vanadium, niobium, tantalum) and 6th group (chromium, molybdenum, tungsten) of the periodic table and rhenium.
• these materials have excellent dimensional stability even at high temperatures and are chemically resistant to many melts.
• containers of these materials are used for the melting of glass, oxide ceramics and metals.
• Refractory metals are made by melting or powder metallurgical
• Joining techniques that do not involve gas uptake for example electron beam melting
• coarsening for example
• Diffusion welding lead are very expensive and / or very limited in terms of possible geometries. Therefore, containers used for the melting of glass, oxide ceramics and metals are manufactured on an industrial scale only by metal forming or powder metallurgy net-shaping processes. However, these methods are liable procedural or economic disadvantages. For example, tungsten and its alloys can not be reshaped into large containers due to the material-inherent brittleness. Also the height to diameter ratio is limited. In the case of containers made by powder metallurgical net-shaping processes, disadvantageous product properties are also to be mentioned. These
• Processes typically involve only powder compaction and sintering, whereby the component density is about 85 to 95%. Because the pores are preferred
• Grain boundaries lie, so containers produced in comparison to melts often inadequate corrosion resistance, since the melt can penetrate along the weakened by the pores grain boundaries to the outside.
• a coated container is known, for example, from WO 2010/072566 A1.
• a crucible which is made of a refractory metal, at least partially with a protective layer of an oxidic material, in the temperature range of 20 ° C to 1 .800 ° C none
• Phase transformation is subject, covered. This provides an additional
• the object of the invention is therefore to provide a container which does not have the disadvantages described above.
• Another object of the invention is to provide a method that inexpensively results in dense, corrosion resistant containers.
• the container can be open or closed, for example by a lid.
• the container comprises at least two parts which are interconnected. At least one part consists of refractory metal or one
• Refractory metal alloy wherein the refractory metal content is> 80% by mass.
• refractory metals refers to the materials of the 5th (vanadium, niobium, tantalum) and 6th group (chromium, molybdenum, tungsten) of the periodic table and rhenium.
• 5th vanadium, niobium, tantalum
• 6th group chromium, molybdenum, tungsten
• Components of the refractory metal alloy are refractory ceramic compounds, such as oxides, which preferably have a melting point of
• Preferred oxides are the oxides of the metals of the group aluminum, titanium, zirconium, hafnium, calcium, magnesium, strontium,
• the preferred refractory metal content is preferably> 90% by mass, in particular
• refractory metals are molybdenum and tungsten. Refractory metals without further alloying components or refractory metal alloys, in which all alloying components are selected from the group of refractory metals, are also preferred.
• Embodiment of the invention So are suitable for melting of
• Aluminum oxide for example for sapphire single crystal pulling process
• molybdenum technically pure tungsten or molybdenum-tungsten alloys.
• the metal is referred to with customary manufacturing impurities.
• the entire container preferably consists of refractory metal or a refractory metal alloy with a refractory metal content> 80 Ma%.
• thermal spray coating can be clearly recognized by a person skilled in the art on the basis of its microstructure. For example, the spray particles deform on impact with the substrate, resulting in the typical "pancake structure" for thermal spray coatings.
• Thermal spraying techniques include molten bath spraying,
• Plasma spraying again differentiates depending on the spray atmosphere, the atmospheric plasma spraying, the plasma spraying under inert gas and the vacuum plasma spraying.
• Spray layer forms an excellent connection with the parts to be joined, which makes it possible to produce containers which are the inventive
• the container according to the invention may have a variety of shapes (for example, in terms of diameter (round container), length / width (in rectangular container) and height, which is not feasible with crucibles according to the prior art.
• the binding zone spray layer / part is formed as cohesive and / or positive connection.
• connection partners are held together by atomic or molecular forces.
• the spray droplets have a temperature which is above the particular solidus temperature.
• the substrate is usually heated.
• a positive connection is understood to be a connection that results from the intermeshing of at least two connection partners. If, for example, the parts to be joined have roughness, the recesses are filled with the spray material during thermal spraying. This creates a gearing effect and thus a positive connection. A person skilled in the art can also unambiguously distinguish a positive connection from other connection techniques.
• the compound is cohesively or
• the sprayed layer is preferably formed as a seam.
• the seam is preferably formed from many spray layers.
• the spray seam is preferably designed as a U, V, Y or I seam.
• a fillet weld is also a preferred embodiment.
• Particularly preferred seam shapes are the U and V seams.
• the opening angle of the V or U-seam can be chosen within a wide range, whereby also angles that extend beyond the usual range of welds, can be selected.
• a preferred range is 45 ° to 230 °. Such large angles can not be achieved with conventional welding.
• the V includes the area of the parts to be joined.
• For larger thicknesses of the parts to be joined can also be a double-V seam (X-seam) or a
• Double U-seam to be particularly advantageous.
• fillet welds are suitable for a secure connection of two or more parts.
• other embodiments such as, for example, a connection by means of a spray applied in two dimensions, are possible and advantageous.
• the parts to be joined are fixed to each other by a positive connection or connected to each other before applying the spray coating.
• the parts are at least partially formed so that this allows a positive connection.
• Feather connection as well as the pinning call.
• Advantageous non-positive connections are press, shrink and wedge joints. By caulking both a positive and non-positive connection is achieved.
• the refractory metal is molybdenum or tungsten.
• Advantageous molybdenum or tungsten alloys are Mo-W alloys in the entire concentration range and molybdenum or
• Tungsten-based alloys having a molybdenum or tungsten content of> 80% by mass, advantageously> 90% by mass, in particular advantageously> 95% by mass, the remainder being advantageously a high-melting oxide.
• the oxide lies in
• Mo-0.01 to 20% by mass of mixed oxide which is at least 50 mol% of an oxide selected from the group consisting of HfO 2 , ZrO 2 , TiO 2 , Al 2 O 3 , Y 2 O 3 , Sc 2 O 3 , rare earth metal oxide, SrO, CaO and MgO.
• W-0.01 to 20 Ma% of at least one oxide selected from the group consisting of HfO 2 , ZrO 2 , TiO 2 , Al 2 O 3 , Y 2 O 3 , Sc 2 O 3 , rare earth metal oxide, SrO, CaO and MgO ,
• compound oxide containing at least 50 mol% of an oxide selected from the group consisting of HfO 2, ZrO 2, TiO 2, Al 2 O 3, Y 2 O 3, Sc 2 O 3, Rare earth metal oxide, SrO, CaO and MgO.
• Mo-W alloy (0.5 Ma% ⁇ W ⁇ 99.5 Ma%) - 0.01 to 20 Ma% of at least one oxide selected from the group consisting of HfO 2 , ZrO 2 , TiO 2 , Al 2 O 3 , Y 2 O 3 , Sc 2 O 3 , rare earth metal oxide, SrO, CaO and MgO.
• the sprayed layer is formed by plasma spraying.
• plasma spraying the coating material is melted by the high plasma temperature.
• the plasma stream travels with the particles and hurls them at the parts to be connected. Due to the high temperature of the particles when hitting the parts to be joined, it is ensured that a cohesive connection reliably forms between the sprayed layer and the parts to be joined.
• the parts to be joined before the Applying the spray coating, the parts to be joined to a temperature> 500 ° C, preferably> 1000 ° C, more preferably> 1500 ° C warmed.
• the advantageous range is limited at the top by the melting point of the parts to be joined.
• the plasma spraying is preferably carried out in a protective gas atmosphere (eg argon) or in a vacuum.
• a protective gas atmosphere eg argon
• Coating process is ensured in a vacuum, that in the area of the interface layer / part no oxide layer or oxide areas can be formed, which affects both the bond strength, and on the
• Grain boundary corrosion resistance adversely affects / impact.
• Preferred materials for the spray coating are shown in the following table.
• an oxide selected from the group consisting of HfO 2 , ZrO 2 , TiO 2 , Al 2 O 3 , Y 2 O 3 , Sc 2 O 3 , Rare earth metal oxide, SrO, CaO and MgO.
• Mo-W alloy (0.5 Ma% ⁇ Mo ⁇ 99.5 Ma%) - 0.01 to 20 Ma%
• Mo-Ta alloy with 0.1 Ma% ⁇ Ta ⁇ 99 Ma%
• a further preferred embodiment of the invention is when both the sprayed layer and the parts to be joined are formed from refractory metal or a refractory metal alloy. It is particularly advantageous if
• Spray layer and parts to be joined consist of the same material or in the case of an alloy have at least the same base material.
• the container is advantageous as a round container, e.g. as a crucible, formed.
• the round container is formed by at least two parts, which are formed as hollow cylinder segments, and at least one bottom part.
• the rectangular container is formed by at least two side parts and at least one U-shaped or plate-shaped bottom part. Rectangular containers can be produced according to the prior art only by Netshape-Press / sintering process. Forming technology, for example by deep drawing, a production of larger rectangular containers is not possible.
• the high density of the container is achieved by making the parts to be joined (e.g., hollow cylinder and bottom part) of deformed material.
• the parts to be joined e.g., hollow cylinder and bottom part
• the sprayed layer of the container is sealed against a ceramic melt (for example Al 2 O 3). Material damage, such as grain boundary contamination, pores at grain boundaries and
• Grain boundary cracks can greatly reduce the tightness of a melt container. It is therefore very surprising for a person skilled in the art that a sprayed coating, which usually also has material effects, is also tight over an A Oa melt for very long times. Unlike pressed and sintered parts (pores are mainly at the grain boundaries), pores in the spray layer, which are largely in isolated form, affect the seal to a lesser extent.
• the spray layer can advantageously not only serve as a connecting element between the parts, but also, applied in a flat form, improve the tightness of the parts. This is particularly advantageous in only pressed / sintered parts. The spray layer can easily before the
• Connection process can be applied. This makes it possible in a simple manner to produce containers which are provided inside and / or outside at least partially with a thermal spray coating.
• the relative density (measured density based on theoretical density) of the spray layer in the region of the connection zone and / or the spray applied over the surface is preferably> 95%. Excellent results can be obtained if the relative density is> 98%, particularly advantageously> 99%.
• Ceramic melt may be the case.
• the objective task is also supported by a procedure for
• the container consists at least partially of refractory metal or a refractory metal alloy, wherein the refractory metal content is> 80 Ma%.
• the process comprises at least the following steps:
• At least regional application of a thermal spray coating so that the spray layer at least partially forms at least one compound selected from the group consisting of material bond and positive connection between at least two parts.
• the production of the parts is advantageously carried out by conventional powder metallurgy and / or forming techniques.
• the parts can be produced by pressing, sintering and subsequent forming, for example rolling. Further forming steps advantageously include bending or stamping.
• the preparation by hot isostatic pressing (HIPen), optionally followed by a forming process, is a preferred method.
• the application of the thermal spray layer is preferably carried out by
• the container has at least one of the following
• the sprayed layer is formed as a seam.
• the seam has a U, V, Y or I shape or is a fillet weld
• the parts to be joined are at least partially formed so that they are fixed to each other by a form or material connection or connected to each other.
• the refractory metal is molybdenum or tungsten.
• the sprayed layer is formed by plasma spraying.
• the sprayed layer and the connecting parts are made of refractory metal or a refractory metal alloy.
• the container is designed as a round container.
• the round container is characterized by at least two parts, as
• Hollow cylinder segments are formed, and formed at least one bottom part.
• the container is designed as a rectangular container.
• the rectangular container is formed by at least two side parts and at least one U-shaped or plate-shaped bottom part.
• the sprayed layer is tight against a ceramic melt.
• the parts to be joined are mechanically processed before the application of the spray coating so that they are at least partially fixed in shape, force and / or material fit to each other or connected to each other can be.
• Particularly advantageous connections are the tongue and groove, pin, press and shrink connection.
• the parts are advantageously preferably processed mechanically so that the joining of the parts by a thermally sprayed seam is possible.
• a particularly advantageous thermal spraying method is the plasma spraying, and here again to call the vacuum plasma spraying.
• the material for the sprayed layer is advantageously introduced radially as a powder into a plasma jet generated by a DC arc discharge, melted in the plasma jet, and the molten droplets are deposited on a base body. Since the process is carried out under reduced pressure, oxidation of the coating material is avoided.
• a particularly advantageous method is the inductive vacuum plasma spraying (IVPS).
• IVPS inductive vacuum plasma spraying
• An essential difference compared to conventional plasma spraying is that the plasma is generated by inductive heating, whereby the
• Spray powder in a simple manner can be introduced axially before the formation of the plasma jet.
• the powder particles linger much longer in the plasma jet.
• the energy transfer from the plasma to the individual particles of the spray powder improves, so that even larger particles are heated completely above their melting temperature and can be deposited as fully molten droplets.
• the resulting in inductive plasma spraying structure has in comparison to conventionally produced plasma sprayed layers on a still further improved density (relative density preferably> 98%) over even very thin liquid ceramic melts. Even the low
• Beam diameter has a favorable effect on the coating process.
• a further improvement of the cohesive connection can be achieved if the parts to be joined are preheated with the plasma jet, for example to a temperature greater than 700 ° C. (for example 700 to 2000 ° C.). If a procedure is used which results in a low density junction zone, the junction zone may be sealed by the action of a slurry, optionally followed by annealing.
• the powder particles of the slurry are advantageously also made of a refractory metal or a
• Refractory metal alloy wherein advantageously the mean particle size (measured by laser diffraction) ⁇ 1 ⁇ .
• inventive container for melting alumina by conventional methods, such as the Kyropoulos, HEM, EFG, CHES, Bagdasarov or Czochralski process.
• the invention will now be described by way of example.
• Figure 1 to 17 represent embodiments of the invention.
• FIG. 1 shows, in an exploded view, the parts of a schematic diagram
• Figure 2 shows schematically a round container, constructed from the parts
• Figure 3 shows schematically a rectangular container in the material fit
• Figure 4 shows schematically a rectangular container in the material fit
• FIG. 5 shows a photograph of a rectangularly connected rectangular container
• Mo is used in the examples of technical grade Mo.
• Figure 6 shows schematically two parts, materially connected by a V-seam.
• Figure 7 shows schematically two parts, cohesively by a U-seam
• Figure 8 shows schematically two parts, positively to each other by a
• Figure 9 shows schematically two parts, positively and non-positively fixed to each other by caulking and materially connected by a U-seam, and a sprayed layer to the inside and a sprayed layer to the outside sealing.
• Figure 10 shows schematically two parts, positively to each other
• Figure 1 1 shows schematically two mutually positively by a tongue and groove connection fixed parts, an externally applied sprayed layer for cohesive connection and sealing and an internally mounted sprayed layer for sealing.
• FIG. 12 schematically shows two parts which are positively fixed relative to one another by a tongue and groove connection and are connected in a materially bonded manner by a U-seam.
• FIG. 13 shows schematically two parts which are positively fixed by a tongue and groove connection and a sprayed layer for sealing and one
• Figure 14 shows schematically two mutually positive and non-positive by
• FIG. 15 shows a scanning electron micrograph of the joining zone
• FIG. 16 shows a light micrograph of a sprayed (IVPS)
• Spray chamber mounted.
• For the injection process was a commercial product that was used for the injection process.
• the IVPS injection process was carried out using parameters customary for refractory metals (see, for example, EP 0 874 385 A1). After the injection process, the rectangular container () was removed from the vacuum chamber and the faces were machined by means of machining (milling, grinding). A photograph of the rectangular container (1) is shown in FIG.
• Sapphire single crystals the usual melt temperature is about 2150 ° C, the smelting process was carried out at 2300 ° C to simulate more severe conditions. The trial period was 24 h. Thereafter, the round container (1) was examined by metallography. There was no penetration of alumina in the area of the cohesive connection (see FIG. 15).
• Two hollow cylinder segments (2a, b) the hollow cylinder segments (2a, b)
• Bottom plate (2c) The bottom plate (2c) was made of a sintered
• the blank (2c) was provided on one side (bottom inside of the finished container (1)) by means of IVPS with a W-layer (4b). The layer thickness was about 300 pm.
• IVPS injection process
• the IVPS injection process was carried out using parameters customary for refractory metals (see, for example, EP 0 874 385 A1).
• the bottom plate (2c) was connected to the joints to be joined by
• Contour milling provided with a profile (5c) and with a recess for a U-seam (3a) corresponding to Figure 9.
• the parts (2a, b, c) were then fixed to each other by caulking in the area (5b) positive and non-locking and interconnected (see Figures 9 and 14).
• the cohesive joining of the parts (2a, b, c) took place via a thermally sprayed U-seam (3a) made of W, which was produced by IVPS.
• Round container (1) removed from the vacuum chamber and machined the end faces by means of machining (milling, grinding). The outside of the bottom was also provided with an approximately 300 pm thick W layer (4a). Subsequently, in this round container (1) alumina according to
• Example 1 melted. The metallographic examination showed no penetration of alumina in the area of the cohesive connection.
• Fig. 16 shows that the W layer (4a) has fewer pores than the W sintered plate (2c).
• Part (2f) which forms the bottom and side surfaces longitudinally: This part (2f) was made from a U-shaped forged Mo-1 Ma% Zr0 2 plate
• Parts (2d, e) that make the side surfaces wide The parts (2d, e) were made from a rolled Mo plate Mo-1 Ma% Zr0 2 that had been machined and ground on all sides. The wall thickness was 8 mm. The
• Parts (2d, e) were provided on the joints to be joined by means of contour milling with a profile (5b) and with a recess for a U-seam (3a) according to FIG.
• Two hollow cylinder segments (2a, b) the hollow cylinder segments (2a, b)
• Bottom plate (2c) The bottom plate (2c) was rolled out
• the parts (2a, b, c) were then fixed positively to one another via the tongue and groove connection (5b).
• the cohesive joining of the parts (2a, b, c) took place via a thermally sprayed Mo U seam (3a), which was produced by IVPS.
• the production of the layer (3a) was carried out according to Example 1. After the injection process, the round container (1) was removed from the vacuum chamber and machined the end faces by means of machining (milling, grinding).
• a ring of Inconel 718 having the composition 0.04 Ma% C; 19% by mass; 3.0% Mo; 52.5% by mass Ni; 0.9 Ma% AI; ⁇ 0.1 Ma% Cu; 5.1 Ma% Nb; 0.9 Ma% Ti and 19 Ma% Fe were combined with a bottom plate (2c) of Mo.
• the cohesive connection was realized via a sprayed V-seam (3b) (see FIG. 6).
• the material used for the spray was Mo. Even with alien (Ni-base superalloy and refractory metal) materials could a
• Round container (1) are produced with a tight, cohesive connection.
• FIG. 7 Bonded connection by means of a U-seam (3a), application of an outside sealing layer (4a)
• FIG. 8 Positive fixing by pinning (FIG. 5a), integral connection by a U-seam (FIG. 3a), application of an outside
• Figure 1 positive locking by a tongue and groove connection (5b), cohesive bonding by a surface applied layer (3c), applying an outside (4a) and inside (4b) sealing layer
• FIG. 12 positive fixing by a tongue and groove connection (5b), material connection by a U-seam (3a)
• FIG. 13 positive fixing by a tongue-and-groove connection (5b), application of a sealing layer (4a, b), integral connection by a monolithic applied Mo-spray layer (3c)

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