US20180318931A1 - Use of a deformable interface for the fabrication of complex parts - Google Patents

Use of a deformable interface for the fabrication of complex parts Download PDF

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US20180318931A1
US20180318931A1 US15/773,791 US201615773791A US2018318931A1 US 20180318931 A1 US20180318931 A1 US 20180318931A1 US 201615773791 A US201615773791 A US 201615773791A US 2018318931 A1 US2018318931 A1 US 2018318931A1
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counter
volume
densification
assembly
densified
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Claude Estournes
Charles Maniere
Lise Durand
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Universite Toulouse Iii -- Paul Sabatier
Centre National de la Recherche Scientifique CNRS
Universite Toulouse III Paul Sabatier
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Universite Toulouse Iii -- Paul Sabatier
Centre National de la Recherche Scientifique CNRS
Universite Toulouse III Paul Sabatier
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    • 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
    • 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
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • 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
    • B22F5/003—Articles made for being fractured or separated into parts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00—Moulds or cores; Details thereof or accessories therefor
    • B29C33/0011—Moulds or cores; Details thereof or accessories therefor thin-walled moulds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00—Moulds or cores; Details thereof or accessories therefor
    • B29C33/0011—Moulds or cores; Details thereof or accessories therefor thin-walled moulds
    • B29C33/0016—Lost moulds, e.g. staying on the moulded object
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006—Pressing and sintering powders, granules or fibres
    • 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
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C—CHEMISTRY; METALLURGY
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    • 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
    • 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
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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
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63424—Polyacrylates; Polymethacrylates
    • 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
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/05—Light metals
    • B22F2301/052—Aluminium
    • 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
    • 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
    • B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94—Products characterised by their shape
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94—Products characterised by their shape
    • C04B2235/945—Products containing grooves, cuts, recesses or protusions

Definitions

  • the field of the invention is that of the fabrication of mechanical parts of complex shapes by the densification of powdery or porous materials.
  • the invention relates to the improvement of an assembly of powdery or porous materials adapted to being densified under load both in its use and the technical characteristics of the complex mechanical parts obtained.
  • SPS especially is a known way of subjecting a cylindrical volume of compressed powder to a pulsed current enabling a significant increase in the kinetics of densification of these powders and thus making it possible to obtain mechanical parts of which the fine microstructures are preserved.
  • the modes of densification used by SPS however have the drawback of causing inhomogeneities of densification when complex-shaped parts shapes have major differences in thickness.
  • a cylindrical T-shape possesses, at the end of sintering, a porous zone with a relative density of the order of 70%.
  • FIGS. 1 to 3 The initial assembling geometry of the SPS technique as well as the densification field and the end-of-cycle vertical displacement field are illustrated by FIGS. 1 to 3 .
  • the simulation consists of a purely mechanical model, with a temperature cycle, imposed on the entire geometry.
  • the boundary conditions are constituted by a fixed displacement, along the z axis of the cylinder of the lower piston.
  • a compression force is applied to the top face of a cylindrical volume of alumina powder.
  • the lateral conditions are no-penetration conditions.
  • the thermal cycle is defined according to a temperature ramp of 100 K/minute up to 1400° C. followed by a five-minute dwell time. The force applied is 18000 N.
  • the low thickness zone is dense, and the high thickness zone is porous with a relative density of the order of 80% ( FIG. 2 ).
  • the vertical displacement field ( FIG. 3 ) is expressed by highly curved iso-displacement lines that contrast with the lines of a frictionless cylindrical sample, where the iso-displacement lines are horizontal. This result can be explained by the non-uniformity of the shrinkage observed between the two zones of different thicknesses.
  • the low thickness zone gets densified more rapidly because, for equal displacements, its distance of maximum shrinkage is attained more rapidly than within the high thickness zone.
  • the proposed technique does not have these drawbacks of the prior art. More particularly, in at least one embodiment, the proposed technique refers an assembly for densification under load along at least one direction of compression, comprising:
  • method of densification under load is understood to mean any process of sintering under load or creep effect seeking to consolidate a defined volume of metal powder, ceramics, polymers, by heating of this powder and the application of a unixial, multiaxial or isostatic pressure.
  • These methods include especially forging, hot pressing, hot isostatic pressing, SPS or any other known method following this same general principle of operation.
  • the invention therefore relates to assembling adapted to the implementation of such methods of densification under load, and having specific technical characteristics (melting point, thermal capacity, activation energy etc.) enabling it to withstand major thermal stresses (for example sudden temperature increases of the order of thousands of degrees) and mechanical stresses (compression of the order of about tens of thousands of Newtons).
  • volume to be densified designates a volume of powders and/or porous materials that are to form a mechanical part following the use of the densification method. This gives an equivalent designation, “part to be formed”, used in the present description.
  • a volume has a complex shape, and this is structurally expressed by variations in thickness of continuous segments of the volume to be densified, in the context of a projection along the direction of compression. It is necessary to distinguish the thickness of a shape and its height, this height possibly designating discontinuous segments of a volume along this same projection.
  • a volume with the shape of a dual cone generated by revolution when considered along its axis of revolution, has a constant height but a variable thickness.
  • a surface portion of the volume to be densified i.e. all or part of its external surface, has a complementarity of shape with at least one face of a counter-form.
  • the assembly can also include a plurality of counter-forms.
  • An interface layer for its part, acts as a separation between this portion of the part to be formed and the counter-form.
  • the deformable character of the interface layer is expressed by a thickness, a chemical reactivity and a capacity of compaction that are negligible as compared with those of materials forming part of the respective compositions of the volume to be densified and of the counter-form.
  • this interface layer will thus get deformed and follow the shrinkage of the volume to be densified until the forming of a counter-form of the concerned portion of the part to be fabricated, once the process of densification is completed.
  • the shifting of the interface layer enables the homogenous distribution, on the complex part to be formed, of all the stresses transmitted by the counter-form and the tooling using for the densification under load (piston-die).
  • the complex part obtained therefore has a scaling of shrinkage on its entire surface (portion) in contact with the interface layer.
  • the flaws and fractures that can be generated within the counter-form during the densification process and/or a subsequent step of fracturing are entirely or partly blocked by the deformable interface layer and therefore do not spread in the part to be formed, of which the surface appearance and more generally the microstructure are preserved.
  • such an assembly enables the simultaneous fabrication of one or more parts of complex shapes in the context of a method of densification under load, the compressive directions of which are limited (for example uniaxial compression).
  • the present invention thus relies on a novel and inventive concept of providing an assembly for densification under load of complex shapes, implementing a deformable interface layer, enabling the simultaneous fabrication of one or more complex-shaped parts, said parts having a scaling of densification as well as a preserved microstructure.
  • Such an assembly provides especially the advantage of being capable of implementation in the context of a method of densification under load having low complexity.
  • the variations of thicknesses are continuous.
  • the application of the invention therefore enables a scaling of densification as well as a microstructure that is kept for complex volumes having constant variations of thickness, for example spherical or pyramid-shaped volumes.
  • said counter-form and said volume to be densified are of distinct shapes.
  • the counter-form includes the volume in its totality.
  • Such a configuration thus enables the fabrication of parts, the entire rim of which has a scaling of densification.
  • the counter-form includes only one part of the volume to be densified.
  • the speed of densification of the material constituting said volume is greater than or equal to the speed of densification of the material constituting said counter-form.
  • Such a variation and speed of densification can be due to the differences in chemical composition existing between two materials, for example between alumina and zirconia, or differences in microstructure, for example between two materials of a same chemical composition but of different grain sizes.
  • the volume to be densified and the counter-form have a chemical composition and a microstructure that are identical.
  • the implementing of materials of a same chemical composition and the same microstructure for the part to be formed and the counter-form or forms has the advantage of facilitating the forecasting of shrinkages of material generated during the step of densification.
  • the volumes to be densified and the counter-form have a conical composition and/or microstructure that are different.
  • said portion and said face are separated by a plurality of consecutive deformable interface layers.
  • the assembly comprises a plurality of complex-shaped volumes to be densified, and at least one counter-form, all having a powdery and/or porous composition, said counter-form has at least one face facing at least one portion of each of said volumes, and said faces and each of said portions are separated by at least one deformable interface layer.
  • the volume to be densified undergoes deformation between an initial geometrical shape and a distinct final geometrical shape.
  • This deformation results from stresses exerted by the counter-form on the complex-shaped rim of the volume to be densified. It must be noted that such a geometrical deformation does not come into play in the context of densification of a simple shape, this shape preserving the same geometrical shape throughout the densification (despite of course a reduction of its thickness).
  • the final height at any desired point (h f ) of the part to be formed responds to the following relationship:
  • h i represents the height of stretching at any point and d i and d f represent the initial and final relative densities of the part to be formed.
  • the said step of incorporation is implemented by powdery deposition of said interface layers on the zones of said counter-form(s) placed so as to be facing the part to be formed but also between the counter-forms if necessary.
  • said step of incorporation is implemented by the insertion, within said assembly, of one or more solid interface layers preferably a flexible graphite foil (for example Papyex)° prior to a step for filling said assembly with materials respectively constituting the part to be formed and said counter-form or counter-forms.
  • a flexible graphite foil for example Papyex
  • the method of fabrication comprises a step for the extraction of said part from said assembly by the sacrificial destruction of said counter-form or counter-forms and/or said deformable interface layers.
  • FIG. 1 is a schematic view of an initial assembly for SPS of the prior art implementing a cylindrical part having a step
  • FIG. 2 is a simulation illustrating the relative density field at the end of sintering of a cylindrical part possessing a step
  • FIG. 3 is a simulation illustrating the vertical displacement field at the end of sintering of a cylindrical part possessing a step
  • FIG. 4 is a schematic view of the successive steps of the forming of an assembly according to one particular embodiment of the invention.
  • FIG. 5 is a series of photographs illustrating the step of extraction of a mechanical part following the densification, under load, of an assembly according to one particular embodiment of the invention
  • FIG. 6 is a series of photographs illustrating the imprint used for the generation of the initial shape of the part to be formed and the formed part after densification of an assembly according to one particular embodiment of the invention
  • FIG. 7 is a schematic view of the successive steps for forming an assembly according to one alternative embodiment of the invention.
  • FIG. 8 is a photograph illustrating a conical part as well as fragments of the counter-form obtained following the densification under load of an assembly according to one particular embodiment of the invention.
  • FIG. 9 is a photograph illustrating a part with a square-based pyramid shape as well as fragments of the counter-form obtained following the densification under load of an assembly according to one particular embodiment of the invention.
  • FIG. 10 is a photograph illustrating a part with a star-based pyramid shape obtained following densification under load of an assembly according to one particular embodiment of the invention.
  • FIG. 11 is a photograph illustrating two fragments of the counter-form obtained following the densification under load of an assembly according to one particular embodiment of the invention.
  • FIG. 12 is an image made by a scanning electron microscope (SEM) of the microstructure of a fracture present on a sacrificial part of a pyramid following the densification under load of an assembly according to one particular embodiment of the invention
  • FIG. 13 is a photograph illustrating a cone of zirconia with a density at 99% and a part of the counter-form (alumina density at 98%) obtained following densification under load of an assembly according to one particular embodiment of the invention
  • FIG. 14 is an SEM image of the microstructure of a fracture deliberately provoked at the center of a cone made of zirconia following the densification under load of an assembly according to one particular embodiment of the invention
  • FIG. 15 is an SEM image of the microstructure of a fracture deliberately provoked at the edge of the fine zones of a cone made of zirconia following the densification under load of an assembly according to one particular embodiment of the invention.
  • the invention relates to the fabrication 1 of complex parts 3 that can have a great diversity of shape with the possible adapting of the method of fabrication 1 to the degree of complexity of these shapes.
  • the complexity of shape results from variations in the thicknesses of this shape along the direction of compression. This complexity increases for parts having:
  • the step of densification 2 is not limited to SPS but also relates to forging, hot pressing, isostatic hot pressing or any other known method of consolidation and creep effect for powdery and/or porous materials.
  • FIG. 4 illustrates the subsequent steps of a method of fabrication 1 aimed densifying an assembly by implementing an SPS method 2 in order to obtain a semi-sphere 3 made of poly methyl methacrylate (PMMA).
  • PMMA poly methyl methacrylate
  • the approach adopted by the inventors consists in placing, in a cylindrical mold 8 , a half-ellipsoid 5 of PM MA powder and a porous sacrificial counter-form 6 integrating a face 7 facing the half-ellipsoid, with a deformable interface layer 9 enabling the demolding of the obtained part 3 and of the sacrificial counter-form 6 after sintering.
  • the PMMA powder that goes into the composition of the part to be formed 5 can be replaced by alumina powder, zirconia powder or any other known powdery and/or porous composition.
  • the counter-form 6 can be constituted by any type of known powdery and/or porous material, having preferably a densification curve close to that of the material constituting the part to be formed 5 and preferably the pair formed is formed by two materials of a same class (for example: metal/metal or ceramic/ceramic or polymer/polymer).
  • the half-ellipsoid shape has been chosen because it is the stretched form of the desired semi-sphere.
  • the stretching height at any point (h i ) is related to the relative initial and final densities of the part (d i , d f ) and the final height at any desired point (h f ) by the following formula:
  • the Multiphysics COMPSOL® simulation is used to simulate the distances of shrinkage and deformation induced on a given volume following the implementation of a method of densification.
  • the following publications G. Molisset, L. Durand, J. Galy, A. Couret, “Temperature Control in Spark Plasma Sintering: An FEM Approach” in Journal of Metallurgy. 2010 (2010); A. Pavia, L. Durand, F. Ajustron, V. Bley, A. Peigney, C. Estournès, “Electro-thermal measurements and finite element method simulations of a spark plasma sintering device”, in Journal of Materials Processing Technology, 213(8), (2013), 1327-1336, and T. Voisin, L.
  • the PMMA powder is introduced into a graphite mold 8 .
  • one or more binders such as water, RhodoviolTM can be incorporated into the powdery mixture in order to improve its technical characteristics.
  • an imprint is formed (step 10 a ) on the powder bed by means of a half-ellipsoid counter-form obtained by 3D printing.
  • the counter-form can also be formed via a method of machining.
  • a layer 9 of boron nitrite powder (a powder that is inert under sintering) is then deposited (step 10 b ) in the form of spray on the surface of the imprint.
  • this boron nitride powder can be replaced by graphite powder or any other material that is inert in consolidation and chemically non-reactive with the material constituting the part to be formed 5 .
  • the internal cavity is then filled with PMMA powder (step 10 c ) thus forming the volume 5 intended to shape the desired part 3 .
  • the unit enclosed by two graphite pistons is placed in an SPS device for the sintering step 2 .
  • the interface layer 9 of boron nitride will get thus deformed and follow the half-ellipsoid that will get crushed as and when the sintering takes place until the formation of a semi-sphere 3 once the material is densified.
  • the deformation of the interface layer 9 along the lower portion 5 ′ of the half-ellipsoid 5 enables the homogenous distribution therein of all the stresses transmitted by counter-form 6 .
  • the semi-sphere 3 obtained therefore has a scaling of shrinkage on the entire surface 5 ′ in contact with the deformed interface layer 9 .
  • the final step is the extraction 11 of the semi-spherical part 3 from the sacrificial counter-form 6 achieved by fracturing of the sacrificial counter-form 6 and the interface layer 9 . It has been observed that, following this step of extraction 11 , the cracks stop appreciably at the level of the interface layer 9 of boron nitride, thus preserving the semi-spherical part 3 which remains intact.
  • FIG. 5 presents a series of photographs illustrating the step of extraction of the part 3 from the assembly and especially the interface layer 9 .
  • FIG. 6 for its part illustrates the change in shape induced in the interface layer 9 following the use of the SPS step 2 .
  • a cone, a square-based pyramid and a star-based pyramid are sintered from an aluminum powder using a graphite foil ((papyex®) as an interface layer 9 .
  • the step 10 for placing the assembly consists in giving the desired shape of the interface layer 9 to the papyex by folding and then positioning (step 10 ′ a ) the papyex 9 within the assembly, before filling the zones corresponding to the parts to be formed 5 (step 10 ′ c ) and to the counter-form 6 (step 10 ′ b ) with a powdery and/or porous material.
  • FIGS. 8 to 11 are photographs illustrating the cone-shaped and pyramid-shaped parts 3 as well as the counter-form fragments obtained following the densification under load of an assembly according to these particular embodiments of the invention. As indicated in these photographs, the respective densities of the parts obtained range from 97% to 99%. It is observed that the two pyramid shapes both have well-defined straight ridges. This result is clearly difficult to achieve by known methods of casting in molds without machining.
  • FIG. 12 is an image made through a scanning electron microscope (SEM) of the microstructure of a fracture presented on a sacrificial part of the pyramid. This image especially reflects the low porosity and the satisfactory ductility of the interface layer 9 .
  • SEM scanning electron microscope
  • the respective chemical compositions of the volume 5 intended to form the part and the counter-form 6 are different.
  • the use of materials of a same nature has the advantage of facilitating the planning of shrinkages of material generated during the densification step
  • the use of materials of different natures for its part broadens the possibilities offered to the designer in the choice of materials entering into the composition of the part to be formed 5 or the composition of the counter-form 6 . It is thus possible, for the constitution of the part to be formed 5 , to use a material having advanced technical properties while at the same time selecting a low-cost material for the constitution of the sacrificial counter-form 6 .
  • a conical volume 5 is composed of zirconia powder (ZrO 2 ) when the counter-form 6 is composed of alumina powder.
  • ZrO 2 zirconia powder
  • the coupling of these two powders is based on their behavior under sintering (temperature and densification curve) which are relatively similar.
  • the zirconia powder forming the conical volume 5 thus gets densified slightly more rapidly than the alumina powder forming the counter-form 6 and thus makes it possible to obtain a totally densified part.
  • FIG. 13 is a photograph illustrating a cone of zirconia with density at 99% and a fragment of alumina with density at 98% obtained following the implementing of SPS sintering.
  • FIGS. 14 and 15 are the SEM images of the fracture obtained at the center and edges of the zirconia cone 3 . These SEM images are used especially to observe the fact that the microstructure at the center and at the edge of the cone 3 is homogenous and shows an average grain size of 200 nanometers.

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US15/773,791 2015-11-04 2016-11-04 Use of a deformable interface for the fabrication of complex parts Abandoned US20180318931A1 (en)

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FR1560564A FR3042992B1 (fr) 2015-11-04 2015-11-04 Mise en œuvre d'une interface mobile pour la fabrication de pieces complexes
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PCT/EP2016/076657 WO2017077028A1 (fr) 2015-11-04 2016-11-04 Mise en oeuvre d'une interface déformable pour la fabrication de pièces complexes

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Cited By (2)

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US20180304362A1 (en) * 2017-04-21 2018-10-25 Mikro Systems, Inc. Systems, devices and methods for spark plasma sintering
WO2019191299A1 (en) * 2018-03-27 2019-10-03 San Diego State University In situ partially degradable separation interface for fabrication of complex near net shape objects by pressure assisted sintering

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FR3071178B1 (fr) * 2017-09-15 2022-02-25 Safran Procede de fabrication d'une piece de turbomachine par fabrication additive et frittage flash
FR3086566B1 (fr) 2018-10-02 2022-05-27 Norimat Procede de fabrication de piece de forme complexe par frittage sous pression a partir d'une preforme
FR3086567B1 (fr) 2018-10-02 2022-07-22 Norimat Procede de realisation de contreforme et procede de fabrication de piece de forme complexe utilisant une telle contre-forme
FR3088017B1 (fr) 2018-11-02 2020-11-13 Univ Paul Sabatier Toulouse 3 Procede de fabrication d’une piece par densification sous charge
FR3088016B1 (fr) 2018-11-02 2021-01-29 Univ Paul Sabatier Toulouse 3 Procede de fabrication d’une piece par densification sous charge
FR3137598A1 (fr) * 2022-07-08 2024-01-12 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procédé de fabrication d’une pièce de forme complexe et d’une contre-forme densifiable utile pour la préparation de ladite pièce

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US4673549A (en) * 1986-03-06 1987-06-16 Gunes Ecer Method for preparing fully dense, near-net-shaped objects by powder metallurgy
JPH0531830A (ja) * 1991-08-02 1993-02-09 Mitsubishi Materials Corp ラバープレスによる球体の成形方法
JP3421479B2 (ja) * 1995-08-09 2003-06-30 株式会社日本製鋼所 傾斜機能材料の製造方法
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EP2314401A1 (en) 2009-09-09 2011-04-27 DePuy Products, Inc. Mould design and powder moulding process
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KR101476887B1 (ko) * 2012-09-14 2014-12-26 주식회사 쎄타텍 분말사출성형방법 및 이에 따른 분말사출성형품
FR3008644B1 (fr) * 2013-07-16 2015-07-17 Commissariat Energie Atomique Procede de fabrication par frittage d'une piece multicouche

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180304362A1 (en) * 2017-04-21 2018-10-25 Mikro Systems, Inc. Systems, devices and methods for spark plasma sintering
US11229950B2 (en) * 2017-04-21 2022-01-25 Raytheon Technologies Corporation Systems, devices and methods for spark plasma sintering
WO2019191299A1 (en) * 2018-03-27 2019-10-03 San Diego State University In situ partially degradable separation interface for fabrication of complex near net shape objects by pressure assisted sintering
US20210016499A1 (en) * 2018-03-27 2021-01-21 UNITED STATES OF AMERICA has certain rights in the invention from DOE Grant No. DE-SC0008581 In situ partially degradable separation interface for fabrication of complex near net shape objects by pressure assisted sintering
US11926091B2 (en) * 2018-03-27 2024-03-12 UNITED STATES OF AMERICA has certain rights in the invention from DOE Grant No. DE-SC0008581 In situ partially degradable separation interface for fabrication of complex near net shape objects by pressure assisted sintering

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CA3003545A1 (fr) 2017-05-11
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WO2017077028A1 (fr) 2017-05-11
EP3370902B1 (fr) 2019-09-18
EP3370902A1 (fr) 2018-09-12
US20220266336A1 (en) 2022-08-25
FR3042992B1 (fr) 2021-09-10
FR3042992A1 (fr) 2017-05-05

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