EP4601823A1 - Préparation d'un monolithe métallique au moyen d'un procédé de pressage à chaud rapide - Google Patents

Préparation d'un monolithe métallique au moyen d'un procédé de pressage à chaud rapide

Info

Publication number
EP4601823A1
EP4601823A1 EP23794269.3A EP23794269A EP4601823A1 EP 4601823 A1 EP4601823 A1 EP 4601823A1 EP 23794269 A EP23794269 A EP 23794269A EP 4601823 A1 EP4601823 A1 EP 4601823A1
Authority
EP
European Patent Office
Prior art keywords
mould
metal
monolith
pressure
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
EP23794269.3A
Other languages
German (de)
English (en)
Inventor
Mythili PRAKASAM
Alain Largeteau
Jean-François SILVAIN
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.)
Centre National de la Recherche Scientifique CNRS
Universite de Bordeaux
Institut Polytechnique de Bordeaux
Original Assignee
Centre National de la Recherche Scientifique CNRS
Universite de Bordeaux
Institut Polytechnique de Bordeaux
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 Centre National de la Recherche Scientifique CNRS, Universite de Bordeaux, Institut Polytechnique de Bordeaux filed Critical Centre National de la Recherche Scientifique CNRS
Publication of EP4601823A1 publication Critical patent/EP4601823A1/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • 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
    • B22F3/003—Apparatus, e.g. furnaces
    • 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
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/02—Dies; Inserts therefor; Mounting thereof; Moulds
    • B30B15/022—Moulds for compacting material in powder, granular of pasta form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/34—Heating or cooling presses or parts thereof
    • 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
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the applicant has developed a method of making a metal monolith from a metal powder exempt of any binder or other sintering aid additive, the method comprising the steps of:
  • a Rapid Hot Press equipment (usually known by the acronym RHP) comprising a high-pressure mould for receiving said metal powder in which the heat is provided by induction with an inductive coil disposed around the high-pressure mould and a press, said inductive coil being coupled to a RF electrical power supply;
  • RHP Rapid Hot Press equipment
  • the induction heating is a non-oxidizing process carried out under air ambient highly mechanical resistant mould, the induction heating comprising a heating ramp from a temperature To of 20°C to a temperature Ti being comprised between 50°C and 550°C and preferably between 100°C and 400°C, while applying a uniaxial pressure to the mould greater than 0.1 MPa, said mould being a mould made of high strength material having a yield strength of at least 0.1 GPa, preferably at least 1.2 GPa.
  • the method according to the invention allows to consolidate under air in extreme short duration (notably for a time range 1-60 minutes) , avoiding oxidation and metal chemical reaction in the case of mixture of metal chemical elements.
  • the method of the invention allows to reali ze dense or lowly / highly (more than 50% ) porous metal monolith at temperatures below those involved in conventional inductive heating equipment applying the use of atmosphere protection, vacuum or inert gas to avoid oxidation of metal powder during the process .
  • the method of the invention has a shorter duration, simplified process steps , easy handling, economical costs , easy adj ustment of porosity ( si ze , ratio ) compared to currently known processes .
  • the measurement of the temperature may be reali zed within the mould by means of a thermocouple placed within the mould and capable of being eas ily manipulated to and from the mould, the inductive coil partially encircling the mould so as to present an open configuration to allow the thermocouple to be inserted into the mould without heating it and to facilitate handling of the apparatus .
  • the inductive coil may be in the form of a single loop forming several U-shaped folds , which are arranged on either side of a central loop- free part .
  • the measurement of the temperature may be reali zed within the mould by means of an optical pyrometer, the inductive coi l presenting a closed configuration with respect to each other .
  • i f a dense monolith is to be made by the process according to the invention, then an uniaxial pressure of between 100 MPa and 1200 MPa, and preferably between 500 MPa and 1200 MPa, may be applied to the mould at temperatures T1 equal to or greater than 100 ° C .
  • an uniaxial pressure of between 100 MPa and 1200 MPa, and preferably between 500 MPa and 1200 MPa, may be applied to the mould at temperatures T1 equal to or greater than 100 ° C .
  • the method of the invention may allow the control of pore size of the metal monolith through the temporary use of a space holder template mixed with the metal powder, so as to create a well- defined size porosity in the metal monolith up to 80% by applying a pressure from 0,1 MPa up to 1200 MPa, said space holder template being removed at the end of uniaxial pressing, or
  • the method of the invention may allow the creation of a porous monolith having a porosity up to 80% by applying a low pressure from 0.1 MPa up to 1200 MPa,
  • the space holder template may be for example sugar, or any powdered material easily soluble in water (salt, sugar, bicarbonate, ..) or easily degradable in an oven (corn, ..) :
  • the space holder template can be made of a natural or synthetic organic material that is able to remain solid and that does not degrade (burn or oxidise) in air up to 550°C.
  • the space holder template may be made of NaCl and can be easily removed by washing with water from the metal monolith. This dissolving process may be made faster by washing with water in an ultrasonic tank at room temperature or by boiling the water .
  • the induction heating of the method of the invention may comprise a heating ramp from To to Ti carried out at a heating rate o f 50 ° C/min, a plateau at Tl and a cooling ramp from To to Ti carried out at a cooling rate of 25 °C/min, for instance by means of an air j et or by by heat exchange fluid circulation .
  • the duration of the plateau may be between 1 s and 24 hours , and preferably between 1 and 3 minutes .
  • the metal powder for use in the present invention may comprises one single metal element or at least two metal elements , said metal elements of the metal powder being preferably selected from Al , Ti , Cu and mixtures thereof ( for example ) .
  • the metal powder presents a micrometric distribution .
  • the metal monolith according to the invention may be a dense monolith presenting a poros ity lower than 2 % or a porous monolith presenting a porosity comprised greater than 2 % , and preferably greater than 50% and up to 80% .
  • said Rapid Hot Press equipment further comprises a thermocouple placed within the mould and capable of being easily manipulated to and from the mould, while the inductive coil partially surrounding the mould as a single loop forming a plurality of U-shaped folds arranged around the mould symmetrically on either side of a central part of the mould .
  • the mould may be made of a material selected from metals and ceramics or ceramic-metal composite such as cermet , and preferably made of steel or a nickel alloy .
  • FIG . l is a picture showing the Rapid Hot Press Equipment of the invention.
  • FIG . 2 is a detailed view of the Rapid Hot Press Equipment shown in figure 1 , notably showing the high pressure mould ( internal diameter 10 mm) 2 for receiving the metal powder, the inductive coil 3 disposed around the mould 2 and a uniaxial press 4 ;
  • Figure 4 is a curve showing the effect of high uniaxial pressure on the relative density of a copper monolith obtained from a copper powder comprising dentritic Cu particles of 26 pm, when using the method according to the invention with induction heating including a plateau at 20°C and 150°C (Tl) for 1 minute (see example 2) ;
  • Figure 7 is a curve showing the effect of the temperature on the relative density of a titanium monolith from a titanium powder comprising spherical Ti particles of 50 pm in diameter, when using the method according to the invention with induction heating for 10 minutes and uniaxial pressing of 820 MPa or with induction heating for 1 minute and uniaxial pressing of 990 MPa;
  • Figure 9 is a XRD dif f ractogram (see example 9) showing the non-oxidation under air of titanium during the execution of the method according to the invention, obtained from a titanium powder comprising spherical Ti particles, when using the method according to the invention with induction heating including a plateau at 400°C (TI) for 10 minutes and uniaxial pressing of 970 MPa with and/or without the presence of a space holder template of NaCl;
  • Figure 11 is a curve (see example 13) showing the effect of the pressure on the relative density of an aluminium monolith obtained from an aluminium powder comprising Al particles of 40 pm in diameter, when using the method according to the invention with induction heating including a plateau at 20°C or 150°C (Tl) for 1 minute or at 400°C for 1 minute;
  • Figure 12 is a curve (see example 15) showing the effect of the pressure on the relative density of a metal monolith obtained from a metal powder comprising spherical Cu particles (50% in weight of the powder) and Al particles of 50 pm in diameter (50% in weight of the powder) , for elaborating a metal-metal composite, when using the method according to the invention with induction heating including a plateau at 150°C or 400°C (Tl) for 1 minute or 60 minutes;
  • - powder comprising a mixture of dentritic Cu particles ( 60% in weight of the powder ) and carbon fibres ( 40% in weight of the powder ) ( see example 6 ) ; - titanium powder comprising spherical Ti particles of 50 pm in diameter (see examples 7 to 9) ;
  • Figure 3 shows that it is possible, by applying a pressure as low as 0.1 kN, to realize a copper monolith with a relative porosity of 80% (from dentritic particles) while it is not possible to achieve a consolidation of the monolith (diameter 10 mm) under 1.2 kN when using spherical particles.
  • a pressure as low as 0.1 kN
  • By adjusting the force (for very low uniaxial forces) it is possible to make a very porous monolith, whose porosity can be adjusted.
  • the use of dentritic copper particles allows very high porosities to be achieved without the use of templates .
  • Example 2 effect of high force on Cu densif ication and consolidation
  • Figure 5 shows the non-oxidation of copper during the execution of the method according to the invention, without or in presence of NaCl (template) after H2O washing.
  • Example 4 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) in Cu dendritic Experimental conditions:
  • Example 5 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) on Metal Matrix Composite (MMC)
  • Figure 6 shows the non-oxidation of copper during the execution of the method according to the invention, without or in presence of NaCl (template) after H2O washing.
  • the method of the invention avoids this oxidation problem existing on the surface of the grains, initially, because the applied lower temperature : there is no oxidation under air due to the protective effect of the electromagnetic field generated by the inductive heating.
  • titanium powder comprising spherical Ti particles of 50 pm; induction heating including a plateau at 20°C and 150°C for 1 and 10 minutes, by applying different pressures from 10 MPa to 1 GPa.
  • Figure 8 shows that a very dense monolith (90% of density) can be obtained even at very low temperatures (20°C) if high pressures (1 GPa) are applied.
  • Induction heating including a plateau at 400°C for 10 minutes and uniaxial pressing of 970 MPa (without the presence of a space holder template of NaCl) .
  • Figure 9 shows the non-oxidation of Ti during the execution of the method according to the invention.
  • Example 10 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) in Ti spherical (50pm)
  • Hot- pressing the simplest of the hot consolidation techniques , consists of loading a loose powder into a graphite mold that is then placed between two punches and heated in an enclosed furnace .
  • the most conventional heating method for hot- pressing is high-temperature resistance ; however , other options are available , such as inductive hot-pressing where the heating of the powder is done by means of the surrounding graphite mold as susceptor republic
  • Example 11 effect of high force on the densif ication and consolidation of a mixture of 2 metals (dentritic Cu and spherical Ti)
  • metal powder comprising dentritic of 50% in weight of Cu particles of 26 pm and 50% in weight of spherical Ti particles of (50 pm) ; induction heating including a plateau at 20°C, 150°C and 400°C for 1 minute and 60 minutes.
  • Figure 10 shows that it is possible to obtain dense monoliths (more than 80%) even at 20°C by applying a pressure of 375 MPa. With a pressure of 1 GPa, a highly dense monolith (above 90%) can be obtained at 150°C, using the RHP equipment according to the invention.
  • Example 12 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) in a mixture of Ti spherical and Cu dendritic
  • Example 13 effect of high force on the densif ication and consolidation of aluminium
  • aluminium powder comprising of Al particles of 40 pm; induction heating including a plateau at 20°C, 150°C and
  • Figure 11 shows that it is pos ;ible to obtain dense monoliths (more than 85%) even at 20°C by applying a pressure of 250 MPa. With a pressure of 1 GPa, a highly dense monolith (above 95%) can be obtained even at 20°C, using the RHP equipment according to the invention.
  • Example 14 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) in an aluminium powder (40 pm)
  • Example 15 effect of high force on the densif ication and consolidation of a mixture of 2 metals
  • metal powder comprising 50% in volume of Cu spherical (15 pm) and 50% in volume of Al (40pm) ; induction heating including a plateau at 150°C and 400°C for 1 minute and 60 minutes.
  • Figure 12 shows that it is possible to obtain dense monoliths (more than 90%) even at 150°C by applying a pressure of 250 MPa. With a pressure of 1 GPa, a highly dense monolith (above 95%) can be obtained even at 150°C, using the RHP equipment according to the invention.
  • Example 16 Effect of addition of NaCl (grinding + sieving) as space holder (to calibrate the porosity size) in a mixture of Cu spherical and Ti spherical.
  • Example 17 Demonstration on the possibility for elaborating a multi-phase metal with the presence of interphase (alloy) or without (metal-metal composite) between both metals and non-oxidation of metals.
  • Figure 13 shows that long time duration (50 minutes) allows the allow formation (CU9AI4) .
  • Example 18 Demonstration of cold welding between grains: consolidation effect
  • Figure 14 comprises different SEM photographs showing of different monoliths obtained by the method according to the invention from different metal powders (a) spherical Cu particles, b) mixture of dentritic Cu particles and carbon fibers, c) Ti particles, d) dentritic Cu particles) : the pictures show the cold welding between grains (consolidation effect) .

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

La présente invention concerne un procédé à haute pression de préparation d'un monolithe métallique soit sous une forme dense, soit sous une forme hautement poreuse, à l'aide d'un équipement de pressage à chaud par chauffage inductif rapide. Le procédé de l'invention permet d'obtenir un monolithe métallique à partir d'une poudre métallique sans liant ni tout autre additif.
EP23794269.3A 2022-10-14 2023-10-09 Préparation d'un monolithe métallique au moyen d'un procédé de pressage à chaud rapide Pending EP4601823A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP22306557.4A EP4353383A1 (fr) 2022-10-14 2022-10-14 Préparation d'un monolithe métallique par un procédé de pressage à chaud rapide
PCT/EP2023/077820 WO2024079014A1 (fr) 2022-10-14 2023-10-09 Préparation d'un monolithe métallique au moyen d'un procédé de pressage à chaud rapide

Publications (1)

Publication Number Publication Date
EP4601823A1 true EP4601823A1 (fr) 2025-08-20

Family

ID=84360954

Family Applications (2)

Application Number Title Priority Date Filing Date
EP22306557.4A Pending EP4353383A1 (fr) 2022-10-14 2022-10-14 Préparation d'un monolithe métallique par un procédé de pressage à chaud rapide
EP23794269.3A Pending EP4601823A1 (fr) 2022-10-14 2023-10-09 Préparation d'un monolithe métallique au moyen d'un procédé de pressage à chaud rapide

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP22306557.4A Pending EP4353383A1 (fr) 2022-10-14 2022-10-14 Préparation d'un monolithe métallique par un procédé de pressage à chaud rapide

Country Status (3)

Country Link
EP (2) EP4353383A1 (fr)
JP (1) JP2025533760A (fr)
WO (1) WO2024079014A1 (fr)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3441392A (en) * 1967-03-27 1969-04-29 Melpar Inc Preparation of fiber-reinforced metal alloy composites by compaction in the semimolten phase
GB1220592A (en) * 1967-06-08 1971-01-27 Atomic Energy Authority Uk Improvements in or relating to powder-compacting dies
US20120098162A1 (en) 2010-10-26 2012-04-26 California Institute Of Technology Rapid hot pressing using an inductive heater
JP7201332B2 (ja) * 2018-04-09 2023-01-10 トヨタ自動車株式会社 希土類磁石の製造方法及びそれに用いられる製造装置

Also Published As

Publication number Publication date
EP4353383A1 (fr) 2024-04-17
WO2024079014A1 (fr) 2024-04-18
JP2025533760A (ja) 2025-10-09

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