EP3254785B1 - Procédé de formation de poudre mo-si-b - Google Patents

Procédé de formation de poudre mo-si-b Download PDF

Info

Publication number
EP3254785B1
EP3254785B1 EP17175229.8A EP17175229A EP3254785B1 EP 3254785 B1 EP3254785 B1 EP 3254785B1 EP 17175229 A EP17175229 A EP 17175229A EP 3254785 B1 EP3254785 B1 EP 3254785B1
Authority
EP
European Patent Office
Prior art keywords
powder
alloy powder
pieces
milling
alloy
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.)
Active
Application number
EP17175229.8A
Other languages
German (de)
English (en)
Other versions
EP3254785A1 (fr
Inventor
Brendan M. Lenz
Shiela R. Woodard
Douglas Michael Berczik
Mark Thomas UCASZ
William John BAJOREK
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.)
RTX Corp
Original Assignee
Raytheon Technologies Corp
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 Raytheon Technologies Corp filed Critical Raytheon Technologies Corp
Publication of EP3254785A1 publication Critical patent/EP3254785A1/fr
Application granted granted Critical
Publication of EP3254785B1 publication Critical patent/EP3254785B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C22C1/045—Alloys based on refractory metals
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • Molybdenum (Mo) has excellent high temperature strength which makes it attractive for structural applications at elevated temperatures.
  • the first oxidation product that forms is molybdenum trioxide (MoO 3 ).
  • MoO 3 has a high vapor pressure and sublimes at substantial rates above 1000°F (538°C), resulting in accelerated metal loss from the alloy.
  • Mo and Mo-based alloys are therefore largely limited to use in non-oxidizing environments at elevated temperatures without some form of externally applied oxidation protective coating.
  • Mo-Si-B alloys formed from some powder precursors require handling in the proper environment and/or thermal treatments to achieve the desired microstructure/phase assembly and/or interstitial element levels. This thermal processing can result in partial sintering of the material, forming pieces that are more difficult to process into a final product than a fine Mo-Si-B alloy powder.
  • EP 2799163 discloses a Mo-Si-B based alloy powder for use in a heat-resistant material, a metal-material raw material powder using the Mo-Si-B based alloy powder and a method of manufacturing the Mo-Si-B based alloy powder.
  • Cabouro et al., Powder Technology, 2011, 526 discloses formation of Mo/Si MA-agglomerates prepared using a high-energy planetary ball-mill.
  • US 2009/011266 relates to composite materials including molybdenum, molybdenum silicides, and molybdenum silicon boride.
  • US 2003/133824 discloses a ferritic steel and methods of producing it.
  • the present invention provides a method of forming Mo-Si-B powder according to claim 1.
  • the method of forming Mo-Si-B alloy powder includes preparing a mixture that includes Mo powder, Si 3 N 4 powder and BN powder, adding a polymer binder and liquid to the mixture to form a slurry, spray drying the slurry to form a spray dried powder containing Mo powder, Si 3 N 4 powder and BN powder particles, and thermally treating the spray dried powder to remove the binder, alloy the powders of the spray dried powder, and remove carbon, nitrogen and oxygen atoms, wherein thermally treating the spray dried powder forms at least some partially sintered Mo-Si-B alloy powder pieces.
  • the partially sintered Mo-Si-B alloy powder pieces are then milled in a milling container having contact surfaces composed of Mo-based material or lined and/or coated with Mo-based material to break down the pieces, and the milled Mo-Si-B alloy powder pieces are sieved to reclaim the Mo-Si-B alloy powder.
  • Milling the partially sintered Mo-Si-B alloy powder pieces comprises operation of a milling media composed of Mo-based material or lined and/or coated with Mo-based material that breaks down the pieces in the milling container.
  • An aspect of the present disclosure not forming part of the invention relates to a milling assembly for milling partially sintered Mo-Si-B alloy powder pieces to form Mo-Si-B alloy powder includes a milling container configured to receive the partially sintered Mo-Si-B alloy powder pieces.
  • the milling container has contact surfaces being composed of Mo-based material or lined and/or coated with Mo-based material.
  • a milling media is provided inside or complementary to the milling container, the milling media having contact surfaces that are composed of Mo-based material or lined and/or coated with Mo-based material and configured to break down the partially sintered Mo-Si-B alloy powder pieces to form the Mo-Si-B alloy powder.
  • Mo-Si-B alloys are attractive candidates for next generation high temperature structural materials in gas turbine engines.
  • the alloys of interest include ⁇ -Mo solid solutions and intermetallic phases such as Mo 5 SiB 2 , Mo 5 Si 3 , Mo 3 Si, Mo 2 B and others depending on alloying elements added to increase high temperature mechanical properties, oxidation resistance and other properties.
  • An example fabrication process in accordance with embodiments of the present disclosure for bulk components utilizes powder precursor materials.
  • a manufacturing process 10 for forming Mo-Si-B alloy powder and a component formed of Mo-Si-B alloy powder according to an embodiment of the present disclosure is shown in FIG. 1 .
  • the starting powders may include Mo powder, Si 3 N 4 powder, BN powder, and other alloying elements (step 12).
  • the powders may be mixed with a binder, such as an organic binder, and a suitable liquid to form a slurry (step 14).
  • suitable liquids include, without limitation, acetone, water, isopropyl alcohol, ethanol and mixtures thereof.
  • binders are polymethyl methacrylate (PMMA), polyvinyl alcohol (PVA), poly ethyl methacrylate (PEMA), and hydroxypropylcellulose.
  • the slurry is be spray dried to form spray dried powder containing Mo powder, Si 3 N 4 powder, BN powder and other alloy powder (step 16).
  • the powder is then thermally treated in an appropriately controlled environment (step 18), with the times and temperatures of the thermal treatment being controlled so that the binder is removed, and so that the constituent powders are alloyed to form Mo-Si-B alloy powder and undesirable atoms such as carbon, nitrogen and oxygen are removed.
  • steps 18 the times and temperatures of the thermal treatment being controlled so that the binder is removed, and so that the constituent powders are alloyed to form Mo-Si-B alloy powder and undesirable atoms such as carbon, nitrogen and oxygen are removed.
  • various thermal treatments can be employed without departing from the scope of the present disclosure.
  • thermal treatments as discussed in the following document can be used: " Fabrication, strength and oxidation of molybdenum-silicon-boron alloys from reaction synthesis", Middlemas, Michael Robert (2009) (Doctoral dissertation), retrieved from Georgia Tech University SMARTech libary, https://smartech.gatech.edu/handle/1853/28253 .
  • the Mo-Si-B powder sinters partially together. These partially sintered Mo-Si-B powder pieces need to be separated back into a relatively fine powder in order to be used for certain applications, such as being formed into a billet for producing a Mo-Si-B component, for example.
  • the partially sintered Mo-Si-B powder pieces In order to transform the partially sintered Mo-Si-B powder pieces into powder, it is necessary to first pulverize large partially sintered Mo-Si-B powder pieces to form smaller pieces of partially sintered alloy powder Alternatively, in some situations, not forming part of the invention, the partially sintered Mo-Si-B powder pieces may be sufficiently small that this step is not needed, or later processing steps may not require the pieces to be particularly small.
  • an alumina mortar and pestle may be used, for example, possibly in an inert atmosphere in some embodiments.
  • the pieces may be pulverized into smaller pieces for further processing that are about 0.20 to about 0.62 inch (5.1 to 15.8 mm) in diameter, although other size ranges may be used in other embodiments.
  • the pieces may be stored in a container under an inert atmosphere in some embodiments, such as an argon atmosphere in one particular example.
  • the pieces are milled (step 24).
  • the milling process may be performed in a number of different ways and with different types of equipment, and generally involves a milling container in which the partially sintered pieces are placed and milled, either with a milling media or by self-milling.
  • the milling container and any milling media that is employed are either composed of Mo-based material or have contact surfaces that are lined and/or coated with Mo-based material. Examples of milling processes that may be employed include jar milling, mortar grinding, planetary ball milling, and attritor milling, among others.
  • Jar milling (e.g., where the milling container is a jar composed of a Mo-based material or a jar having inner contact surfaces lined and/or coated with Mo-based material) is an example of a suitable milling process in which jars are rotated on automated rollers and the partially sintered Mo-Si-B powder pieces self-mill with no other milling media present.
  • milling media is included inside or complementary to the milling container to break down the partially sintered Mo-Si-B powder pieces.
  • contact surfaces of the milling container and any milling media By forming the contact surfaces of the milling container and any milling media out of Mo-based material or lining and/or coating the contact surfaces of the milling container and any milling media with Mo-based material, levels of contamination in the Mo-Si-B powder after milling can be minimized.
  • contamination of Mo-Si-B powder produced as described herein can be maintained below 0.08wt/% carbon and 0.06wt/% oxygen, or more particularly below 0.006wt% carbon and 0.01wt% oxygen, and even more particularly below 0.003wt% carbon and 0.004wt% oxygen, for example.
  • the term "contact surfaces” as used herein refers to surfaces of the milling container and milling media that come into contact with the pieces being milled during a milling operation (and therefore would have the potential to introduce contamination to the pieces being milled).
  • milling may be periodically interrupted and the powder sieved to reclaim fine powder from larger pieces (step 26).
  • Sieving with a coarse sieve such as a 16 mesh sieve for example (although other sizes may be used), may separate milled Mo-Si-B alloy powder pieces over a threshold size (for example, particles over 0.05 inch (1.27 mm) in diameter) for further milling.
  • a finer sieve such as a 120 mesh sieve for example (although other sizes may be used), may then separate particles to obtain a desired (e.g., final) powder size, such as by separating particles smaller than 4.7 micro inches (0.12 microns) in diameter that form the alloy powder, in a specific non-limiting example.
  • the Mo-Si-B alloy powder can be used in a number of applications, such as for the formation of a Mo-Si-B alloy component.
  • the Mo-Si-B alloy powder may be consolidated by sealing the powder in a can under vacuum (step 28) and then hot isostatically pressing (HIPing) the powder to form a billet (step 30).
  • the billet may then be thermal mechanically processed, heat treated, and machined to form the Mo-Si-B alloy component (step 32).
  • FIG. 2 An exploded view of an exemplary milling assembly, not forming part of the invention, that includes a Mo milling container (which has contact surfaces that may be composed of Mo-based material or lined and/or coated with Mo-based material) that may be used to mill partially sintered Mo-Si-B powder pieces, is shown in FIG. 2 .
  • the milling container is a milling jar 40 composed of Mo-based material that includes cylindrical body 42, defining a cavity C therein, end flanges 44 and 46 and end caps 48 and 50.
  • body 42, end flanges 44 and 46, and end caps 48 and 50 of milling jar 40 may be composed of Mo-based material or lined and/or coated with Mo-based material so that surfaces coming into contact with partially sintered Mo-Si-B powder pieces to be milled do not introduce contamination to the pieces during the milling process.
  • End caps 48 and 50 are attached to flanges 44 and 46 by bolts 52 and nuts 54, although other attachment or securing mechanisms can be used without departing from the scope of the present disclosure.
  • the ends of milling jar 40 are hermetically sealed by O-rings 56, although other sealing mechanisms can be used without departing from the scope of the present disclosure.
  • the cylindrical body 42 has an outer diameter D1 and an inner diameter D2.
  • Milling jar 40 (cylindrical body 42 plus end flanges 44, 46 and end caps 48, 50) has a length L1, as shown in FIG. 2 .
  • the outer diameter D1 of cylindrical body 42 can be 5.8 inches (14.7 cm), and overall length L1 with the end caps on can be 8.5 inches (21.6 cm).
  • the inner diameter D2 of the cylindrical body can be 5.3 inches (13.5 cm).
  • the partially sintered Mo-Si-B powder pieces may be self-milled with no added milling media, which helps to ensure that the Mo-Si-B powder is not contaminated during the milling process.
  • milling may be carried out under an inert atmosphere.
  • a milling assembly not forming part of the invention that may be used to mill partially sintered Mo-Si-B powder pieces
  • an apparatus employing a mortar as the milling container and a pestle as the milling media.
  • the contact surfaces of the mortar and the pestle are composed of Mo-based material or lined and/or coated with Mo-based material.
  • Such an apparatus may be an automatic mortar grinder or a manually operated mortar and pestle, where the pestle and mortar function complementary to one another to grind the partially sintered Mo-Si-B powder pieces between them to break down the pieces and form the Mo-Si-B alloy powder.
  • a further example of a milling assembly not forming part of the invention, that may be used to mill partially sintered Mo-Si-B powder pieces is a planetary ball mill, in which contact surfaces of a milling container and one or more balls (employed as a milling media inside the milling container) are composed of Mo-based material or lined and/or coated with Mo-based material.
  • a milling assembly not forming part of the invention that may be used to mill partially sintered Mo-Si-B powder pieces is an attritor mill, in which contact surfaces of a milling container and rotating attritor milling media inside the milling container are composed of Mo-based material or lined and/or coated with Mo-based material.
  • contact surfaces of the milling container and/or milling media being composed of Mo-based material or lined and/or coated with Mo-based material is intended to include the use of pure (100%) molybdenum for these contact surfaces, as well as phases of molybdenum borosilicates, molybdenum silicides and other Mo-Si-B chemistries.
  • Chemistry examples may include but are not limited to: MoSi 2 , Mo 5 SiB 2 , Mo 3 Si and Mo-Si-B chemistries called out in U.S. Patent Nos. 5,595,616 , 5,693,156 and 6,652,674 , for example.
  • milling assemblies Although several examples of milling assemblies have been disclosed, it should be understood that other milling assemblies may be used in which a milling container and milling media each have contact surfaces that are composed of Mo-based material or lined and/or coated with Mo-based material, in order to minimize contamination of Mo-Si-B powder produced in the manner disclosed herein, and the present disclosure is not limited to the examples disclosed.
  • a method of forming Mo-Si-B alloy powder includes: preparing a mixture that includes Mo powder, Si3N4 powder and BN powder; adding a polymer binder and liquid to the mixture to form a slurry; spray drying the slurry to form a spray dried powder containing Mo powder, Si3N4 powder and BN powder particles; thermally treating the spray dried powder to remove the binder, alloy the powders of the spray dried powder, and remove carbon, nitrogen and oxygen atoms, wherein thermally treating the spray dried powder forms at least some partially sintered Mo-Si-B alloy powder pieces; milling the partially sintered Mo-Si-B alloy powder pieces in a milling container (e.g.
  • Milling the partially sintered Mo-Si-B alloy powder pieces comprises operation of a milling media composed of Mo-based material or lined and/or coated with Mo-based material that breaks down the pieces in the milling container.
  • the method of the preceding paragraph can optionally include, additionally and/or alternatively any, one or more of the following features, configurations and/or additional components:
  • Milling the partially sintered Mo-Si-B alloy powder pieces may include jar milling the partially sintered Mo-Si-B alloy powder pieces in a jar composed of, or having contact surfaces composed, of Mo-based material or lined and/or coated with Mo-based material with no other milling media, to break down the pieces by self-milling in the jar.
  • Pulverizing the partially sintered Mo-Si-B alloy powder pieces to reduce a size of the partially sintered Mo-Si-B alloy powder pieces that are milled in the milling container may be performed.
  • the partially sintered Mo-Si-B alloy powder pieces that are milled in the milling container may be about 0.20 to 0.62 in (5.1 to 15.8 mm) in diameter.
  • the binder may be polymethyl methacrylate (PMMA), polyvinyl alcohol (PVA), polyethyl methacrylate (PEMA), or hydroxypropylcellulose.
  • PMMA polymethyl methacrylate
  • PVA polyvinyl alcohol
  • PEMA polyethyl methacrylate
  • hydroxypropylcellulose hydroxypropylcellulose
  • the liquid may be acetone, water, isopropyl alcohol (IPA), ethanol, or mixtures thereof.
  • IPA isopropyl alcohol
  • Sieving the milled Mo-Si-B alloy powder pieces may include sieving with a coarse sieve to separate milled Mo-Si-B alloy powder pieces over a threshold size for further milling, and sieving with a fine sieve to collect Mo-Si-B alloy powder.
  • the threshold size of Mo-Si-B powder pieces separated by the coarse sieve may be 0.05 in (1.27 mm) in diameter, and particles of the Mo-Si-B alloy powder may have a diameter smaller than 4.7 micro inches (0.12 microns).
  • the Mo-Si-B alloy powder may formed with contamination, e.g. interstitial contamination, that is less than 0.08wt/% carbon and 0.06wt/% oxygen.
  • the Mo-Si-B alloy powder may be formed with contamination, e.g. interstitial contamination, that is less than 0.006wt% carbon and 0.01 wt% oxygen.
  • the Mo-Si-B alloy powder may be formed with contamination, e.g. interstitial contamination, that is less than 0.003wt% carbon and 0.004wt% oxygen.
  • a method of forming a Mo-Si-B component includes producing Mo-Si-B powder by a method including any of the features, configurations and/or additional components listed above; sealing the Mo-Si-B powder under vacuum in a can; hot isostatic pressing (HIP) the can to form a billet; and forging, heat treating and machining the billet to form the Mo-Si-B alloy component.
  • HIP hot isostatic pressing

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Claims (10)

  1. Procédé de formation de poudre d'alliage Mo-Si-B comprenant :
    la préparation d'un mélange qui comporte de la poudre Mo, de la poudre Si3N4 et de la poudre BN ;
    l'ajout d'un liant et liquide polymère au mélange pour former une suspension ;
    le séchage par pulvérisation de la suspension pour former une poudre séchée par pulvérisation contenant des particules de poudre Mo, de poudre Si3N4 et de poudre BN ;
    le traitement thermique de la poudre séchée par pulvérisation pour éliminer le liant, allier les poudres de la poudre séchée par pulvérisation, et éliminer les atomes de carbone, d'azote et d'oxygène, dans lequel le traitement thermique de la poudre séchée par pulvérisation forme au moins quelques morceaux de poudre d'alliage Mo-Si-B partiellement frittés ;
    le broyage des morceaux de poudre d'alliage Mo-Si-B partiellement frittés dans un récipient de broyage ayant des surfaces de contact composées de matériau à base de Mo ou
    doublées et/ou revêtues de matériau à base de Mo pour décomposer les morceaux ; et
    le tamisage des morceaux de poudre d'alliage Mo-Si-B broyés pour récupérer la poudre d'alliage Mo-Si-B,
    dans lequel le broyage des morceaux de poudre d'alliage Mo-Si-B partiellement frittés comprend l'utilisation d'un agent de broyage composé de matériau à base de Mo ou doublé et/ou revêtu de matériau à base de Mo qui décompose les morceaux dans le récipient de broyage.
  2. Procédé selon la revendication 1, comprenant en outre :
    la pulvérisation des morceaux de poudre d'alliage Mo-Si-B partiellement frittés pour réduire une taille des morceaux de poudre d'alliage Mo-Si-B partiellement frittés qui sont broyés dans le récipient de broyage, et/ou
    dans lequel les morceaux de poudre d'alliage Mo-Si-B partiellement frittés qui sont broyés dans le récipient de broyage ont un diamètre de 0,20 à 0,62 pouce (5,1 à 15,8 mm).
  3. Procédé selon une quelconque revendication précédente, dans lequel le liant comprend du polyméthacrylate de méthyle (PMMA), de l'alcool polyvinylique (PVA), du polyméthacrylate d'éthyle (PEMA) ou de l'hydroxypropylcellulose.
  4. Procédé selon une quelconque revendication précédente dans lequel le liquide comprend de l'acétone, de l'eau, de l'alcool isopropylique (IPA), de l'éthanol ou des mélanges de ceux-ci.
  5. Procédé selon une quelconque revendication précédente, dans lequel le tamisage des morceaux de poudre d'alliage Mo-Si-B broyés comprend le tamisage avec un tamis grossier pour séparer les morceaux d'alliage de poudre Mo-Si-B broyés au-dessus d'une taille seuil pour un broyage supplémentaire, et le tamisage avec un tamis fin pour collecter de la poudre d'alliage Mo-Si-B.
  6. Procédé selon une quelconque revendication précédente, dans lequel la taille seuil des morceaux de poudre Mo-Si-B séparés par le tamis grossier a un diamètre de 0,05 pouce (1,27 mm), et des particules de poudre d'alliage Mo-Si-B ont un diamètre inférieur à 4,7 micropouces (0,12 micromètre).
  7. Procédé selon une quelconque revendication précédente, dans lequel la poudre d'alliage Mo-Si-B est formée avec une contamination qui est inférieure à 0,08 % en poids de carbone et à 0,06 % en poids d'oxygène.
  8. Procédé selon une quelconque revendication précédente, dans lequel la poudre d'alliage Mo-Si-B est formée avec une contamination qui est inférieure à 0,006 % en poids de carbone et à 0,01 % en poids d'oxygène.
  9. Procédé selon une quelconque revendication précédente, dans lequel la poudre d'alliage Mo-Si-B est formée avec une contamination interstitielle qui est inférieure à 0,003 % en poids de carbone et à 0,004 % en poids d'oxygène.
  10. Procédé de formation d'un composant d'alliage Mo-Si-B comprenant :
    la production d'une poudre d'alliage Mo-Si-B par le procédé selon une quelconque revendication précédente ;
    le scellement hermétique de la poudre d'alliage Mo-Si-B sous vide dans une boîte ;
    le pressage isostatique à chaud (HIP) de la boîte pour former une billette ; et
    le forgeage, le traitement thermique et l'usinage de la billette pour former le composant d'alliage Mo-Si-B.
EP17175229.8A 2016-06-10 2017-06-09 Procédé de formation de poudre mo-si-b Active EP3254785B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US201615179622A 2016-06-10 2016-06-10

Publications (2)

Publication Number Publication Date
EP3254785A1 EP3254785A1 (fr) 2017-12-13
EP3254785B1 true EP3254785B1 (fr) 2021-11-24

Family

ID=59067502

Family Applications (1)

Application Number Title Priority Date Filing Date
EP17175229.8A Active EP3254785B1 (fr) 2016-06-10 2017-06-09 Procédé de formation de poudre mo-si-b

Country Status (1)

Country Link
EP (1) EP3254785B1 (fr)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030133824A1 (en) * 2001-09-21 2003-07-17 Masami Taguchi High-toughness and high-strength ferritic steel and method of producing the same

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5693156A (en) 1993-12-21 1997-12-02 United Technologies Corporation Oxidation resistant molybdenum alloy
US6652674B1 (en) 2002-07-19 2003-11-25 United Technologies Corporation Oxidation resistant molybdenum
US20090011266A1 (en) * 2007-07-02 2009-01-08 Georgia Tech Research Corporation Intermetallic Composite Formation and Fabrication from Nitride-Metal Reactions
US9884367B2 (en) * 2011-12-28 2018-02-06 A.L.M.T. Corp. Mo—Si—B-based alloy powder, metal-material raw material powder, and method of manufacturing a Mo—Si—B-based alloy powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030133824A1 (en) * 2001-09-21 2003-07-17 Masami Taguchi High-toughness and high-strength ferritic steel and method of producing the same

Also Published As

Publication number Publication date
EP3254785A1 (fr) 2017-12-13

Similar Documents

Publication Publication Date Title
Moshtaghioun et al. Additive-free superhard B4C with ultrafine-grained dense microstructures
US20230133590A1 (en) Die and piston of an sps apparatus, sps apparatus comprising same, and method of sintering, densification or assembly in an oxidising atmosphere using said apparatus
US6753085B2 (en) Heat-resistant coated member
Ota et al. Application of high pressure gas jet mill process to fabricate high performance harmonic structure designed pure titanium
TWI464133B (zh) Polycrystalline MgO sintered body and its manufacturing method and MgO target for sputtering
US20120171098A1 (en) Method of consolidating ultrafine metal carbide and metal boride particles and products made therefrom
US5223186A (en) Microwave sintering of nanophase ceramics without concomitant grain growth
Yamanoglu Pressureless spark plasma sintering: A perspective from conventional sintering to accelerated sintering without pressure
JP2023543687A (ja) 大きな寸法の焼結セラミック体及びその作製方法
Shimizu et al. Fabrication and mechanical properties of monolithic MoSi2 by spark plasma sintering
JP2018145528A (ja) 溶射成形体
EP3254785B1 (fr) Procédé de formation de poudre mo-si-b
CN110392743B (zh) 硬质烧结体
KR102112725B1 (ko) 분산강화 금속 소결체의 제조방법
US7217386B2 (en) Preparation of nanocomposites of alumina and titania
GB2560256A (en) Coated superhard particles and composite materials made from coated superhard particles
EP1965940B1 (fr) Stabilite thermique amelioree de corps poreux en acier inoxydable ou en alliage
CN116134003A (zh) 大尺寸的烧结氧化钇体
JP6888294B2 (ja) Ｃｕ−Ｇａ合金スパッタリングターゲットの製造方法、及び、Ｃｕ−Ｇａ合金スパッタリングターゲット
Pogozhev et al. Features of the synthesis and consolidation of MeIVB2–(MeIV, Mo) Si2 ceramic powder for high-temperature applications
Md Raihanuzzaman et al. Refinement behavior of scrap silicon by mechanical milling
EP4219427A1 (fr) Procédé de fabrication de matériaux composites céramiques à des fins balistiques à base de b4c, tib2 et b4c/tib2
Astapov et al. HEAT-RESISTANT COATINGS FORMED FROM SHS POWDER OF THE ZrSi2–MoSi2–ZrB2 SYSTEM FOR CARBON COMPOSITES
KR20180137333A (ko) 치과소재 가공 툴용 텅스텐 카바이드계 소결체 제조방법
US5240691A (en) High density crystalline boron prepared by hot isostatic pressing in refractory metal containers

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION HAS BEEN PUBLISHED

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE

17P Request for examination filed

Effective date: 20180613

RBV Designated contracting states (corrected)

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

17Q First examination report despatched

Effective date: 20200409

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: RAYTHEON TECHNOLOGIES CORPORATION

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

INTG Intention to grant announced

Effective date: 20210602

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 1449462

Country of ref document: AT

Kind code of ref document: T

Effective date: 20211215

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602017049681

Country of ref document: DE

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG9D

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20211124

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 1449462

Country of ref document: AT

Kind code of ref document: T

Effective date: 20211124

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20220224

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20220324

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20220324

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20220224

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20220225

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602017049681

Country of ref document: DE

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

26N No opposition filed

Effective date: 20220825

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20220630

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220609

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220630

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220609

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220630

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220630

P01 Opt-out of the competence of the unified patent court (upc) registered

Effective date: 20230520

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20170609

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20240521

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20240521

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20240521

Year of fee payment: 8

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211124