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

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

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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
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Prior art keywords
powder
alloy powder
pieces
milling
alloy
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German (de)
English (en)
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EP3254785A1 (fr
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Brendan M. Lenz
Shiela R. Woodard
Douglas Michael Berczik
Mark Thomas UCASZ
William John BAJOREK
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RTX Corp
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Raytheon Technologies Corp
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/047Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes 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

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  • 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)

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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

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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

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