US3814635A - Production of powder alloy products - Google Patents

Production of powder alloy products Download PDF

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Publication number
US3814635A
US3814635A US00324313A US32431373A US3814635A US 3814635 A US3814635 A US 3814635A US 00324313 A US00324313 A US 00324313A US 32431373 A US32431373 A US 32431373A US 3814635 A US3814635 A US 3814635A
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US
United States
Prior art keywords
grain
hot
product
extrusion
powder
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.)
Expired - Lifetime
Application number
US00324313A
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English (en)
Inventor
D Cometto
I Kirk
J Morse
R Crickmer
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.)
Huntington Alloys Corp
Original Assignee
International Nickel Co Inc
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Publication date
Application filed by International Nickel Co Inc filed Critical International Nickel Co Inc
Priority to US00324313A priority Critical patent/US3814635A/en
Priority to CA174,612A priority patent/CA990979A/en
Priority to JP48115991A priority patent/JPS49102506A/ja
Priority to AU64263/74A priority patent/AU6426374A/en
Priority to GB168474A priority patent/GB1433852A/en
Priority to FR7401278A priority patent/FR2213990B1/fr
Priority to DE2401849A priority patent/DE2401849C2/de
Priority to SE7400534A priority patent/SE403626B/xx
Application granted granted Critical
Publication of US3814635A publication Critical patent/US3814635A/en
Priority to IT47738/74A priority patent/IT1013046B/it
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • B22F3/24—After-treatment of workpieces or articles

Definitions

  • the present invention relates to powder metallurgy, and more particularly to the production of dispersion strengthened, mechanically alloyed superalloys characterized by an improved combination of characteristics at elevated temperature, e.g., about 1800 F. and above.
  • the subject invention involves (a) hot consolidating, as by extrusion, superalloy powder, particularly mechanically alloyed powder containing a fine, well distributed, inert dispersoid, under (i) conditions of temperature, reduction ratio, and strain rate correlated (ii) to provide a solid product having a fine grain, e.g., having dimensions less than about microns and such that upon (b) heating the solid product to a grain coarsening temperature of about 1200 C to 1350 C.
  • a coarse grain structure e.g., a grain structure having a minimum value of the smallest grain dimension of at least about 10 microns and having an average value of the smallest grain dimension of at least about 200 microns, i.e., a grain structure essentially free of fine grains.
  • This processing is then followed by (c) hot working the consolidated grain-coarsened product to achieve a hot worked product characterized by coarse, elongated grains having an aspect ratio of greater than 8: 1, e.g., 16:1 and higher, whereby substantially improved stress-rupture properties are attained as compared with the properties of the material in the initially graincoarsened condition.
  • solid products obtained by hot extrusion can, prior to initial grain coarsening, be beneficially further hot worked, as by, for example, hot rolling or swaging and the like.
  • the condition of the resultant solid product should be such that, when subjected to a subsequent high temperature grain coarsening heat treatment, essentially all of the resulting grains measure greater than about 10 microns in their smallest dimension. It is preferred that the grains after this treatment have an average value for their smallest dimension of at least 200 microns, e.g., 1000 microns for more.
  • the aspect ratio being the ratio of the maximum dimension of a grain to the minimum dimension of the grain.
  • the consideration heretofore has generally been to achieve high aspect ratios by this type of grain coarsening treatment, say greater than 10:1 and up to 50:1 or more. It is deemed beneficial that the average grain aspect ratio imparted by the initial grain coarsening not exceed about 4:1. A ratio of up to about 8:1 is contemplated; however, it is considered marginal.
  • the present invention is applicable to a wide variety of dispersion-strengthened metal systems, and is particularly advantageous for producing dispersion-strengthened superalloys containing, by weight, up to about chromium, up to about 8% aluminum, up to about 8% titanium, up to about 40% molybdenum, up to about 40% tungsten, up to about 20% columbium, up to about 30% tantalum, up to about 40% copper, up to about 3% vanadium, up to about 15% manganese, up to about 2% carbon, up to about 2% silicon, up to about 1% boron, up to about 2% zirconium, up to about 0.8% magnesium, up to about 4% hafnium, up to about 10 volume percent refractory dispersoid material, the balance being essentially at least one iron group metal (iron, nickel, cobalt) with the sum of the iron group metals being at least 25%.
  • iron group metal iron, nickel, cobalt
  • the melting point of the superalloys are desirably in the temperature range of about 1200 C. to about 1375 C. or higher.
  • the superalloys contain about 5 to about 50 to 60%, e.g., about 5 to 35%, chromium; up to about 6.5%, e.g., about 0.2 to about 5%, aluminum; up to about 6.5%, e.g., about 0.2 to about 5%, titanium; up to about 10 or 15%, e.g., up to about 4%, molybdenum; up to about 20%, e.g., up to about 6%, tungsten; up to about 10%, columbium; up to about 10%, e.g., up to about 3%, tantalum; up to about 2%, vanadium; up to about 2% manganese; up to about 1% silicon; up to about 0.75% carbon; up to about 0.1% boron; up to about 1% zirconium; up to about 0.2% magnesium, up to about 40%iron
  • Refractory compounds that can be used as the dispersoid include refractory oxides, carbides. nitrides, borides, notably the oxides, carbides, nitrides and borides of such refractory metals as yttrium, lanthanum and thorium.
  • Other refractory oxides such as those of zirconium, titanium, cerium, beryllium, aluminum and the like may be utilized.
  • the refractory oxides generally include the oxides of those metals whose negative free energy of formation of the oxides per gram-atom of oxygen at about 25 C., is about 90 kcal. or more negative and whose melting point is at least about 1300 C.
  • Dispersoid materials that are particularly useful include yttria, lanthana, ceria, zirconia and thoria in sizes smaller than about one micron and advantageously, smaller than 0.1 micron.
  • the powder be mechanically alloyed beyond the milling time required to attain saturation hardness for the composition to provide compositional homogeneity or uniformity, including substantially uniform distribution of finely-divided dispersoid materal therethrough.
  • the homogeneity of the powder should be such that when a polished section is viewed at 250 diameters, initial constituents of the powder mix cannot be identified.
  • the mechanically alloyed composite powders range in size from about 3 microns to about 200 microns, more preferably, about 20 microns to about 200 microns, it being possible for the powder particles to range in size up to about 500 microns.
  • the mechanical alloying operation be conducted for longer times where a lower impeller speed is employed in order to provide homogeneous powder.
  • Other factors including the particle size and composition of constitutent powders in the initial powder mixture can affect the milling time required to provide powders of homogeneous structure and composition. While it has been found beneficial to mechanically alloy nickel-base superalloy compositions under a flowing atmosphere mixture of, for example, nitrogen with about 0.25% air, an atmosphere of sealed air, or an atmosphere of other gas mixtures may also be used, e.g., argon and air.
  • Interdispersion cold bonding agents as described in U.S. applications Ser. Nos. 327,321 and 327,323, both filed Jan. 29, 1973, can also be employed.
  • the most easily controllable parameters are temperature and reduction ratio.
  • Strain rate another important parameter, is a function of power available in the consolidation equipment employed. As indicated above, this consolidation step can be carried out by hot extrusion. It is generally desirable that the extrusion be conducted within the range of about 900 C. to about 1150 C., at a ratio of not less than about 4:1, preferably at least 5:1 or higher, and a relatively high strain rate. In the case of hot extrusion, strain rate is directly proportional to ram speed.
  • the requisite grain structure essentially free of fine grains is obtained in an extruded product which has been given the high temperature grain coarsening heat treatment without any additional hot-working prior'to heat treatment when, with reference to an extrusion having a 9-inch diameter container, the extrusion temperature is maintained between about 900 C. and about 1066" C., the extrusion ratio is maintained between about 5 :1 to about 50:1 and the ram speed exceeds a minimum required value which depends upon the temperature and ratio.
  • the mechanically alloyed powder can be consolidated by other means, for example, by hot pressing or hot rolling. In such operations, strain rates and reduction ratios are lower than in hot extrusion.
  • the resulting consolidated product is subjected to further working in a separate operation, e.g., swaging, rolling, etc., before the grain coarsening heat treatment to develop grain structure which is essentially free of fine grains.
  • the solid superalloy product will usually have a fine grain size, e.g., less than 10 microns. It is then heated to an elevated temperature below the incipient melting point to achieve grain coarsening. For substantially complete grain coarsening, the solid product is heated at a temperature of about 1200 C. or higher, e.g., about 1220 to about 1345 C., but below the incipent melting point, for the requisite time, e.g., about one-half hour.
  • the solid product is then hot worked to mechanically transform the grains to coarse, elongated shape so that the grains in the final product have a high aspect ratio of about 8:1 to 64:1 or higher.
  • the working of the grain coarsened product preferably is carried out at an elevated temperature, e.g., about 980 C. to about 1200" C. to reduce the product by an amount suflicient to produce the desired aspect ratio. Hot working temperatures, reductions, and reduction rates should be correlated, so as to prevent any substantial metallurgical transformation to fine grain.
  • An outstanding advantage of the present invention is that the grain coarsened product can besubjected to large hot reductions, e.g., reductions of up to 75% or 90% 'or even higher, to provide the desired coarse, elongated grains and, consequently, superior elevated temperature properties.
  • This capability is an important and significant advantage in operations for producing sheet, foil, plate, bars, etc., where large amounts of hot reduction provide cost savings and other advantages.
  • Such working advantageously can be carried out by hot rolling the grain coarsened product either unidirectionally, as by rolling in a single direction, or multidirectionally, as by cross-rolling, for example. Rolling in a single direction generally results in a fibrous grain morphology, while two-directional rolling produces plate-like grains, when viewed two-dimensionally.
  • This hot working step can also be accomplished by hot forging or other methods.
  • hot working the grain coarsened product to produce coarse, elongated grains therein is carried out at a temperature in the range of about 980 C. to about 1200 C., preferably, about 1065 C. to about 1180 C., e.g., about 1090 C. to 1150 C. to achieve a working reduction of about 35% or more, preferably about 50% or more, e.g., about 75%.
  • a reduction per pass of less than about 40% and preferably less than about 30%, e.g., not greater than about 25% of the cross-sectional area of the grain coarsened product.
  • the hot rolled products should exhibit virtually no fine grains at magnifications as high as 1000 diameters, the absence thereof contributing to the consistently superior high temperature properties of products produced in accordance herewith.
  • the uniform distribution of the dispersoid in the solid products produced according to the present invention remains substantially unaffected by the grain-coarsening heat treatment and the subsequent hot working procedure above described, there being no evidence of agglomeration of the dispersoid particle in the product at magnifications up to 20,000 diameters even after the grain coarsening heat treatment at 2400,'F. for one-half hour and notwithstanding the large size of the resulting coarsened grains.
  • EXAMPLE I A 36.25 kg. powder charge containing 24.86 kg. of nickel powder of. 4 micron size, 7.52 kg. of 6 micron chromium powder, 3.37 kg. of -200 mesh nickel-titanium-aluminum master alloy, and 0.50 kg. of 28 millimicron yttria was mechanically alloyed for hours under a flowing atmosphere, consisting of nitrogen with about 0.25% air in a 100-gallon capacity Szegvari attritor operated at an impeller speed of 98 rpm. and with 1600 pounds of inch diameter steel balls providing a ballto-powder ratio of 20:1, to produce compositepowder particles of Alloy A that were substantially homogeneous in composition.
  • the composite powder was filled into a 8%-ll'l0h diameter mild steel can, which was then sealed to air.
  • the canned composite powder was then heated to a temperature of about 980 C. and extruded, with an extrusion ram speed of 2.5 inches per second in a press having a 9-inch diameter container at a 16:1 extrusion ratio.
  • a portion of the extrusion thus produced was grain coarsened by heat treating it at 1315 C. for one-half hour and metallographic examination thereof indicated the grain coarsened product to have an average grain aspect ratio of 8:1 (on the high side) and to be free of fine grain.
  • a specimen cut from the grain coarsened product was stress-rupture tested at 1038 C. under a load of 17,500 p.s.i., the resulting rupture life being 26.9 hours. This value is quite good and is representative of the prior art for this alloy.
  • the product provided in accordance with the invention is useful in the production of articles such as gas turbine blades and vanes and other articles subjected in use to the combined effects of elevated temperature and stress.
  • a process for improving elevated temperature stress rupture properties of products made from mechanically alloyed powder which comprises hot consolidating the powder to provide a solid product having fine grains, heating the solid product at a temperature above about 1200" C. but below the incipient melting point of the alloy to achieve a coarse grain structure free of detrimental fine grains and characterized by a relatively low average grain aspect ratio, and thereafter hot working the coarse grained solid product to achieve a product characterized by coarse, elongated grains, the structure remaining free of deleterious fine grains.
  • the alloy product contains about 5% to about 50% chromium, up to about 6.5% each of aluminum and titanium, up to about 15% molybdenum, up to about 20% tungsten, up to about 10% columbium, up to about 10% tantalum, up to about 1% silicon, up to about 0.75% carbon, up to about 0.1% boron, up to 1% zirconium, up to about 2% each of manganese and vanadium, up to about 0.3% magnesium, up to about 40% iron, up to about 7% by volume of refractory dispersoid material, and the balance essentially nickel.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)
US00324313A 1973-01-17 1973-01-17 Production of powder alloy products Expired - Lifetime US3814635A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US00324313A US3814635A (en) 1973-01-17 1973-01-17 Production of powder alloy products
CA174,612A CA990979A (en) 1973-01-17 1973-06-21 Production of powder alloy products
JP48115991A JPS49102506A (enrdf_load_stackoverflow) 1973-01-17 1973-10-17
AU64263/74A AU6426374A (en) 1973-01-17 1974-01-07 Manufacture of wrought dispersion strengthened coarse grained super strength alloys
GB168474A GB1433852A (en) 1973-01-17 1974-01-14 Powder metallurgy process
FR7401278A FR2213990B1 (enrdf_load_stackoverflow) 1973-01-17 1974-01-15
DE2401849A DE2401849C2 (de) 1973-01-17 1974-01-16 Verfahren zum Herstellen von verformten Gegenständen aus einer dispersionsverfestigten Legierung
SE7400534A SE403626B (sv) 1973-01-17 1974-01-16 Sett att framstella en plastiskt bearbetad, dispersionsherdad legering med grova langstreckta korn
IT47738/74A IT1013046B (it) 1973-01-17 1977-01-15 Procedimento per preparare prodotti lavorati di leghe rafforzate in di spersione

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US00324313A US3814635A (en) 1973-01-17 1973-01-17 Production of powder alloy products

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US3814635A true US3814635A (en) 1974-06-04

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US00324313A Expired - Lifetime US3814635A (en) 1973-01-17 1973-01-17 Production of powder alloy products

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US (1) US3814635A (enrdf_load_stackoverflow)
JP (1) JPS49102506A (enrdf_load_stackoverflow)
AU (1) AU6426374A (enrdf_load_stackoverflow)
CA (1) CA990979A (enrdf_load_stackoverflow)
DE (1) DE2401849C2 (enrdf_load_stackoverflow)
FR (1) FR2213990B1 (enrdf_load_stackoverflow)
GB (1) GB1433852A (enrdf_load_stackoverflow)
IT (1) IT1013046B (enrdf_load_stackoverflow)
SE (1) SE403626B (enrdf_load_stackoverflow)

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909309A (en) * 1973-09-11 1975-09-30 Int Nickel Co Post working of mechanically alloyed products
US4619699A (en) * 1983-08-17 1986-10-28 Exxon Research And Engineering Co. Composite dispersion strengthened composite metal powders
US4627959A (en) * 1985-06-18 1986-12-09 Inco Alloys International, Inc. Production of mechanically alloyed powder
US5085679A (en) * 1990-11-23 1992-02-04 Owens-Corning Fiberglas Corporation Glass spinner manufacture
US5118332A (en) * 1991-06-04 1992-06-02 Owens-Corning Fiberglas Corporation Composite brazed spinner
US5328499A (en) * 1993-04-28 1994-07-12 Inco Alloys International, Inc. Mechanically alloyed nickel-base composition having improved hot formability characteristics
US5743157A (en) * 1996-07-31 1998-04-28 Owens-Corning Fiberglas Technology, Inc. Method for making a strengthened spinner having integrally formed ribs
US20040118245A1 (en) * 2002-12-23 2004-06-24 Ott Eric Allen Method for meltless manufacturing of rod, and its use as a welding rod
US20040208775A1 (en) * 2003-04-16 2004-10-21 National Research Council Of Canada Process for agglomeration and densification of nanometer sized particles
US20070034048A1 (en) * 2003-01-13 2007-02-15 Liu Shaiw-Rong S Hardmetal materials for high-temperature applications
US20070119276A1 (en) * 2005-03-15 2007-05-31 Liu Shaiw-Rong S High-Performance Friction Stir Welding Tools
US20070186416A1 (en) * 2006-01-24 2007-08-16 Jens Birkner Component repair process
US20080257107A1 (en) * 2003-01-13 2008-10-23 Genius Metal, Inc. Compositions of Hardmetal Materials with Novel Binders
US20100061875A1 (en) * 2008-09-08 2010-03-11 Siemens Power Generation, Inc. Combustion Turbine Component Having Rare-Earth Elements and Associated Methods
US20100180514A1 (en) * 2003-01-13 2010-07-22 Genius Metal, Inc. High-Performance Hardmetal Materials
US10100386B2 (en) 2002-06-14 2018-10-16 General Electric Company Method for preparing a metallic article having an other additive constituent, without any melting
US20200024689A1 (en) * 2017-07-24 2020-01-23 U.S. Army Research Laboratory Aluminum based nanogalvanic compositions useful for generating hydrogen gas and low temperature processing thereof
US10604452B2 (en) 2004-11-12 2020-03-31 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3444712A1 (de) * 1984-12-07 1986-06-12 Seilstorfer GmbH & Co Metallurgische Verfahrenstechnik KG, 8092 Haag Stahlmatrix-hartstoff-verbundwerkstoff
DE3714239C2 (de) * 1987-04-29 1996-05-15 Krupp Ag Hoesch Krupp Verfahren zur Herstellung eines Werkstoffs mit einem Gefüge nanokristalliner Struktur
DE102006031366C5 (de) * 2006-07-06 2010-01-28 Ecka Granulate Velden Gmbh Verfahren zur Herstellung von Formteilen aus dispersionsverfestigten Metalllegierungen

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1487993A (fr) * 1965-07-29 1967-07-07 Du Pont Nouveaux alliages nickel-chrome et procédé pour leur fabrication

Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909309A (en) * 1973-09-11 1975-09-30 Int Nickel Co Post working of mechanically alloyed products
US4619699A (en) * 1983-08-17 1986-10-28 Exxon Research And Engineering Co. Composite dispersion strengthened composite metal powders
US4647304A (en) * 1983-08-17 1987-03-03 Exxon Research And Engineering Company Method for producing dispersion strengthened metal powders
US4627959A (en) * 1985-06-18 1986-12-09 Inco Alloys International, Inc. Production of mechanically alloyed powder
US5085679A (en) * 1990-11-23 1992-02-04 Owens-Corning Fiberglas Corporation Glass spinner manufacture
US5118332A (en) * 1991-06-04 1992-06-02 Owens-Corning Fiberglas Corporation Composite brazed spinner
US5328499A (en) * 1993-04-28 1994-07-12 Inco Alloys International, Inc. Mechanically alloyed nickel-base composition having improved hot formability characteristics
US5743157A (en) * 1996-07-31 1998-04-28 Owens-Corning Fiberglas Technology, Inc. Method for making a strengthened spinner having integrally formed ribs
US10100386B2 (en) 2002-06-14 2018-10-16 General Electric Company Method for preparing a metallic article having an other additive constituent, without any melting
US7727462B2 (en) * 2002-12-23 2010-06-01 General Electric Company Method for meltless manufacturing of rod, and its use as a welding rod
US20040118245A1 (en) * 2002-12-23 2004-06-24 Ott Eric Allen Method for meltless manufacturing of rod, and its use as a welding rod
US20070034048A1 (en) * 2003-01-13 2007-02-15 Liu Shaiw-Rong S Hardmetal materials for high-temperature applications
US20080257107A1 (en) * 2003-01-13 2008-10-23 Genius Metal, Inc. Compositions of Hardmetal Materials with Novel Binders
US20100180514A1 (en) * 2003-01-13 2010-07-22 Genius Metal, Inc. High-Performance Hardmetal Materials
US7235118B2 (en) 2003-04-16 2007-06-26 National Research Council Of Canada Process for agglomeration and densification of nanometer sized particles
US20040208775A1 (en) * 2003-04-16 2004-10-21 National Research Council Of Canada Process for agglomeration and densification of nanometer sized particles
US10604452B2 (en) 2004-11-12 2020-03-31 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US20070119276A1 (en) * 2005-03-15 2007-05-31 Liu Shaiw-Rong S High-Performance Friction Stir Welding Tools
US7857188B2 (en) 2005-03-15 2010-12-28 Worldwide Strategy Holding Limited High-performance friction stir welding tools
US20070186416A1 (en) * 2006-01-24 2007-08-16 Jens Birkner Component repair process
US20100061875A1 (en) * 2008-09-08 2010-03-11 Siemens Power Generation, Inc. Combustion Turbine Component Having Rare-Earth Elements and Associated Methods
US20200024689A1 (en) * 2017-07-24 2020-01-23 U.S. Army Research Laboratory Aluminum based nanogalvanic compositions useful for generating hydrogen gas and low temperature processing thereof
US12054809B2 (en) * 2017-07-24 2024-08-06 The United States Of America As Represented By The Secretary Of Army Aluminum based nanogalvanic compositions useful for generating hydrogen gas and low temperature processing thereof

Also Published As

Publication number Publication date
CA990979A (en) 1976-06-15
FR2213990A1 (enrdf_load_stackoverflow) 1974-08-09
DE2401849A1 (de) 1974-08-01
FR2213990B1 (enrdf_load_stackoverflow) 1978-03-10
GB1433852A (en) 1976-04-28
IT1013046B (it) 1977-03-30
SE403626B (sv) 1978-08-28
DE2401849C2 (de) 1983-01-27
JPS49102506A (enrdf_load_stackoverflow) 1974-09-27
AU6426374A (en) 1975-07-10

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