US3909309A - Post working of mechanically alloyed products - Google Patents

Post working of mechanically alloyed products Download PDF

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Publication number
US3909309A
US3909309A US396204A US39620473A US3909309A US 3909309 A US3909309 A US 3909309A US 396204 A US396204 A US 396204A US 39620473 A US39620473 A US 39620473A US 3909309 A US3909309 A US 3909309A
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United States
Prior art keywords
hot
accordance
dispersoid
working
mechanically alloyed
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Expired - Lifetime
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US396204A
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English (en)
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Michael James Bomford
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Huntington Alloys Corp
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International Nickel Co Inc
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Priority to US396204A priority Critical patent/US3909309A/en
Priority to CA207,425A priority patent/CA1041882A/en
Priority to JP49104815A priority patent/JPS591779B2/ja
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof

Definitions

  • thermomechanical processing of mechanically alloyed superalloy composite particles has been accomplished by virtue of extrusion, with improved extrusion parameters having been recently developed as set forth in copending US. Pat. application 131,761.
  • extrusion has dominated the thermomechanical processing scene, so yttria and thoria have received virtually exclusive attention as the dispersoids.
  • cost is always an important factor, other oxide dispersoids have been investigated and this has brought forth an unexpected problem.
  • the overall stress-rupture properties at elevated tempera tures of mechanically alloyed superalloys notably the nickel and/or cobalt-base compositions, dispersionstrengthened by an oxide of a lanthanide series metal are markedly enhanced by extruding a compact of the composite alloy particles and thereafter hot working (as by forging or hot rolling) the extruded product under correlated conditions of temperature and reduction such that upon germinative grain growth heat treatment a product is produced having a coarse, elongated grain structure, there being few, if any, fine grains.
  • the initial powder charge should be carried out to the point of at least substantial saturation hardness, i.e., the level at which there is about at least a 50% difference between the base hardness of the alloy in the unworked condition and its saturated hardness in substantially the fully coldworked condition, this to provide mechanically alloyed powders of substantially homogeneous microstructure, such that upon examination of the structure of the powder at a magnification of, say, 250 diameters there is virtually no evidence of the starting material, the initial powder ingredients having been intimately united and interdispersed.
  • Extrusion of the composite powder should be conducted at a temperature higher than about 1400F., so to achieve substantially 100% density in the consolidated product.
  • the composite powder is preferably consolidated by hot extruding at a temperature of about 1600F. to 2100F. at an extrusion ratio of about 4:1 to 50:1.
  • Post extrusion hot working can be carried out as by hot forging or hot rolling, it being generally preferred that the amount of hot working be greater for alloys containing lower amounts of dispersoid material and less for higher dispersoid contents.
  • a reduction of about 20 to about 80% at about 1600F. can be used where the dispersoid content of the consolidated product is about 1 or l /z% or less, by volume, while about 10 to about 40% reduction at about 2000F. can be used where the dispersoid content is about 3% or more, with a reduction of about 20 to at 1800F. being advantageous with dispersoid contents of about 1.5 to about 3%.
  • Post extrusion hot working or hot rolling should preferably be conducted over the temperature and reduction ranges shown in Table I below, where the consolidated products contain about 0.5 to about 5%, by volume, lanthanide metal oxide dispersoid material having an average particle size of about 50 Angstroms to about 600 Angstroms.
  • hot roll 1700 to 2100 I to 80 (I800 to 2050)* (20 to 60)* R.E.O.(b) hot forge I600 to 2000 10 to 60 (I750 to I900)* (15 to 45)* hot roll I700 to 2000 20 to 60 (I750 to 2000)* (25 to 45)* CeO hot forge 1700 to 2000 10 to 60 (I700 to I850) (I5 to 40)* Preferred (a)NominaI comp: 40-45% Ianthana, 32-37% neodymia, 8-I2% prueseodymia, balance oxides of other lanthanide metals.
  • the hot worked consolidated products described above are thereafter heated to attain coarse elongated grained products.
  • a suitable temperature range is from about 2200F. or higher, up to the incipient melting point of the alloy for periods of about it to 4 hours.
  • the coarsened grains thus produced generally will have average dimensions of about 500 to 5000 microns in length and about 50 to 1000 microns in width, and are elongated in the direction or directions of working. It is important that the hot working operation always precede the grain coarsening heat treatment and it is desirable that the exposure of the consolidated product to elevated temperatures, e.g., 2150F. or higher, prior to hot working be minimal and preferably be avoided, to avoid imparing the producibility of coarse, elongated grains by the grain-coarsening heat treatment subsequent to hot working.
  • EXAMPLE I An 8.5 kg powder charge containing 6.42 kg of nickel having an average particle size of 5 pm, 1.7 kg of Cr having an average size of 50 pm, 1.3 kg of a Ni- 8.5% Al-17% Ti master alloy with an average size of 50 pm, 0.02 kg ofa Ni-29% Zr (master alloy) and .003 kg of a Ni-18% boron master alloy and 0.153 kg of Ianthana having an average particle size of about 400 angstroms, prepared by calcining lanthanum oxalate at a temperature of 1300F., was mechanically alloyed in a IO-gallon capacity attritor for a period of 17 hours at an impeller speed of 182 rpm, the attritor being provided with 390 pounds of inch nickel pellets, which served as the attrition medium.
  • the minus 45 mesh fraction of the mechanically alloyed powder was packed in mild steel cans of 3 /2 inch diameter and the cans were sealed and extruded at 1900F. at ram speed of 0.5 linear feet per second to rectangular bars /8 by "/8 inches in crosssectional dimension, the extrusion reduction ratio being 16:1.
  • the consolidated alloy contained by weight, 20% chromium, 1.2% aluminum, 2.4% titanium, 0.07% zirconium, 0.007% boron, 2% volume lanthana having an average particle size of about 400 Angstroms, the balance being essentially nickel.
  • a portion of the asextruded bar was heated at 2400F. for 2 hours without any prior hot working, and the product exhibited fine grains. Upon aging and the testing at 1900F., it was found that the stress-rupture life was virtually nil at 16,000 psi stress.
  • Pieces of the extruded bar were worked either by forging or rolling, at various elevated temperatures and various reductions (Tables III and IV), the reduction being applied to the inch dimension except where stated otherwise. In the rolling procedure, the reduction per pass was about 15%.
  • the thus-hot worked pieces were given a grain coarsening heat treatment of 2400F. for 2 hours and then were aged by heating at 1975F. for 7 hours and at 1300F. for 16 hours. Specimens from the grain coarsened-and-aged pieces were tested for stress-rupture properties at 1900F. and 1400F., the results being set out in Tables III and IV.
  • Specimen unbroken stess raised "Specimen unbroken A test discontinued grip or furnace failure.
  • grain coarsening treatment revealed grains having average dimensions of about 1000 microns in length and about 80 microns in width. The grain structure was substantially uniform and no finegrained areas were evident.
  • Example II An alloy similar in composition to that in Example I but having 2%% of a dispersoid mixture (herein refractory oxide mixture) comprising, by weight, 25% lanthana, 48% ceria, 17% neodymia, 5% praeseodymia and the balance essentially oxides of other lanthanide series metals (average particle size of about 350 Angstroms), was mechanically alloyed in the manner given in Example I, except the processing time was 20 hours.
  • the minus 45 mesh fraction was sealed in mild steel cans and extruded at 1900F. at a reduction ratio of 16:1 to provide bar extrusions having a rectangular cross section of X 15/ 16-inch dimensions.
  • EXAMPLE III A mechanically alloyed powder having a nominal composition similar to that in Example I except that the tions shown in Table VI and then grain coarsened by heating at 2400F. for 2 hours and stress-rupture tested at 1400F. From the stress-rupture test results given in Table VI, it can be seen that satisfactory intermediate dispersoid comprised about 2 /2 inch volume didymia temperature range properties were obtained.
  • EXAMPLE IV (153 grams, avg. particle size of 350 Angstroms) was EXAMPLE IV produced in the manner described in Example 1, except the mechanical alloying time was 20 hours.'The minus 45 mesh fraction of the powder was extruded at 1900F. with a 16:1 reduction ratio to produce by 15/16 inch rectangular cross-section bar. A piece of this bar was annealed in the as-extruded condition at 2400F. for 2 hours in an attempt to produce coarse elongated grains. Again, as excess of fine grains was found.
  • Alloys that can be processed in accordance with the instant invention include those containing up to about 65% chromium, up to about 8% aluminum, up to about 8% titanium, up to about 40% molybdenum, up to 40% tungsten, up to about 20% columbium, up to about 40% tantalum, up to about 5% vanadium, up to about 15% manganese, up to about 0.5% magnesium, up to about 2% carbon, up to about 3% silicon, up to about 1% boron, up to 2%.zirconium, up to about 6% hafnium, up to about 40% iron, up to about 10% or more by volume of a dispersoid material comprising an oxide of lanthanide series metal, and the balance essentially nickel and/or cobalt.
  • the mechanically alloyed powder charge contain, by weight, about 5 to 35% chromium, at least one metal from the group of aluminum and titanium in a total amount of at least about 0.5 and up to about 13%, e.g., 0.5 to 6.5% of either or both aluminium and titanium, up to about 15% molybdenum up to about tungsten, up to about 10% columbium, up to about 10% tantalum, up to about 3% vanadium, up to about 2% maganese, up to about 2% silicon, up to about 0.75% carbon, up to about 0.1% boron, up to 1% zirconium, up to about 0.2% magnesium, up to about 35% iron and about 1 to 3%, e.g., 1.75% to about 2.5%, by volume, of dispersoid material comprising an oxide of lanthanide series metal. It is preferred that the dispersoid particles have an average particle diameter of about 20 to 2000 Angstroms, more preferably, about 50 to about 1000 Angstroms.
  • a process for achieving enhanced stress-rupture characteristics at elevated temperatures in respect of a mechanically alloyed superalloy composition containing as a dispersoid an oxide of a lanthanide series metal, whereby the alloy is capable of developing a desired structure having coarse elongated grains upon germinative grain growth treatment which comprises hot consolidating a charge of such mechanically alloyed composite superalloy powder particles and thereafter hot working the resulting hot consolidated product, the temperature of hot working and amounts of reduction being correlated such that (a) the formation of small equiaxed grains upon grain coarsening heat treatment is minimized, and (b) the formation of coarse equiaxed grains and/or cracking of the consolidated product during the hot working operation is minimized, whereby coarse elongated grains result upon subsequent heating of the shape at germinative grain growth temperature.
  • the lanthanide metal series oxide dipsersoid is of the group lanthana, didymia, rare earth oxide and ceria, the lanthana, didymia, rare earth oxides being respectively either hot forged or hot rolled within the combination of hot working temperature range and hot working reduction range given below.
  • dipsersoid material is present in an amount of about 1 to 3% by volume.
  • the dispersion-strengthened mechanically alloyed superalloy is of a composition containing up to 65% chromium, up to about 8% aluminum, up to about 8% titanium, up to about 40% molybdenum, up to 40% tungsten, up to about 20% columbium, up to about 40% tantalum, up to about 5% vanadium, up to about 15% manganese, up to about 0.5% magnesium, up to about 2% carbon, up to about 3% silicon, up to about 1% boron, up to 2% zirconium, up to about 6% hafnium, up to about 40% iron, up to about 10% or more by volume of a dispersoid material comprising an oxide of lanthanide series metal, and the balance essentially nickel and/or cobalt.
  • the dispersion-strengthened mechanically alloyed superalloy is of a composition containing about 5% to about 35% chromium, about 0.5% to about 13% of metal from the group 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 3% vanadium, up to about 2% manganese, up to about 2% silicon, up to about 0.75% carbon, up to about 0.1% boron, up to 1% Zirconium, up to about 0.2% magnesium, up to about 35% iron, and about 1 to 3% by volume of dispersoid material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Heat Treatment Of Nonferrous Metals Or Alloys (AREA)
US396204A 1973-09-11 1973-09-11 Post working of mechanically alloyed products Expired - Lifetime US3909309A (en)

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US396204A US3909309A (en) 1973-09-11 1973-09-11 Post working of mechanically alloyed products
CA207,425A CA1041882A (en) 1973-09-11 1974-08-20 Post working of mechanically alloyed products
JP49104815A JPS591779B2 (ja) 1973-09-11 1974-09-11 キカイテキゴウキンカセイヒン ノ アトカコウホウ

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0132371A3 (en) * 1983-07-22 1986-06-04 Inco Alloys International, Inc. Process for making alloys having a coarse elongated grain structure
EP0194683A1 (en) * 1985-03-13 1986-09-17 Inco Alloys International, Inc. Nickel-chromium alloys having a dispersed phase
EP0196513A1 (en) * 1985-03-13 1986-10-08 Inco Alloys International, Inc. Nickel-chromium alloys having a dispersed phase
EP0197347A1 (en) * 1985-03-13 1986-10-15 Inco Alloys International, Inc. Nickel-chromium alloy having a dispersed phase
AT399165B (de) * 1992-05-14 1995-03-27 Plansee Metallwerk Legierung auf chrombasis
US5443787A (en) * 1993-07-13 1995-08-22 Tdk Corporation Method for preparing iron system soft magnetic sintered body
US5725693A (en) * 1996-03-06 1998-03-10 Lockheed Martin Energy Systems, Inc. Filler metal alloy for welding cast nickel aluminide alloys
EP1341639A4 (en) * 2000-12-15 2005-06-15 Rolls Royce Corp SOLDERING ALLOY WITH NICKEL DIFFUSION AND METHOD FOR REPAIRING SUPERALLIAGES
CN111235567A (zh) * 2020-03-10 2020-06-05 昆明理工大学 一种稀土掺杂材料及其涂层的制备方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0035070B1 (de) * 1980-03-03 1985-05-15 BBC Aktiengesellschaft Brown, Boveri & Cie. Gedächtnislegierung auf der Basis eines kupferreichen oder nickelreichen Mischkristalls
EP0045984B1 (de) * 1980-08-08 1984-03-14 BBC Aktiengesellschaft Brown, Boveri & Cie. Verfahren zur Herstellung eines Werkstückes aus einer warmfesten Legierung
US4631082A (en) * 1985-02-20 1986-12-23 Pfizer Hospital Products Group Inc. Cobalt-chromium superalloy
US4668290A (en) * 1985-08-13 1987-05-26 Pfizer Hospital Products Group Inc. Dispersion strengthened cobalt-chromium-molybdenum alloy produced by gas atomization
CN110465666A (zh) * 2019-09-16 2019-11-19 陕西理工大学 纳米界面与超微晶粒钨合金材料的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3346427A (en) * 1964-11-10 1967-10-10 Du Pont Dispersion hardened metal sheet and process
US3494807A (en) * 1968-06-11 1970-02-10 Fansteel Inc Dispersion hardened cobalt alloy sheet and production thereof
US3660049A (en) * 1969-08-27 1972-05-02 Int Nickel Co Dispersion strengthened electrical heating alloys by powder metallurgy
US3746581A (en) * 1972-01-31 1973-07-17 Nat Nickel Co Inc Zone annealing in dispersion strengthened materials
US3749612A (en) * 1971-04-06 1973-07-31 Int Nickel Co Hot working of dispersion-strengthened heat resistant alloys and the product thereof
US3776704A (en) * 1968-03-01 1973-12-04 Int Nickel Co Dispersion-strengthened superalloys
US3814635A (en) * 1973-01-17 1974-06-04 Int Nickel Co Production of powder alloy products

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3346427A (en) * 1964-11-10 1967-10-10 Du Pont Dispersion hardened metal sheet and process
US3776704A (en) * 1968-03-01 1973-12-04 Int Nickel Co Dispersion-strengthened superalloys
US3494807A (en) * 1968-06-11 1970-02-10 Fansteel Inc Dispersion hardened cobalt alloy sheet and production thereof
US3660049A (en) * 1969-08-27 1972-05-02 Int Nickel Co Dispersion strengthened electrical heating alloys by powder metallurgy
US3749612A (en) * 1971-04-06 1973-07-31 Int Nickel Co Hot working of dispersion-strengthened heat resistant alloys and the product thereof
US3746581A (en) * 1972-01-31 1973-07-17 Nat Nickel Co Inc Zone annealing in dispersion strengthened materials
US3814635A (en) * 1973-01-17 1974-06-04 Int Nickel Co Production of powder alloy products

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0132371A3 (en) * 1983-07-22 1986-06-04 Inco Alloys International, Inc. Process for making alloys having a coarse elongated grain structure
EP0194683A1 (en) * 1985-03-13 1986-09-17 Inco Alloys International, Inc. Nickel-chromium alloys having a dispersed phase
EP0196513A1 (en) * 1985-03-13 1986-10-08 Inco Alloys International, Inc. Nickel-chromium alloys having a dispersed phase
EP0197347A1 (en) * 1985-03-13 1986-10-15 Inco Alloys International, Inc. Nickel-chromium alloy having a dispersed phase
AT399165B (de) * 1992-05-14 1995-03-27 Plansee Metallwerk Legierung auf chrombasis
US5608174A (en) * 1992-05-14 1997-03-04 Eck; Ralf Chromium-based alloy
US5443787A (en) * 1993-07-13 1995-08-22 Tdk Corporation Method for preparing iron system soft magnetic sintered body
US5725693A (en) * 1996-03-06 1998-03-10 Lockheed Martin Energy Systems, Inc. Filler metal alloy for welding cast nickel aluminide alloys
EP1341639A4 (en) * 2000-12-15 2005-06-15 Rolls Royce Corp SOLDERING ALLOY WITH NICKEL DIFFUSION AND METHOD FOR REPAIRING SUPERALLIAGES
CN111235567A (zh) * 2020-03-10 2020-06-05 昆明理工大学 一种稀土掺杂材料及其涂层的制备方法

Also Published As

Publication number Publication date
JPS5055510A (enrdf_load_stackoverflow) 1975-05-15
JPS591779B2 (ja) 1984-01-13
CA1041882A (en) 1978-11-07

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