US3824097A - Process for compacting metal powder - Google Patents

Process for compacting metal powder Download PDF

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Publication number
US3824097A
US3824097A US00316490A US31649072A US3824097A US 3824097 A US3824097 A US 3824097A US 00316490 A US00316490 A US 00316490A US 31649072 A US31649072 A US 31649072A US 3824097 A US3824097 A US 3824097A
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United States
Prior art keywords
powder
container
extrusion
compaction
density
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Expired - Lifetime
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US00316490A
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English (en)
Inventor
J Smythe
S Reichman
D Weaver
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.)
ALLEGHENY INTERNATIONAL ACCEPTANCE Corp
Federal Mogul LLC
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Federal Mogul LLC
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Publication date
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Priority to US00316490A priority Critical patent/US3824097A/en
Priority to GB5629773A priority patent/GB1404889A/en
Priority to JP48137429A priority patent/JPS5226721B2/ja
Priority to SE7316683A priority patent/SE399373B/xx
Priority to DE2362499A priority patent/DE2362499C2/de
Priority to FR7345549A priority patent/FR2210468B1/fr
Publication of US3824097A publication Critical patent/US3824097A/en
Application granted granted Critical
Assigned to CITICORP INDUSTRIAL CREDIT, INC., BOND COURT BLDG., STE. 615, 1300 E. 9TH ST., CLEVELAND, OH. 44114 reassignment CITICORP INDUSTRIAL CREDIT, INC., BOND COURT BLDG., STE. 615, 1300 E. 9TH ST., CLEVELAND, OH. 44114 SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SPECIAL METALS CORPORATION
Assigned to AL-INDUSTRIAL PRODUCTS, INC. reassignment AL-INDUSTRIAL PRODUCTS, INC. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SPECIAL METALS CORPORATION A DE CORP
Assigned to ALLEGHENY INTERNATIONAL ACCEPTANCE CORPORATION reassignment ALLEGHENY INTERNATIONAL ACCEPTANCE CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: AL- INDUSTRIAL PRODUCTS INC.
Assigned to HELLER FINANCIAL, INC. reassignment HELLER FINANCIAL, INC. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SPECIAL METALS CORPORATION
Assigned to SPECIAL METALS CORPORATION reassignment SPECIAL METALS CORPORATION RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: CITICORP INDUSTRIAL CREDIT, INC.
Assigned to SPECIAL METALS CORPORATION reassignment SPECIAL METALS CORPORATION RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: AL-INDUSTRIAL PRODUCTS, INC., A CORP. OF PA, ALLEGHENY INTERNATIONAL, INC., A CORP. OF PA
Assigned to SPECIAL METALS CORPORATION reassignment SPECIAL METALS CORPORATION RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: HELLER FINANCIAL, INC.
Anticipated expiration legal-status Critical
Assigned to CREDIT LYONNAIS NEW YORK BRANCH reassignment CREDIT LYONNAIS NEW YORK BRANCH SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SPECIAL METALS CORPORATION
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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding

Definitions

  • Various metal alloys are possessed of a metallurgical structure in the as-cast condition and are possessed of physical properties at both room and elevated temperatures that makes them very difiicult to post form to the desired shape utilizing conventional post-forming techniques.
  • Typical of such metal alloys are the so-called nickel-based superalloys which can be characterized as normally having carbide strengthening and gamma prime strengthening in their cast and wrought forms.
  • Such superalloys contain relatively large quantities of second phase gamma prime and complex carbides in a nickel-chromium gamma matrix.
  • the metal alloy in the form of a powder of controlled particle size and composition is loosely packed wtihin a ductile container which is thereafter sealedto avoid contamination of the powder particles therein and whereafter the powder is heated and densified by hot pressing or extrusion.
  • the compaction of metal alloy powders by extrusion of a ductile container filled with said powder comprises a particularly satisfactory technique for forming relatively large, elongated billets from which rotors, shafts and hubs can be fabricated for use in the hot sections of gas turbine engines and the like.
  • the loosely packed and confined powder is densified from an original density of about 60% to about theoretical density accom panied by a substantial reduction in the cross sectional area of the ductile container as well as an appreciable elongation thereof.
  • extrusion ratios of at least about 6:1 to as high as about 10:1.
  • the extrusion operation is also accompanied by an initial densification of the powder in the container by inward deformation of the rearward end thereof prior to initiation of the extrusion through the die orifice. This frequently is accompanied by a wrinkling or buckling of the container walls such that the resultant billet must be machined to an appreciable depth in order to remove the last traces of the container wall therefrom which comprises a costly operation and also is wasteful of the high cost superalloy material. It has also been observed that in some instances the densification of the powder by the extrusion process has resulted in billets of nonuniform density which incorporate local porous sections and areas of less than 100% theoretical density. The presence of such imperfections renders the compacted billet unsuitable for fabricating components requiring extremely high physical properties at the elevated service temperatures to which they are to be subjected.
  • the benefits and advantages of the present invention are achieved by a process in which the metal, metal alloy, intermetallic and/or nonmetallic material is first reduced to a finely particulated powder form having a particle size usually less than about 250 microns and thereafter the powder is loosely packed at a density of usually 60% to 70% of theoretical density within the interior of a fluid impermeable ductile container.
  • the container is preferably evacuated and thereafter sealed to avoid any contamination of the powder contents.
  • the sealed container and the powder contents thereof are subsequently heated to an elevated temperature, whereafter the container is subjected to an exteriorly applied isostatic fluid pressure of a magnitude usually above about 1000 p.s.i.
  • the preliminarily compacted powder mass and container at an elevated temperature is thereafter passed through an extrusion die in a longitudinally oriented direction at an extrusion ratio of at least about 2:1 and in a manner to effect an extrusion and an elongation of the container an a densification of the powder therein into a coherent mass approaching substantially 100% theoretical density.
  • the container encapsulating the periphery thereof is removed such as by machining or the like.
  • FIG. 1 is a longitudinal cross-sectional view of a typical container filled with metallic powder which is sealed therein preparatory to compaction in accordance with the practice of the present invention
  • FIG. 2 is a longitudinal vertical sectional view of the container and powder contents thereof after completion of the preliminary hot isostatic compaction step
  • FIG. 3 is a longitudinal vertical sectional view of the final extruded billet produced by the hot extrusion of the preliminary compacted powder mass and container of FIG. 2.
  • the process accordingly, can be advantageously employed for producing compacted billets of powdered materials of the types which are characterized as being difficult to post form in an as-cast conditions, and/ or which are difficult to machine, and/or which are of relatively high cost and/or which, in some instances, undergo madrosegregation during the post forming of solid ingots thereof, thereby preventing the attainment of optimum physical properties.
  • the reduction of metal alloys of the types enumerated in Table 1 can be conveniently and efficiently achieved by any one of the variety of known processing techniques of which the microcasting of a molten mass of the metal alloy by gas atomization constitutes a preferred method.
  • the gas atomization of a molten mass of metal can conveniently be achieved by employing apparatuses of the types described in U.S. Pat. No. 3,253,783, which is assigned to the same assignee as the present invention and the teachings of which are incorporated herein by reference.
  • the permissible oxygen content of the powder is in part determined by the specific composition of the powder material and the deleterious effects of oxides on the resultant physical properties of the compacted powder mass.
  • a high degree of precaution is necessary because of the propensity of these two elements to react with oxygen particularly at the high temperatures at which the microcasting is performed.
  • the contamination of such superalloy powders with oxides in an amount above about 200 p.p.rn.
  • the microcasting operation is usually carried out in a substantially dry inert atmosphere so that the superalloy powder has an oxygen content of less than about 100 p.p.m.
  • Particularly satisfactory results have been obtained by employing helium or commercially available argon gases which contain only minimal amounts of conventional impurities as the atomizing medium and also the atmosphere in which the solidification, collection and classification of the microcast powder is effected.
  • the individual powder particles are of substantially the same or similar alloy chemistry. In the case of mixtures of two or more dissimilar powders, a preliminary blending is effected to assure a substantially uniform distribution of the particles throughout the mass.
  • the particular shape of the individual powder particles is not critical, although superalloy powders derived from microcasting are conventionally of a spherical configuration.
  • the powder particles are also selected so as to be of an average size up to about 250 microns down to a size as small as about one micron.
  • the average particle size be controlled within a range of from about 150 microns to about 10 microns with the particles being ran- TABLE 1.NOMINAL COMPOSITIONS OF SOME NICKEL-BASED SUPERALLOYS Percent by weight Al Ti Mo W C 0 Ch B domly distributed over the aforementioned range, thereby providing for a maximum packing density of the powder within the container.
  • Loose packing densities of the powder in the container will usually range from about 60% to about 70% of theoretical density and this can be maximized for any particular powder configuration and size by further subjecting the container and its powder contents to sonic or supersonic vibrations during the filling operation.
  • a device for use in accordance with the process for compaction of metallic powers comprises an elongated container 10, as shown in FIG. 1, which is composed of a ductile fluid-impervious material, of which metals such as mild steel or stainless steel are typical.
  • the container comprises a front end plate 12, a thin-walled body section 14 and a rearward end plate 16 which are joined together by welding and which, in combination, define an elongated internal chamber 18.
  • the chamber 18, in the exemplary embodiment shown, is of a right cylindrical configuration.
  • the chamber 18 is loosely filled and packed with a metal powder 20 which is introduced through a deformable tube 22 secured such as by means of welding to the outer face of the end plate and in alignment with a port 24.
  • the filling operation is preferably performed under vacuum.
  • the deformable tube 22 can be satisfactorily crimped, such as indicated at 26, and further welded, if desired, to assure the formation of a fluid-tight seal.
  • the two-step compaction operation enables the use of containers comprised of mild steel, such as AISI Type 1010 steel, particularly when the hot isostatic compaction is performed employing a pressurized inert gas, such as argon, which prevents oxidation attack of the surface of the container at the elevated temperatures employed.
  • mild steel such as AISI Type 1010 steel
  • a pressurized inert gas such as argon
  • the filled container 10 containing the metallic powder loosely packed to a density usually ranging from about 60% to about 70% of theoretical density is placed within an autoclave in which it is adapted to be heated and subjected to an external pressure for a period of time sufiicient to effect a compaction of the metallic powder contents to a density of at least about 90% and prefer ably greater than about 98% of theoretical density.
  • a densification of the metallic powder in excess of 99% and approaching 100% theoretical density can be achieved within reasonable time periods.
  • the temperature to which the container and its powder contents are heated during the hot isostatic pressing step can range from about 1000" F. (eg. for aluminum and aluminum alloy powders) up to about 3000 F. (eg. for intermetallic compounds such as tungsten carbide).
  • the temperature is usually controlled within about 1900" F. to about 2300 F. and preferably from about 2000 F. to about 2200 F.
  • the pressure to which the container and its powder contents are subjected may range from as low as about 1000 p.s.i.
  • pressures of from about 5000 to about 15,000 p.s.i. are employed for most metal powders which, in combination with temperatures of from about 2000 to about 2200 F., provide for a substantially complete compaction of the powder within reasonable time periods of up to about "10 hours.
  • the pressure transmitting medium comprises a gas, of which any one or a variety of the inert gases can be employed for this purpose. Particularly satisfactory results are achieved utilizing argon of commercial quality as the fluid medium for app-lying pressure simultaneously and equally over the entire surface area of the container whereby the resultant compacted powder mass is of substantial uniform density throughout.
  • FIG. 2 is illustrative of a container 28 which has been reduced in size and containing a preliminarily compacted powder 30 which has been densified by the hot isostatic pressing technique.
  • the container 28 is of a reduced length and diameter in comparison to the container 10 of FIG. 1.
  • the reduction in size of the container is a direct function of the increase in density of the powder contents achieved during the hot isostatic pressing. Surprisingly, a substantially uniform increase in the wall thickness of the container is also experienced.
  • the container 28 and the preliminarily densified powder 30, while still at an elevated temperature, are directly transferred to the next extrusion step in which the container is forced through an extrusion die of reduced cross sectional area in a manner so as to effect a further densification and lateral forging of the individual powder particles, producing an elongated extruded billet indicated at 32 in FIG. 3 which is possessed of a wrought-type grain structure.
  • the extrusion of the container is facilitated by the use of a tapered nose section 34 as shown in FIG. 2 which may be separate or can be afiixed to one end of the container prior to extrusion.
  • the container 28 is oriented with its longitudinal axis aligned with the axis of the extrusion die and with the tapered nose section 34 positioned adjacent to the die orifice.
  • the extrusion step is carried out at an extrusion ratio greater than about 2:1 and preferably at extrusion ratios greater than about 3:1 up to as high as about 10:1.
  • the extrusion ratio i.e., the original cross sectional area divided by the final cross sectional area, is selected so as to produce a billet which is of substantially theoretical density and which is possessed of the desired wroughttype grain structure.
  • the specific size of the extrusion orifice is controlled so as to provide a resultant billet of a size suitable for fabricating the desired components therefrom. Because of the increased density of the powder provided by the hot isostatic pressing step, extrusion ratios can be employed which are substantially lower than those required for effecting a compaction of powder which is in a loosely-packed condition of about 60% to 70% of theoretical density.
  • the temperature of the preliminarily densified powder 30 prior to the extrusion step can vary within the temperature ranges previously described as being suitable for the hot isostatic compaction step. In the case of superalloy powders, extrusion temperatures of from about 1800 to about 2200 F. are preferred.
  • the extruded billet 32 is allowed to cool, whereafter the elongated body section, indicated at 36, is removed such as by machining or grinding from the periphery of the densified powder mass, indicated at 38, and the extruded nose section 40 and end plate similarly are removed, providing therewith an elongated billet of the desired cross sectional configuration.
  • the process for making consolidated billets from powder which comprises the steps of confining a nickelbase superalloy powder of an average particle size ranging from about one micron to about 250 microns which contains less than about 200 p.p.m. oxygen in a fluidimpermeable and sealed ductile container, heating said container and said powder therein to a first elevated temperature, subjecting the heated said container and powder to an exteriorly-applied isostatic fluid pressure for a period of time sufficient to effect a compaction of said container and said powder therein to a density of at least about 90% of theoretical density, further densifying said powder by passing the compacted said container and said powder at a second elevated temperature longitudinally through an extrusion die at an extrusion ratio of at least about 2:1 and in a manner to effect an extrusion and an elongation of said container and a compaction of said powder therein into a coherent mass approaching 10% theoretical density, and thereafter removing said container from the periphery of said mass.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Extrusion Of Metal (AREA)
US00316490A 1972-12-19 1972-12-19 Process for compacting metal powder Expired - Lifetime US3824097A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US00316490A US3824097A (en) 1972-12-19 1972-12-19 Process for compacting metal powder
GB5629773A GB1404889A (en) 1972-12-19 1973-12-05 Process for producing billets by compacting powder
JP48137429A JPS5226721B2 (enrdf_load_stackoverflow) 1972-12-19 1973-12-11
SE7316683A SE399373B (sv) 1972-12-19 1973-12-11 Forfarande for framstellning av konsoliderade, gjutna foremal av pulver
DE2362499A DE2362499C2 (de) 1972-12-19 1973-12-15 Verfahren zur pulvermetallurgischen Herstellung von Strangprßkörpern
FR7345549A FR2210468B1 (enrdf_load_stackoverflow) 1972-12-19 1973-12-19

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Application Number Priority Date Filing Date Title
US00316490A US3824097A (en) 1972-12-19 1972-12-19 Process for compacting metal powder

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US3824097A true US3824097A (en) 1974-07-16

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US00316490A Expired - Lifetime US3824097A (en) 1972-12-19 1972-12-19 Process for compacting metal powder

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US (1) US3824097A (enrdf_load_stackoverflow)
JP (1) JPS5226721B2 (enrdf_load_stackoverflow)
DE (1) DE2362499C2 (enrdf_load_stackoverflow)
FR (1) FR2210468B1 (enrdf_load_stackoverflow)
GB (1) GB1404889A (enrdf_load_stackoverflow)
SE (1) SE399373B (enrdf_load_stackoverflow)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4050143A (en) * 1974-04-19 1977-09-27 Granges Nyby Ab Method of producing dense metal tubes or the like
DE2821429A1 (de) * 1977-05-16 1978-11-30 Carpenter Technology Corp Gegenstand mit einem schwierig zu bearbeitenden substrat aus einem verdichteten metallpulver und einer duktilen plattierung
US4178178A (en) * 1976-12-01 1979-12-11 Asea Ab Method of sealing hot isostatic containers
US4259413A (en) * 1977-05-16 1981-03-31 Carpenter Technology Corporation Composite stainless steel boron-containing article
WO1981002265A1 (en) * 1980-02-13 1981-08-20 Uk Nii Container for hot extrusion of metallic powder
US4377622A (en) * 1980-08-25 1983-03-22 General Electric Company Method for producing compacts and cladding from glassy metallic alloy filaments by warm extrusion
USRE31355E (en) * 1976-06-03 1983-08-23 Kelsey-Hayes Company Method for hot consolidating powder
US4486385A (en) * 1980-03-14 1984-12-04 Nyby Uddeholm Ab Tubular composite elements processes and a pressing for their production
WO1986001196A1 (en) * 1984-08-08 1986-02-27 The Dow Chemical Company Novel composite ceramics with improved toughness
US4602952A (en) * 1985-04-23 1986-07-29 Cameron Iron Works, Inc. Process for making a composite powder metallurgical billet
GB2181745A (en) * 1985-08-28 1987-04-29 Avesta Nyby Powder Ab Hot-deformed powder metallurgy articles
WO1987004425A1 (en) * 1986-01-27 1987-07-30 The Dow Chemical Company Novel composite ceramics with improved toughness
US4748088A (en) * 1984-06-19 1988-05-31 Kloster Speedsteel Aktiebolag Tool die blank and manufacturing method thereof
GB2198749A (en) * 1986-12-12 1988-06-22 Mannesmann Ag Method of manufacturing blocks or profiled sections by extrusion
CN109789457A (zh) * 2016-09-30 2019-05-21 日立金属株式会社 Ni基超耐热合金挤出材的制造方法及Ni基超耐热合金挤出材
CN113305289A (zh) * 2021-07-29 2021-08-27 西安欧中材料科技有限公司 一种镍基粉末高温合金的平模热挤压工艺

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5132606U (enrdf_load_stackoverflow) * 1975-04-16 1976-03-10
DE3065931D1 (en) * 1980-03-03 1984-01-26 Bbc Brown Boveri & Cie Process for making a memory alloy
FR2684028B1 (fr) * 1991-11-27 1994-02-25 Centre Nal Recherc Scientifique Procede de fabrication d'une barre comprenant une ame poudreuse gainee d'une matiere metallique.
US20200030863A1 (en) * 2016-09-29 2020-01-30 Hitachi Metals, Ltd. HOT EXTRUSION-MOLDING METHOD FOR Ni-BASED SUPER HEAT-RESISTANT ALLOY AND PRODUCTION METHOD FOR Ni-BASED SUPER HEAT-RESISTANT ALLOY EXTRUSION MATERIAL

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3649257A (en) * 1970-02-18 1972-03-14 Latrobe Steel Co Fully dense consolidated-powder superalloys

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4050143A (en) * 1974-04-19 1977-09-27 Granges Nyby Ab Method of producing dense metal tubes or the like
USRE31355E (en) * 1976-06-03 1983-08-23 Kelsey-Hayes Company Method for hot consolidating powder
US4178178A (en) * 1976-12-01 1979-12-11 Asea Ab Method of sealing hot isostatic containers
DE2821429A1 (de) * 1977-05-16 1978-11-30 Carpenter Technology Corp Gegenstand mit einem schwierig zu bearbeitenden substrat aus einem verdichteten metallpulver und einer duktilen plattierung
US4259413A (en) * 1977-05-16 1981-03-31 Carpenter Technology Corporation Composite stainless steel boron-containing article
AT375574B (de) * 1980-02-13 1984-08-27 Uk Nii Sp Stalej Behaelter zum strangpressen von metallpulver
WO1981002265A1 (en) * 1980-02-13 1981-08-20 Uk Nii Container for hot extrusion of metallic powder
US4486385A (en) * 1980-03-14 1984-12-04 Nyby Uddeholm Ab Tubular composite elements processes and a pressing for their production
US4377622A (en) * 1980-08-25 1983-03-22 General Electric Company Method for producing compacts and cladding from glassy metallic alloy filaments by warm extrusion
US4748088A (en) * 1984-06-19 1988-05-31 Kloster Speedsteel Aktiebolag Tool die blank and manufacturing method thereof
WO1986001196A1 (en) * 1984-08-08 1986-02-27 The Dow Chemical Company Novel composite ceramics with improved toughness
US4602952A (en) * 1985-04-23 1986-07-29 Cameron Iron Works, Inc. Process for making a composite powder metallurgical billet
GB2181745A (en) * 1985-08-28 1987-04-29 Avesta Nyby Powder Ab Hot-deformed powder metallurgy articles
GB2181745B (en) * 1985-08-28 1990-03-21 Avesta Nyby Powder Ab A process for the production of powder-metallurgy articles
WO1987004425A1 (en) * 1986-01-27 1987-07-30 The Dow Chemical Company Novel composite ceramics with improved toughness
GB2198749A (en) * 1986-12-12 1988-06-22 Mannesmann Ag Method of manufacturing blocks or profiled sections by extrusion
GB2198749B (en) * 1986-12-12 1990-07-25 Mannesmann Ag A method of manufacturing blocks or profiled sections
CN109789457A (zh) * 2016-09-30 2019-05-21 日立金属株式会社 Ni基超耐热合金挤出材的制造方法及Ni基超耐热合金挤出材
CN113305289A (zh) * 2021-07-29 2021-08-27 西安欧中材料科技有限公司 一种镍基粉末高温合金的平模热挤压工艺

Also Published As

Publication number Publication date
JPS5024108A (enrdf_load_stackoverflow) 1975-03-15
SE399373B (sv) 1978-02-13
FR2210468B1 (enrdf_load_stackoverflow) 1980-06-06
DE2362499C2 (de) 1982-02-04
DE2362499A1 (de) 1974-06-20
JPS5226721B2 (enrdf_load_stackoverflow) 1977-07-15
FR2210468A1 (enrdf_load_stackoverflow) 1974-07-12
GB1404889A (en) 1975-09-03

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