US3890145A - Processes for the manufacture of tungsten-based alloys and in the corresponding materials - Google Patents

Processes for the manufacture of tungsten-based alloys and in the corresponding materials Download PDF

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Publication number
US3890145A
US3890145A US090220A US9022070A US3890145A US 3890145 A US3890145 A US 3890145A US 090220 A US090220 A US 090220A US 9022070 A US9022070 A US 9022070A US 3890145 A US3890145 A US 3890145A
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Prior art keywords
binder
process according
tungsten
mixture
carbide
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Expired - Lifetime
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US090220A
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English (en)
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Andre R Hivert
Philippe M Galmiche
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Office National dEtudes et de Recherches Aerospatiales ONERA
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Office National dEtudes et de Recherches Aerospatiales ONERA
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F42—AMMUNITION; BLASTING
    • F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
    • F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
    • F42B12/72—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the material
    • F42B12/74—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the material of the core or solid body

Definitions

  • the invention relates,
  • tungsten-based alloys i.e. heavy alloys containing at least 50% of tungsten, such alloys being particularly sought for certain industrial applications and, espe cially, for the manufacture of perforating cores for munitions, of balancing weights for aerospace engines, etc.
  • tungsten can be easily obtained in the very fine powdered state 'by simple reduction, at about 900 C, from its oxide in hydrogen.
  • the process according to the invention for the manufacture of a tungsten-based alloy, consists of sintering very fine tungsten powder mixed in the cold with a metallic binder as a powder occuring in the liquid state at the sintering temperature, the abovesaid process being characterised by the fact that this metallic binder is constituted by very fine powder, of a granulometry of the order of several microns, containing 65 to 90% of nickel (Ni), from 5 to 20% of chromium (Cr) and from 5 to 15% of phosphorus (P), the phosphorus being introduced in the form of an alloy powder containing one at least of the two other constituents of the binder and, preferably, these two other constituents, the binder then having, in this latter case, the form of a nickelbased ternary alloy of the nickel-chromiumphosphorus type whose the constituents occur within the ranges of percentages by weight indicated above.
  • the proportion by weight of the binder thus constituted, in the mixture formed by the tungsten powder supplemented with the said binder, is preferably comprised between 5 and 20% and, preferably again, between and As for the sintering treatment proper, there is preferably adopted a treatment conducted in a halogenatedhydrogenated atmosphere at a temperature which is a function of the exact composition of the final alloy and in any case greater than the fusion temperature of the metallic binder used, this sintering temperature being then, generally, between 800 and 1150C.
  • a binder of low melting point (less than or equal to 1000C) enables the enlargement of the grains of tungsten to be avoided which could result from a recrystallization at a higher temperature. This enables the fine structure of the alloy to be preserved, and consequently, its resilience.
  • the invention enables the obtaining of tungstenbased alloys whose density varies from 14 to 16.5 according to the constitution and the proportions of the metallic binder, whose hardness is comprised between 40 and 45 Rc and whose resilience is good (no crumbling on grinding and behavior similar to that of hardened steel).
  • the hardness can be increased up to Re by adding a low proportion (below or equal to 5%) of a metallic carbide selected from among the hardest and with a heat of formation greater than that of tungsten carbide CW, such as the carbides of titanium or of zirconium, or, better still, tantalum carbide on account of its density.
  • a metallic carbide selected from among the hardest and with a heat of formation greater than that of tungsten carbide CW, such as the carbides of titanium or of zirconium, or, better still, tantalum carbide on account of its density.
  • tungsten powder from one to several microns
  • metallic binder in a very fine powder(also from one to several microns) constituted by the ternary alloy Ni (77%) Cr (13%) P (10%).
  • This ternary alloy is sold commercially under the name NICROBRAZ, by the American firm Wall Colmonoy Corporation of Detroit (Michigan), and it is in the form of a powder whose granulometry is about 40 microns, i.e. well above that desired (from one to several microns).
  • EXAMPLE 1 The commercial NICROBRAZ powder (grains of 40 microns) is previously converted into a fine powder by the following process:
  • the powder obtained is supplemented with 4% of camphor by means of an alcoholic solution. After evaporation of the alcohol, the mixture is granulated on an 80 mesh metallic gauze.
  • the granulate obtained is introduced into a rubber bag of diameter mm and length 70 mm.
  • the cylinders obtained are arranged upright on plates of molybdenum covered with a fine layer of magnesium fluoride to avoid sticking.
  • the whole is placed in a partially sealed casing of chromed iron at the bottom of which there is placed a bed of 2 to 3 cm of chrome granulate (2 to 3 mm) including a small amount of bivalent chromium fluoride and of ammonium acid fluoride.
  • a chromed nickel gauze caps the parts to be sintered.
  • the box provided with its cover is placed in a vertical oven of the bell type supplied with a light current of hydrogen.
  • the program of heating is arranged so as to describe the following cycle 1. from 20 to 150C in an one-half hour,
  • the sintered parts have a density of 15.50 and a hardness of 685 Vickers (53 Rockwell C).
  • the sintered parts obtained have a density of 15.7 and a hardness of 43 Rockwell C.
  • the remainder of the manufacture is similar to the case of Example 1 except for the final sintering temperature which is brought from 950C to 990C.
  • the density of the parts obtained is 15.25 and their hardness is 46 Rockwell C.
  • EXAMPLE 4 The NICROBRAZ is replaced by a nickel alloy (74%) phosphorus (10%) chromium (16%) reduced to a powder of granulometry of 40 microns by pulverisation in a liquid state. This powder is milled under the same conditions as the NICROBRAZ of the Example 1.
  • the sequence of the process is identical with that of Example 1 and the sintered parts obtained have a density of 15.2 and a hardness of 55 Rockwell C.
  • EXAMPLE 5 There is prepared by electrolysis of a mixture of sodium phosphate and nickel oxide the compound Ni P. The latter, which is fragile, is crushed then milled as in the case of Example 1.
  • Process for the manufacture of tungsten-based alloys comprising forming a mixture of very fine tungsten powder with a metallic binder and sintering said mixture in a non-oxidizing, halogenated atmosphere, said binder occurring in the liquid state at the sintering temperature and being constituted by a very fine powder, containing as the only three constituents 65 to of nickel, 5 to 20% of chromium and 5 to 15% of phosphorus, the phosphorus being introduced in the form of an alloy powder containing one at least of the two other constituents of the binder.
  • said alloy powder contains also said two other constituents, the binder then being in the form of a nickel-based ternary alloy of the nickel-chromium-phosphorus type whose constituents are within the above-indicated ranges of percentage by weight.
  • Process according to claim 3 wherein the proportion by weight of the binder in the mixture formed by the tungsten powder supplemented with the said binder, is comprised between and 5.
  • Process according to claim 1, comprising first forming a mixture of the powders, introducing the tungsten and the constituents of the metallic binder, then cold shaping the mixture by compression in the presence of an easily removable conventional agglomerant, then removing said agglomerant by heating at a temperature at least equal to the temperature of volatisisation of said agglomerant but well below the fusion temperature of the metallic binder, and lastly carrying out the sintering.
  • Process according to claim 1, comprising adding to the mixture, in a proportion at least equal to 5%, a hard metallic carbide having a heat of formation higher than that of tungsten carbide.
  • said hard carbide is titanium carbide.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Powder Metallurgy (AREA)
US090220A 1969-10-28 1970-10-26 Processes for the manufacture of tungsten-based alloys and in the corresponding materials Expired - Lifetime US3890145A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR6936877A FR2225980A5 (enrdf_load_stackoverflow) 1969-10-28 1969-10-28

Publications (1)

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US3890145A true US3890145A (en) 1975-06-17

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US090220A Expired - Lifetime US3890145A (en) 1969-10-28 1970-10-26 Processes for the manufacture of tungsten-based alloys and in the corresponding materials

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US (1) US3890145A (enrdf_load_stackoverflow)
DE (1) DE2047143C1 (enrdf_load_stackoverflow)
FR (1) FR2225980A5 (enrdf_load_stackoverflow)
GB (1) GB1379220A (enrdf_load_stackoverflow)
IT (1) IT975521B (enrdf_load_stackoverflow)
LU (1) LU61881A1 (enrdf_load_stackoverflow)

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4698096A (en) * 1984-10-20 1987-10-06 Rainer Schmidberger Sintering process
US4777015A (en) * 1988-01-14 1988-10-11 Gte Products Corporation Process for producing tungsten heavy alloy sheet using a metallic salt binder system
US4793969A (en) * 1988-01-14 1988-12-27 Gte Products Corporation Process for producing tungsten heavy alloy sheet using high temperature processing techniques
US4800064A (en) * 1988-01-14 1989-01-24 Gte Products Corporation Process for producing tungsten heavy alloy sheet using hydrometallurgically produced tungsten heavy alloy
US4960563A (en) * 1987-10-23 1990-10-02 Cime Bocuze Heavy tungsten-nickel-iron alloys with very high mechanical characteristics
US5069869A (en) * 1988-06-22 1991-12-03 Cime Bocuze Process for direct shaping and optimization of the mechanical characteristics of penetrating projectiles of high-density tungsten alloy
US5527376A (en) * 1994-10-18 1996-06-18 Teledyne Industries, Inc. Composite shot
US5689796A (en) * 1995-07-18 1997-11-18 Citizen Watch Co., Ltd. Method of manufacturing molded copper-chromium family metal alloy article
US5713981A (en) * 1992-05-05 1998-02-03 Teledyne Industries, Inc. Composite shot
US5897962A (en) * 1993-07-16 1999-04-27 Osram Sylvania Inc. Method of making flowable tungsten/copper composite powder
WO2000010752A1 (de) * 1998-08-25 2000-03-02 Ges. Für Wolfram Industrie Mbh Giesswerkzeug für das giessen von formteilen aus nicht-eisenmetallen
US6248150B1 (en) 1999-07-20 2001-06-19 Darryl Dean Amick Method for manufacturing tungsten-based materials and articles by mechanical alloying
US6270549B1 (en) 1998-09-04 2001-08-07 Darryl Dean Amick Ductile, high-density, non-toxic shot and other articles and method for producing same
EP1080240A4 (en) * 1998-04-22 2002-06-19 Sinterfire Inc FRIABLE METAL PROJECTILES, AMMUNITION AND MANUFACTURING METHOD THEREOF
US6527880B2 (en) 1998-09-04 2003-03-04 Darryl D. Amick Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US6589310B1 (en) * 2000-05-16 2003-07-08 Brush Wellman Inc. High conductivity copper/refractory metal composites and method for making same
US6749802B2 (en) 2002-01-30 2004-06-15 Darryl D. Amick Pressing process for tungsten articles
US20040112243A1 (en) * 2002-01-30 2004-06-17 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US20040216589A1 (en) * 2002-10-31 2004-11-04 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US20050008522A1 (en) * 2001-01-09 2005-01-13 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US20050034558A1 (en) * 2003-04-11 2005-02-17 Amick Darryl D. System and method for processing ferrotungsten and other tungsten alloys, articles formed therefrom and methods for detecting the same
US6884276B2 (en) 2000-01-14 2005-04-26 Darryl D. Amick Methods for producing medium-density articles from high-density tungsten alloys
US7000547B2 (en) 2002-10-31 2006-02-21 Amick Darryl D Tungsten-containing firearm slug
US20070119523A1 (en) * 1998-09-04 2007-05-31 Amick Darryl D Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US7399334B1 (en) 2004-05-10 2008-07-15 Spherical Precision, Inc. High density nontoxic projectiles and other articles, and methods for making the same
US20100215983A1 (en) * 2009-02-20 2010-08-26 Kennametal Inc. Brazed Claddings for Cast Iron Substrates
US8122832B1 (en) 2006-05-11 2012-02-28 Spherical Precision, Inc. Projectiles for shotgun shells and the like, and methods of manufacturing the same
US9677860B2 (en) 2011-12-08 2017-06-13 Environ-Metal, Inc. Shot shells with performance-enhancing absorbers
US10260850B2 (en) 2016-03-18 2019-04-16 Environ-Metal, Inc. Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same
US10690465B2 (en) 2016-03-18 2020-06-23 Environ-Metal, Inc. Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3226648C2 (de) * 1982-07-16 1984-12-06 Dornier System Gmbh, 7990 Friedrichshafen Heterogenes Wolfram-Legierungspulver
GB2235145B (en) * 1988-12-23 1992-11-18 Royal Ordnance Plc Metal matrix composite materials
AU6044996A (en) * 1995-06-07 1996-12-30 Lockheed Martin Energy Systems, Inc. Non-lead, environmentally safe projectiles and explosives co ntainers
FR2784690B1 (fr) * 1998-10-16 2001-10-12 Eurotungstene Poudres Poudres metalliques microniques a base de tungstene et/ou de molybdene et de materiaux de transition 3d

Citations (10)

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US2762706A (en) * 1954-10-19 1956-09-11 Coast Metals Inc Low melting point alloys
US2793951A (en) * 1953-06-19 1957-05-28 Gen Electric Co Ltd Powder metallurgical process for producing dense tungsten alloys
US2864693A (en) * 1956-04-24 1958-12-16 Coast Metals Inc Brazing alloys
US2916809A (en) * 1958-06-30 1959-12-15 Donald H Schell Tungsten base alloys
US3110101A (en) * 1961-05-09 1963-11-12 Schwarzkopf Dev Company Method for welding bodies of molybdenum, tungsten and bodies of their alloys
US3116146A (en) * 1961-07-27 1963-12-31 Gen Electric Method for sintering tungsten powder
US3188203A (en) * 1957-09-03 1965-06-08 Wall Colmonoy Corp Brazing alloys
US3292255A (en) * 1964-06-25 1966-12-20 James C Marshall Brazing alloys for tungsten and molybdenum
US3300285A (en) * 1964-12-21 1967-01-24 Gen Electric Powder-metallurgical tungsten-base alloy and methods of making same
US3312539A (en) * 1964-09-11 1967-04-04 James C Marshall Brazing alloys for tungsten and molybdenum

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2793951A (en) * 1953-06-19 1957-05-28 Gen Electric Co Ltd Powder metallurgical process for producing dense tungsten alloys
US2762706A (en) * 1954-10-19 1956-09-11 Coast Metals Inc Low melting point alloys
US2864693A (en) * 1956-04-24 1958-12-16 Coast Metals Inc Brazing alloys
US3188203A (en) * 1957-09-03 1965-06-08 Wall Colmonoy Corp Brazing alloys
US2916809A (en) * 1958-06-30 1959-12-15 Donald H Schell Tungsten base alloys
US3110101A (en) * 1961-05-09 1963-11-12 Schwarzkopf Dev Company Method for welding bodies of molybdenum, tungsten and bodies of their alloys
US3116146A (en) * 1961-07-27 1963-12-31 Gen Electric Method for sintering tungsten powder
US3292255A (en) * 1964-06-25 1966-12-20 James C Marshall Brazing alloys for tungsten and molybdenum
US3312539A (en) * 1964-09-11 1967-04-04 James C Marshall Brazing alloys for tungsten and molybdenum
US3300285A (en) * 1964-12-21 1967-01-24 Gen Electric Powder-metallurgical tungsten-base alloy and methods of making same

Cited By (48)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4698096A (en) * 1984-10-20 1987-10-06 Rainer Schmidberger Sintering process
US4960563A (en) * 1987-10-23 1990-10-02 Cime Bocuze Heavy tungsten-nickel-iron alloys with very high mechanical characteristics
US4777015A (en) * 1988-01-14 1988-10-11 Gte Products Corporation Process for producing tungsten heavy alloy sheet using a metallic salt binder system
US4793969A (en) * 1988-01-14 1988-12-27 Gte Products Corporation Process for producing tungsten heavy alloy sheet using high temperature processing techniques
US4800064A (en) * 1988-01-14 1989-01-24 Gte Products Corporation Process for producing tungsten heavy alloy sheet using hydrometallurgically produced tungsten heavy alloy
US5069869A (en) * 1988-06-22 1991-12-03 Cime Bocuze Process for direct shaping and optimization of the mechanical characteristics of penetrating projectiles of high-density tungsten alloy
US5713981A (en) * 1992-05-05 1998-02-03 Teledyne Industries, Inc. Composite shot
US5897962A (en) * 1993-07-16 1999-04-27 Osram Sylvania Inc. Method of making flowable tungsten/copper composite powder
US5527376A (en) * 1994-10-18 1996-06-18 Teledyne Industries, Inc. Composite shot
US5689796A (en) * 1995-07-18 1997-11-18 Citizen Watch Co., Ltd. Method of manufacturing molded copper-chromium family metal alloy article
EP1080240A4 (en) * 1998-04-22 2002-06-19 Sinterfire Inc FRIABLE METAL PROJECTILES, AMMUNITION AND MANUFACTURING METHOD THEREOF
WO2000010752A1 (de) * 1998-08-25 2000-03-02 Ges. Für Wolfram Industrie Mbh Giesswerkzeug für das giessen von formteilen aus nicht-eisenmetallen
US6270549B1 (en) 1998-09-04 2001-08-07 Darryl Dean Amick Ductile, high-density, non-toxic shot and other articles and method for producing same
US6527880B2 (en) 1998-09-04 2003-03-04 Darryl D. Amick Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US7640861B2 (en) 1998-09-04 2010-01-05 Amick Darryl D Ductile medium- and high-density, non-toxic shot and other articles and method for producing the same
US20030172775A1 (en) * 1998-09-04 2003-09-18 Amick Darryl D. Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US7267794B2 (en) 1998-09-04 2007-09-11 Amick Darryl D Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US20070119523A1 (en) * 1998-09-04 2007-05-31 Amick Darryl D Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US20050211125A1 (en) * 1998-09-04 2005-09-29 Amick Darryl D Ductile medium-and high-density, non-toxic shot and other articles and method for producing the same
US6890480B2 (en) 1998-09-04 2005-05-10 Darryl D. Amick Ductile medium- and high-density, non-toxic shot and other articles and method for producing the same
US6248150B1 (en) 1999-07-20 2001-06-19 Darryl Dean Amick Method for manufacturing tungsten-based materials and articles by mechanical alloying
US6527824B2 (en) 1999-07-20 2003-03-04 Darryl D. Amick Method for manufacturing tungsten-based materials and articles by mechanical alloying
US6884276B2 (en) 2000-01-14 2005-04-26 Darryl D. Amick Methods for producing medium-density articles from high-density tungsten alloys
US7329382B2 (en) 2000-01-14 2008-02-12 Amick Darryl D Methods for producing medium-density articles from high-density tungsten alloys
US20050188790A1 (en) * 2000-01-14 2005-09-01 Amick Darryl D. Methods for producing medium-density articles from high-density tungsten alloys
US6589310B1 (en) * 2000-05-16 2003-07-08 Brush Wellman Inc. High conductivity copper/refractory metal composites and method for making same
US7217389B2 (en) 2001-01-09 2007-05-15 Amick Darryl D Tungsten-containing articles and methods for forming the same
US20050008522A1 (en) * 2001-01-09 2005-01-13 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US6749802B2 (en) 2002-01-30 2004-06-15 Darryl D. Amick Pressing process for tungsten articles
US20040112243A1 (en) * 2002-01-30 2004-06-17 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US6823798B2 (en) 2002-01-30 2004-11-30 Darryl D. Amick Tungsten-containing articles and methods for forming the same
US7059233B2 (en) 2002-10-31 2006-06-13 Amick Darryl D Tungsten-containing articles and methods for forming the same
US7000547B2 (en) 2002-10-31 2006-02-21 Amick Darryl D Tungsten-containing firearm slug
US20040216589A1 (en) * 2002-10-31 2004-11-04 Amick Darryl D. Tungsten-containing articles and methods for forming the same
US7383776B2 (en) 2003-04-11 2008-06-10 Amick Darryl D System and method for processing ferrotungsten and other tungsten alloys, articles formed therefrom and methods for detecting the same
US20050034558A1 (en) * 2003-04-11 2005-02-17 Amick Darryl D. System and method for processing ferrotungsten and other tungsten alloys, articles formed therefrom and methods for detecting the same
US7399334B1 (en) 2004-05-10 2008-07-15 Spherical Precision, Inc. High density nontoxic projectiles and other articles, and methods for making the same
US7422720B1 (en) 2004-05-10 2008-09-09 Spherical Precision, Inc. High density nontoxic projectiles and other articles, and methods for making the same
US8122832B1 (en) 2006-05-11 2012-02-28 Spherical Precision, Inc. Projectiles for shotgun shells and the like, and methods of manufacturing the same
US20100215983A1 (en) * 2009-02-20 2010-08-26 Kennametal Inc. Brazed Claddings for Cast Iron Substrates
WO2010096420A1 (en) * 2009-02-20 2010-08-26 Kennametal Inc. Brazed claddings for cast iron substrates
US9677860B2 (en) 2011-12-08 2017-06-13 Environ-Metal, Inc. Shot shells with performance-enhancing absorbers
US9897424B2 (en) 2011-12-08 2018-02-20 Environ-Metal, Inc. Shot shells with performance-enhancing absorbers
US10209044B2 (en) 2011-12-08 2019-02-19 Environ-Metal, Inc. Shot shells with performance-enhancing absorbers
US10260850B2 (en) 2016-03-18 2019-04-16 Environ-Metal, Inc. Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same
US10690465B2 (en) 2016-03-18 2020-06-23 Environ-Metal, Inc. Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same
US11280597B2 (en) 2016-03-18 2022-03-22 Federal Cartridge Company Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same
US11359896B2 (en) 2016-03-18 2022-06-14 Federal Cartridge Company Frangible firearm projectiles, methods for forming the same, and firearm cartridges containing the same

Also Published As

Publication number Publication date
FR2225980A5 (enrdf_load_stackoverflow) 1974-11-08
LU61881A1 (enrdf_load_stackoverflow) 1974-10-01
DE2047143C1 (de) 1976-07-22
IT975521B (it) 1974-08-10
GB1379220A (en) 1975-01-02

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