US3732091A - Method for preparing mutual dispersions of carbides and metals or alloys and novel products thereof - Google Patents

Method for preparing mutual dispersions of carbides and metals or alloys and novel products thereof Download PDF

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US3732091A
US3732091A US00051470A US3732091DA US3732091A US 3732091 A US3732091 A US 3732091A US 00051470 A US00051470 A US 00051470A US 3732091D A US3732091D A US 3732091DA US 3732091 A US3732091 A US 3732091A
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metal
carbide
dispersion
methane
subjected
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R Paris
D Thibaudon
M Roubin
J Paris
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Bpifrance Financement SA
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Agence National de Valorisation de la Recherche ANVAR
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    • 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
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/907—Oxycarbides; Sulfocarbides; Mixture of carbides
    • 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
    • C22C1/10—Alloys containing non-metals
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S75/00—Specialized metallurgical processes, compositions for use therein, consolidated metal powder compositions, and loose metal particulate mixtures
    • Y10S75/956—Producing particles containing a dispersed phase

Definitions

  • a mixed oxide, a co-precipitate of hydroxides or a mixed complex of a first metal providing the carbide of the dispersion and of a second metal providing the metal of the dispersion are subjected to a heat treatment in an enclosure.
  • the compound thus obtained is subjected, in a reducing and carburizing atmosphere containing hydrogen and methane, to thermal treatment below 1100 C. to reduce all the oxides and carburize the first metal. Heating is effected at a speed of 100 to 400 C./hour.
  • the dispersions comprise particles of single or mixed carbides uniformly distributed in the midst of elementary grains of metal. The dispersions are used in powder metallurgy.
  • the invention relates to a method for the preparation of mutual dispersions of carbides and of metals or alloys, and to the products thereof.
  • the description vw'll relate to a dispersion of carbide in the metal or a dispersion of metal in carbide.
  • the dispersions of the first of these two categories have, with respect to the base metal or alloy, strengthened mechanical properties, particularly as regards hardness and resistance to flow, especially at high temperature.
  • the metal serves as binder between the grains of a powder of carbide intended for sintering.
  • the metal serves as binder between the grains of a powder of carbide intended for sintering.
  • the invention relates also to dispersions of single or mixed carbides in metals or alloys having characteristics which make them novel industrial products.
  • the compound thus obtained is subjected, in the midst of an atmosphere both reducing and carburizing and comprising hydrogen and a hydrocarbon such as methane, to a heat treatment of which the tem- 3,732,531 Patented May 8, 1973 perature (less than 1100 C.) and the duration are selected so that the reduction of all the oxides and the carburation of the first metal are ensured, the heating being effected preferably at a speed of the order of 100 to 400 C./hour.
  • the dispersions according to the invention of carbides in metals are characterised in that they comprise particles of a single or mixed carbide distributed uniformly in the midst of elementary grains of the metal or alloy selected.
  • the dimensions of the particles of the disperse phase are of the order of 5 to 500 III/1..
  • the metal occurs localised at the junctions of the grains of carbide.
  • the dimensions of the particles before sintering are of the order of 5 to 500 mu.
  • the metallic phase be constituted by an alloy
  • a mixed oxide of metals of the second group there is employed a mixed oxide of metals of the second group.
  • this step is followed by a supplementary treatment of reduction in pure hydrogen at the same temperature for a time suificient to completely reduce the carbide of the said second metal.
  • the method according to the invention may be applied in a fixed bed or in a fluidized bed.
  • the hydrogen and the methane or other hydrocarbon arrive respectively through the pipes 1 and 2 opening into a single pipe 3 which leads the gaseous mixture inside an enclosure 4 which is heated by heating elements 5.
  • the enclosure 4 is arranged horizontally and the product 6 to be treated is stacked in a thin layer in a container 7 inside this enclosure.
  • the treatment gas comes into contact with the surface of the product 6.
  • the enclosure is arranged vertically, the product 6 forming a fiuid bed above the grid 8.
  • This device also enables working in a fixed bed, the treatment gas then passing through the layer of product 6.
  • the apparatus of FIG. 2 enables the treatment of much larger amounts of product 6 in shorter reaction times, Whether in a fixed bed or in a fluid bed, since it achieves a better contact between the product 6 and the treatment gas.
  • the duration of the step of simultaneous reduction and carburation is (in the case of treatment in a fixed bed by means of the apparatus of FIG. 1) generally of the order of 10 to 20 hours.
  • the proportions of hydrogen and of hydrocarbon of the atmosphere used during this step are respectively of the order of 99.0 to and of 1 to 10%. In practice, one adheres to approximately theoretical proportions to avoid cracking of the hydrocarbon.
  • the carburation of a mixed hydroxide or oxide accompanied by reduction of one of the metallic elements to the metallic state according to the method according to the invention is easier than a carburation of a simple oxide, always better ciystallized, hence less reactive.
  • the carbide TiC is then formed between 800 and 1000 C.
  • the hydroxide Ti(OH) or the oxide TiO can be used for the practicing of conventional technics of powder metallurgy, by subjecting them to sintering either as they are, or after having mixed them with a powder of the second metal if the proportion of carbide must be reduced in the final material.
  • EXAMPLE 1 In order to prepare a dispersion of chromium carbide in iron containing 95% by weight of iron, one commences by preparing the mixed oxalic complex obtained by syncrystallization of the complex oxalates of each of the two metals.
  • the product thus obtained is subjected to selective carburation by bringing its temperature to 900 C. at the speed of 250 C./h. in a gaseous current distributed by a mixing metering pump and constituted by hydrogen (21.80 l./h.) and by methane (0.44 l./h.), i.e. containing 2% of methane.
  • a mixing metering pump constituted by hydrogen (21.80 l./h.) and by methane (0.44 l./h.), i.e. containing 2% of methane.
  • EXAMPLE 2 In order to prepare a dispersion of chromium carbide in iron, containing 60% by weight of iron, one starts by preparing the mixed oxalic complex of the desired composition as indicated in Example 1.
  • the product thus obtained is subjected to carburation at 900 C. under conditions of temperature and gaseous fiow given in Example 2. After 16 hours of maintenance at 900 C. in the atmosphere considered, radiocrystallographic analysis reveals the presence of a hexagonal single carbide Cr Cr dispersed in the or iron.
  • EXAMPLE 3 In order to prepare a dispersion of titanium carbide in cobalt, containing 70% by weight of cobalt, one starts by preparing a co-precipitate of hydrated oxides, in the following manner: there is added simultaneously, but separately and drop by drop, an aqueous solution of 69.1 g. of cobalt nitrate Co(No 6H O and 23.2 g. of titanyl sulfate TiOSO 4H O and a three times normal solution of soda in about one litre of water stirred vigorously in a Pyrex reactor of two litres capacity. The simultaneous precipitation of the two hydroxides takes place drop by drop; the very fine precipitated obtained is filtered, washed with boiling water until disappearance of sulfate and sodium ions, and dried for 20 hours in the oven at 110 C.
  • the product thus obtained finely ground, is subjected to simultaneous reduction and carburation by bringing its temperature to 800 C. at the speed of 250 C./h. in a gaseous current constituted of hydrogen (21.80 l./h.) and of methane (1.15 l./h.), i.e. containing 5% of methane.
  • a gaseous current constituted of hydrogen (21.80 l./h.) and of methane (1.15 l./h.), i.e. containing 5% of methane.
  • radiocrystallographic analysis confirms the obtaining of a fine dispersion of titanium carbide TiC in cubic 18 cobalt.
  • the titanium carbide thus obtained at i3 00 C. is fine grained, as shown by the wide diffraction mes.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 880 C. in a gaseous current constituted by hydrogen (21.80 l./h.) and methane (0.56 l./h.) containing 2.5% of methane. After 16 hours of maintenance in the atmosphere concerned, there is obtained a fine dispersion of the carbide TiC in metallic nickel.
  • EMMPLE 5 In order to prepare a dispersion of vanadium carbide in cobalt, containing by weight of cobalt, one starts by preparing the co-precipitate of the two hydrated oxides according to the method of operation described in Example 3, by making a precipitation from a saline solution of cobalt nitrate and vanadyl sulfate with a -solution of commercial ammonia three times diluted. The precipitation having taken place, it is brought to boiling to restore it to pH 7 and to destroy the vanadate which could have formed.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 800 C. in a gaseous current of hydrogen (21.80 l./h.) and of methane (1.15 l./h.), i.e. containing 5% of methane. After 14 hours of maintenance at 800 C. in the atmosphere considered, there is obtained a fine dispersion of vanadium carbide VC in cubic p cobalt.
  • EXAMPLE 6 In order to prepare a dispersion of vanadium carbide in iron, containing 80% by weight of iron, one starts by preparing the co-precipitate of the two hydrated oxides according to the operational method described in Example 3, by precipitating from a saline solution of ferric nitrate and vanadyl sulfate with a commercial solution of ammonia diluted three times.
  • the compound thus obtained is subjected to a simultaneous reduction and carburation by bringing its temperature to 920 C. in a gaseous current of hydrogen (21.80 l./h.) and methane (0.44 l./h.), i.e. containing 2% of methane.
  • radiocrystallographic analysis shows the presence of very little or iron, of cementite Fe C and of cubic vanadium carbide VC.
  • Baking of the preceding product under hydrogen (15 l./h. approximately) enables the cementite to be destroyed and there is obtained after 14 hours of baking at 920 C. or iron, very little Fe C and the carbide VC finely dispersed.
  • a further baking for 13 h. at 920 C. under hydrogen then leads to the desired product, a dispersion of vanadium carbide in the or iron.
  • EXAMPLE 7 In order to prepare a dispersion of niobium carbide in iron, containing 70% by weight of iron, one starts by preparing an intimate mixture obtained by co-evaporation of the complex oxalates (NH [Fe(C O and 4)3[ 2 4)3]- The mixture thus obtained is subjected to a simultaneous reduction and carburation by bringing its temperature to 900 C. in a gaseous current of hydrogen (21.80 l./h.) and of methane (0.44 l./h.), i.e. containing 2% of methane. After 15 hours of maintenance at 900 C., there is obtained a dispersion of NbC carbide in 0: H011.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 950 C. in a gaseous current of hydrogen (21.50 l./h.) and of methane (0.44 l./h.), i.e. containing 2% of methane. After 15 hours of maintenance at 950 C. in the atmosphere considered, radiocrystallographic analysis indicates the presence of the solid solution of the carbides TiC and TaC dispersed in a mixture of hexagonal a cobalt and of cubic B cobalt.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 1050 C. in a gaseous current of hydrogen (21.80 l./h.) and of methane (0.22 l./h.), i.e. containing 1% of methane.
  • a gaseous current of hydrogen 21.80 l./h.
  • methane (0.22 l./h.)
  • radiocrystallographic analysis indicates the presence of the solid solution of TiC and NbC carbides, dispersed in on iron EXAMPLE 10
  • a dispersion of chromium carbide Cr C in copper containing 60% by weight of copper, one starts by preparing the starting compound i.e.
  • the compound thus obtained, finely ground, is first subjected to oxidation in air, for 12 hours at 660 C., which leads to an intimate mixture of cupric oxide CuO and of cupric chromite CuCr O
  • This mixture, finely ground, is then subjected to simultaneous reduction and carburation, by bringing its temperature to 1000" C. in a gaseous current of hydrogen (21.50 l./h.) and of methane (0.22 l./h.) i.e. containing 1% of methane.
  • radiocrystallographic analysis confirms the obtaining of a dispersion of chromium carbide Cr C in copper.
  • IEXAMPLE 11 In order to prepare a ferronickel alloy with 48% by weight of iron and 52% of nickel, containing 3% by weight of vanadium carbide finely dispersed, one commences by preparing the starting product, i.e. a coprecipitate of the three hydrated oxides according to the method of operation described in the Example 3, by making a starting precipitation from a saline solution of ferric nitrate, of nickel chloride and of vanadyl sulfate with 25% ammonia, operating at pH 7.5.
  • the starting product i.e. a coprecipitate of the three hydrated oxides according to the method of operation described in the Example 3
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 950 C. in a gaseous current of hydrogen (21.80 l./h.) and of methane (0.44 l./h.) i.e. containing 2% of methane
  • radiocrystallographic analysis shows that there has been obtained a 6 dispersion of vanadium carbide VC in the ferronickel of cubic structure with centered faces, approximating to 7 iron, of parameter 0:3.5'85 A.
  • EXAMPLE 12 In order to prepare a dispersion of 3% by weight of titanium carbide in a nickel-cobalt alloy of composition by weight Ni-10% Co, one starts by preparing the co-precipitate of the three hydrated oxides according to the method of operating described in Example 3, by effecting a precipitation from a saline solution of the chlorides of nickel and cobalt and of titanyl sulfate in suitable proportions, with three times normal soda.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its temperature to 1020 C. in a gaseous current of hydrogen (21:80 l./h.) and of methane (0.22 l./h.) i.e. containing 1% of methane.
  • a gaseous current of hydrogen 21:80 l./h.
  • methane (0.22 l./h.) i.e. containing 1% of methane.
  • radiocrystallographic analysis confirms the obtaining of a nickel-B cobalt alloy of center faced cubic structure, very close to that of nickel, containing a dispersion of titanium carbide TiC.
  • EXAMPLE 13 In order to prepare a refractory composition based on titanium carbide, containing 6% by weight of cobalt usable as binder phase in sintering, one starts by preparing a co-precipitate of the two hydrated oxides according to the operational method described in Example 3, by effecting a precipitation from an aqueous solution of titanyl sulfate and of cobalt chloride in suitable proportions, with 25% ammonia. During the whole of the operation the pH must not exceed 8.
  • the compound thus obtained is subjected to simultaneous reduction and carburation by bringing its tem perature to 1030 C. in a current of hydrogen (21.80 l./h.) and of methane (0.22 l./h.) i.e. containing 1% of methane. After 20 hours of maintenance at 1030 C. in the atmosphere considered and cooling, there is obtained a grey-black powder. Radiocrystallographic analysis confirms the presence of titanium carbide TiC and of a binding phase of center faced cubic fi-cobalt.
  • the invention is in no way limited to those of its methods of application, nor to those of its methods of production of its various parts, which have been more particularly indicated; it embraces, on the contrary, all variations.
  • Process of preparing a dispersion of at least one carbide in a metallic base comprising subjecting at least one first metal from which the carbide is to be for-med selected from the group consisting of Ti, V, Nb, Ta and Cr, and at least one second metal selected from the group consisting of Fe, Co, Ni, Cu, Zn, Cd, Ag, Sn, Pb, Bi, Ge and Tl, said metals being in the form of a coprecipitate of hydroxides or a mixed complex thereof in an atmosphere of hydrogen and hydrocarbon to a temperature sufficient to permit simultaneous reduction and carbidization of said coprecipitate or mixed complex and less than 1100 C., for a time sufiicient to achieve the reduction of all the oxides and the carbidization of said first metal.

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US00051470A 1969-07-04 1970-07-01 Method for preparing mutual dispersions of carbides and metals or alloys and novel products thereof Expired - Lifetime US3732091A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4274877A (en) * 1975-07-04 1981-06-23 Johnson, Matthey & Co., Limited Metal powders
WO1997003776A1 (fr) * 1995-07-17 1997-02-06 Westaim Technologies Inc. Poudres composites
WO1997046497A1 (fr) * 1996-06-04 1997-12-11 Omg Americas Poudre de carbure metallique et de metal du groupe viii et sa preparation

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4434393A1 (de) * 1994-09-27 1996-03-28 Norddeutsche Affinerie Verfahren zum Herstellen eines dispersoidhaltigen Kupferpulvers und derartiges Kupferpulver

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4274877A (en) * 1975-07-04 1981-06-23 Johnson, Matthey & Co., Limited Metal powders
WO1997003776A1 (fr) * 1995-07-17 1997-02-06 Westaim Technologies Inc. Poudres composites
WO1997046497A1 (fr) * 1996-06-04 1997-12-11 Omg Americas Poudre de carbure metallique et de metal du groupe viii et sa preparation
US5746803A (en) * 1996-06-04 1998-05-05 The Dow Chemical Company Metallic-carbide group VIII metal powder and preparation methods thereof
US6007598A (en) * 1996-06-04 1999-12-28 Omg Americas, Inc. Metallic-carbide-group VIII metal powder and preparation methods thereof

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JPS497285B1 (fr) 1974-02-19
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