US3620518A - Process and device for the treatment of surfaces of workpieces in an annealing furnace - Google Patents

Process and device for the treatment of surfaces of workpieces in an annealing furnace Download PDF

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Publication number
US3620518A
US3620518A US13939A US3620518DA US3620518A US 3620518 A US3620518 A US 3620518A US 13939 A US13939 A US 13939A US 3620518D A US3620518D A US 3620518DA US 3620518 A US3620518 A US 3620518A
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Prior art keywords
gas
furnace
catalyst
fuel
process according
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Expired - Lifetime
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US13939A
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English (en)
Inventor
Karl-Heinz Winter
Ottwin Krach
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Evonik Operations GmbH
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Degussa GmbH
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Priority claimed from DE19691915866 external-priority patent/DE1915866A1/de
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/20—Carburising
    • C23C8/22—Carburising of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • C21D1/763—Adjusting the composition of the atmosphere using a catalyst
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/28—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in one step
    • C23C8/30—Carbo-nitriding
    • C23C8/32—Carbo-nitriding of ferrous surfaces

Definitions

  • PAIENTEDunv 16197! 3 620, 5 1 8 sum 2 or 2 INVENTORS A3924 -/%//rz M/V/"f/P Orrw/A/ AAwc ATTORNEYS PROCESS AND DEVICE FOR THE TREATMENT OF SURFACES OF WORKPIECES IN AN ANNEALING FURNACE
  • the present application is a continuation-in-part of application Ser. No. 715,669, filed Mar. 25, 1968 now U.S. Pat. No. 3,519,257, July 7, 1970. The entire disclosure of the parent application is hereby incorporated by reference.
  • the protective gas generators in which these endothermic reactions are conducted have an additional heated reaction chamber in which a catalyst is placed in order to provide for improved decomposition of the fuel, particularly when the heavier hydrocarbon materials are used for this purpose.
  • Keitel U.S. Pat. No. 3,075,757 It has also been proposed in Keitel U.S. Pat. No. 3,075,757, to line a furnace for the bright annealing of metals with platinum or palladium and then introducing a reducing gas consisting of hydrogen or hydrogen mixed with nitrogen into the furnace.
  • An object of the present invention is to provide a process and device in which various types of gases may be formed in situ in annealing furnaces, and without the attendant formation of carbon black.
  • An important feature of the present invention resides in the use of an annealing furnace which has a catalytically active surface therein for use in the in situ formation of protective and carrier gases from fuel and oxygen.
  • Another important object is to improve such furnace and process by appropriate pretreatment of the oxygen.
  • FIG. 1 shows an annealing furnace in which the process of the present invention may be conducted
  • FIG. 2 shows a modified annealing furnace for carrying out the process in improved fashion.
  • FIG. 1 of the drawings shows an annealing furnace device of the present invention.
  • the device has an outer wall 1.
  • the inside of the furnace is heated by steel heating rods 2 and 3.
  • a gas containing muffle 4 in which there is located area 5 in which workpiece 5a is placed when it is to be processed in the furnace.
  • the atmosphere within the furnace is agitated by means of a rotating ventilator 6 which is turned by means of knob 60 which is attached to ventilator 6 by rod 6b.
  • On the inner wall 7 of the furnace there is a layer of catalyst 7a.
  • the catalyst layer can, for example, as mentioned above, be formed by placing a layer of nickel oxide on wall 7. However, if desired, another catalyst can be used, such as platinum or palladium.
  • inlet tube 8 there can be introduced into the furnace a mixture of air and fuel, such as a heavy hydrocarbon such as butane or propane.
  • a gas which can be used for carburizing the workpiece if formed. If it is desired to form a gas for carbonitriding, then ammonia can also be introduced into the furnace, simultaneously, with the hydrocarbon material.
  • catalyst preparations containing nickel generally with a content of Ni of 3 to 6 percent; but catalysts containing precious metals may also be applied, i.e., metal catalysts, preferably a nickel or a precious metal catalyst on a suitable carrier material, e.g., finely divided aluminum oxide.
  • FIG. 2 shows the presently preferred annealing furnace device of the invention wherein the process and apparatus have been substantially improved by providing for the preheating of the air for combustion.
  • the preheated air and fuel it is especially desirable to subject the preheated air and fuel to a partial process of combustion prior to contact with the catalyst lined furnace surface.
  • the primary advantage of preheating the air is to prevent the formation of carbon black.
  • the oxygen e.g. as air, is preheated to a temperature of 600 to l,600 C., preferably about 800 C. so that there is no formation of carbon black in the annealing chamber.
  • fuel e.g., hydrocarbons of one to l0 carbon atoms
  • air is supplied through conduit 12.
  • the air does not go directly into the furnace chamber but is supplied by way of air preheater 13 to mixing nozzle 14 in which a partial combustion of the gases results.
  • This partially burned gas enters into the furnace chamber and forms, after catalytic combustion on the catalyst layer 16 of the wall 18 of the an nealing furnace, the desired protective or carrier gas atmosphere.
  • liquid hydrocarbons can be employed. There can be used any of the fuel gases or liquids previously set forth.
  • additional catalyst particles 15 can be discontinuously positioned in the furnace chamber, for example, on the floor of the furnace. Most suitable is the entire space between the carrying rails 17 for the load.
  • the invention can also be carried out in such a manner than in place of the ceramic furnace lining with a catalyst coating, e.g., nickel, nickel oxide, platinum or palladium, the furnace muf fle is made of high nickel-containing, heat-resisting material whereby the high nickel-containing construction material acts partially or completely as the catalyst.
  • a catalyst coating e.g., nickel, nickel oxide, platinum or palladium
  • the protective or carrier gas is formed in the furnace during the operation of the furnace under the conditions commonly employed for such processes, i.e.,
  • the time of treatment varies between 1 and 10 hours according to the desired carbon content, depth of carburization and the strength of the nitriding layer.
  • the workpieces that may be treated during such processes in accordance with the present invention include all those types of materials that are commonly treated in such processes, such as, ferrous materials including steel and steel alloys.
  • ferrous materials including steel and steel alloys.
  • To improve hardness and resistance against wear and tear all technical parts of machinery, parts of gear, working parts, the surfaces of which may be carburized, gas carbonitrided and bright hardened, may be treated accordingly.
  • the gases that can be formed in the furnaces in accordance with the present invention include all those commonly employed in annealing furnaces, and preferably those formed in endothermic reactions.
  • a listing of the types of such gases, the precursors which are reacted to form such gases, and the catalysts to be employed in such reactions is as follows:
  • Type of gas Precursors Catalyst Carburlzing (a) C1 to C hydrocarbon (a)N10, Pt, or Pa.
  • Carbonitriding (a) C1 to Ca hydrocarbon (a) N0, Pt or Pa.
  • the preheating of the air e.g., to 800 C. can be employed with the process of example 1.
  • an apparatus including an annealing furnace adapted for the treatment therein of workpieces in an atmosphere of a protective or carrier gas, the improvement comprising an inner surface of said furnace with a layer of catalyst adapted to catalyze the formation of said gas in said furnace during said treatment, means for introducing fuel gas into said furnace, means for preheating an oxygen-containing gas, means for mixing said preheated oxygen-containing gas and said fuel gas to partially react them prior to contact with said catalytic surface and means for introducing said mixture into said furnace whereby said protective or carrier gas is formed from said fuel gas and said oxygen-containing gas.
  • catalyst is selected from the group consisting of nickel, nickel oxide, platinum and palladium.
  • the gas is selected from the group consisting of a carburizing gas, a carbonitriding gas and a bright hardening gas.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Catalysts (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
US13939A 1967-03-23 1970-02-25 Process and device for the treatment of surfaces of workpieces in an annealing furnace Expired - Lifetime US3620518A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DED0052614 1967-03-23
DE19691915866 DE1915866A1 (de) 1969-03-28 1969-03-28 Vorrichtung zur Oberflaechenbehandlung von Werkstuecken in einem Gluehofen

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4069071A (en) * 1975-04-11 1978-01-17 Societe Chimique De La Grande Paroisse, Azote Et Produits Chimiques Method for generating a reducing atmosphere for heat-treating installations
USRE29881E (en) * 1971-06-23 1979-01-16 C. I. Hayes Inc. Method of vacuum carburizing
US4216033A (en) * 1978-12-26 1980-08-05 United States Steel Corporation Method of nitriding steel
US4249965A (en) * 1978-09-19 1981-02-10 Midland-Ross Corporation Method of generating carrier gas
EP0024106A1 (de) * 1979-07-09 1981-02-25 Ford Motor Company Limited Verfahren zur Wärmebehandlung von Werkstücken aus Eisen
US4386972A (en) * 1973-10-26 1983-06-07 Air Products And Chemicals, Inc. Method of heat treating ferrous metal articles under controlled furnace atmospheres
EP0856587A1 (de) * 1997-01-29 1998-08-05 Praxair Technology, Inc. Wärmebehandlungsverfahren von Eisen-Basis-Metallprodukten in einer aktiven Atmosphäre mit höher Kohlenstoffpotential
DE102008029001B3 (de) * 2008-06-20 2009-09-17 Ipsen International Gmbh Verfahren und Einrichtung zur Wärmebehandlung von metallischen Werkstoffen
US20110042866A1 (en) * 2009-08-24 2011-02-24 Ipsen, Inc. Method and Device for Conditioning Process Gases for the Heat Treatment of Metallic Work Pieces in Industrial Furnaces

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2124573A (en) * 1936-10-21 1938-07-26 Carl I Hayes Enveloping atmosphere control
US3290030A (en) * 1963-09-21 1966-12-06 Goehring Werner Apparatus for the generation of a furnace atmosphere for the heat treatment of metals, especially of steel
US3331594A (en) * 1965-02-23 1967-07-18 North American Mfg Method and apparatus for scale free heating of metals
US3519257A (en) * 1967-03-23 1970-07-07 Degussa Process for the treatment of surfaces of workpieces in an annealing furnace

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2124573A (en) * 1936-10-21 1938-07-26 Carl I Hayes Enveloping atmosphere control
US3290030A (en) * 1963-09-21 1966-12-06 Goehring Werner Apparatus for the generation of a furnace atmosphere for the heat treatment of metals, especially of steel
US3331594A (en) * 1965-02-23 1967-07-18 North American Mfg Method and apparatus for scale free heating of metals
US3519257A (en) * 1967-03-23 1970-07-07 Degussa Process for the treatment of surfaces of workpieces in an annealing furnace

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USRE29881E (en) * 1971-06-23 1979-01-16 C. I. Hayes Inc. Method of vacuum carburizing
US4386972A (en) * 1973-10-26 1983-06-07 Air Products And Chemicals, Inc. Method of heat treating ferrous metal articles under controlled furnace atmospheres
US4069071A (en) * 1975-04-11 1978-01-17 Societe Chimique De La Grande Paroisse, Azote Et Produits Chimiques Method for generating a reducing atmosphere for heat-treating installations
US4249965A (en) * 1978-09-19 1981-02-10 Midland-Ross Corporation Method of generating carrier gas
US4216033A (en) * 1978-12-26 1980-08-05 United States Steel Corporation Method of nitriding steel
EP0024106A1 (de) * 1979-07-09 1981-02-25 Ford Motor Company Limited Verfahren zur Wärmebehandlung von Werkstücken aus Eisen
EP0856587A1 (de) * 1997-01-29 1998-08-05 Praxair Technology, Inc. Wärmebehandlungsverfahren von Eisen-Basis-Metallprodukten in einer aktiven Atmosphäre mit höher Kohlenstoffpotential
EP2135961A2 (de) 2008-06-20 2009-12-23 Ipsen International GmbH Verfahren und Einrichtung zur Wärmebehandlung von metallischen Werkstoffen unter Schutzgasatmosphäre
DE102008029001B3 (de) * 2008-06-20 2009-09-17 Ipsen International Gmbh Verfahren und Einrichtung zur Wärmebehandlung von metallischen Werkstoffen
US20090314388A1 (en) * 2008-06-20 2009-12-24 Bernd Edenhofer Method and Device for Thermal Treatment of Metallic Materials
US8313586B2 (en) 2008-06-20 2012-11-20 Ipsen International, Gmbh Method and device for thermal treatment of metallic materials
US20110042866A1 (en) * 2009-08-24 2011-02-24 Ipsen, Inc. Method and Device for Conditioning Process Gases for the Heat Treatment of Metallic Work Pieces in Industrial Furnaces
DE102009038598A1 (de) 2009-08-26 2011-03-24 Ipsen International Gmbh Verfahren und Vorrichtung zur Aufbereitung von Prozessgasen für Wärmebehandlungen von metallischen Werkstoffen/Werkstücken in Industrieöfen
EP2302081A1 (de) 2009-08-26 2011-03-30 Ipsen International GmbH Verfahren und Vorrichtung zur Aufbereitung von Prozessgasen für Wärmebehandlungen von metallischen Werkstoffen/Werkstücken in Industrieöfen
US8333852B2 (en) 2009-08-26 2012-12-18 Ipsen, Inc. Method for conditioning process gases for the heat treatment of metallic work pieces in industrial furnaces
DE102009038598B4 (de) * 2009-08-26 2017-06-22 Ipsen International Gmbh Verfahren und Vorrichtung zur Aufbereitung von Prozessgasen für Wärmebehandlungen von metallischen Werkstoffen/Werkstücken in Industrieöfen

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