WO2012035900A1 - Élément fer/acier ayant une couche d'un composé de l'azote et son procédé de fabrication - Google Patents

Élément fer/acier ayant une couche d'un composé de l'azote et son procédé de fabrication Download PDF

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WO2012035900A1
WO2012035900A1 PCT/JP2011/067425 JP2011067425W WO2012035900A1 WO 2012035900 A1 WO2012035900 A1 WO 2012035900A1 JP 2011067425 W JP2011067425 W JP 2011067425W WO 2012035900 A1 WO2012035900 A1 WO 2012035900A1
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compound layer
treatment
nitrogen compound
layer
nitrogen
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知義 小西
芳宏 池田
正昭 別府
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日本パーカライジング株式会社
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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
    • C23C8/80—After-treatment
    • 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
    • C21D1/06—Surface hardening
    • C21D1/09—Surface hardening by direct application of electrical or wave energy; by particle radiation
    • C21D1/10—Surface hardening by direct application of electrical or wave energy; by particle radiation by electric induction
    • 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
    • C21D1/34—Methods of heating
    • C21D1/42—Induction heating
    • 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
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C23C8/10—Oxidising
    • C23C8/12—Oxidising using elemental oxygen or ozone
    • C23C8/14—Oxidising of ferrous surfaces
    • 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
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • 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
    • C23C8/40—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 liquids, e.g. salt baths, liquid suspensions
    • 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
    • C23C8/40—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 liquids, e.g. salt baths, liquid suspensions
    • C23C8/42—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 liquids, e.g. salt baths, liquid suspensions only one element being applied
    • C23C8/48—Nitriding
    • C23C8/50—Nitriding 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite
    • 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
    • C21D2221/00—Treating localised areas of an article
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present invention relates to a hardened steel material used as a mechanical structural component having excellent mechanical strength such as surface pressure strength, wear resistance, bending fatigue strength, a manufacturing method thereof (composite heat treatment method), and a processing liquid thereof. .
  • nitriding treatment including soft nitriding treatment
  • carburizing and quenching induction hardening, etc.
  • induction hardening etc.
  • a compound layer made of nitride formed on the outermost surface by nitriding treatment is known to have excellent sliding properties, wear resistance, and high seizure resistance (hereinafter referred to as nitrogen compound).
  • nitrogen compound high seizure resistance
  • Called layer effect I in general, nitriding treatment is inferior in surface pressure strength, fatigue strength, etc. compared to carburizing quenching and induction quenching. For example, when a roller pitching test is performed, the nitrogen compound layer peels from the steel substrate. There is a case.
  • the nitrogen compound layer was widely believed to have a negative effect in fatigue tests at high surface pressures exceeding 2 GPa.
  • the present inventors have found that this factor is not in the compound layer itself, but because the hardened layer depth of the substrate supporting the compound layer is shallow. In other words, the nitriding unit alone has insufficient the depth of the hardened layer immediately below it in order to make full use of the good slidability of the outermost compound layer.
  • a steel material containing nitrogen has a finer martensite structure obtained after quenching than a steel material not containing nitrogen, so that the hardness is increased, and the hardening depth is increased by improving the hardenability.
  • the nitriding treatment can also be used as a nitrogen diffusion pretreatment for forming a nitrogen diffusion layer for improving hardenability (hereinafter referred to as effect II by forming a nitrogen compound layer). That is, the characteristics that can be obtained by using this effect II are not due to the action of the nitrogen compound layer itself, but due to the action of diffused nitrogen in the steel material immediately below the nitrogen compound layer generated when the nitrogen compound layer is formed.
  • the nitrogen-containing martensite structure obtained by quenching may have temper softening resistance, high surface pressure strength due to resistance to crack initiation / growth, and high fatigue strength in addition to the above-described high hardness and hardenability improvement. Are known.
  • the quenching temperature needs to be at least the temperature Ac3 transformation point at which an austenite structure is formed, and is usually selected from a temperature range of 850 to 1200 ° C.
  • the nitrogen compound layer formed at a nitriding temperature of 570 ° C. is a combination of iron and nitrogen.
  • the nitrogen compound layer undergoes oxidation and decomposes. It is released as a gas and the nitrogen compound layer disappears. This has been reported for a long time (Non-Patent Document 1).
  • the combined heat treatment technique by nitriding and quenching usually uses only the effect II of the nitrogen diffusion layer obtained by nitriding, and does not use the effect I of the nitrogen compound layer formed by nitriding. That is, the nitrogen compound layer does not stop disappearing during quenching, which is a subsequent process of nitriding.
  • this technology for example, the composite heat treatment disclosed in Patent Documents 1 to 5.
  • Patent Document 6 discloses a composite heat treatment method in which a nitriding treatment is performed at a temperature of 600 ° C. or higher to form a nitrogen compound layer having a thickness of 5 ⁇ m or less, followed by induction hardening to obtain a quenched member having a nitrogen compound layer having a thickness of 2 ⁇ m or less. ing.
  • the reason why the nitriding conditions are set to a high temperature of 600 ° C or higher in this technology is that higher concentrations of nitrogen can be expected to diffuse deeper into the steel, but the nitrogen compound layer obtained at a nitriding temperature exceeding 600 ° C has a hardness. Is a nitrogen compound layer having a low effect I. That is, the present technology also expects only the effect II by the nitrogen compound layer, and the remaining nitrogen compound layer of 2 ⁇ m or less may be omitted.
  • Patent Document 7 discloses this.
  • Patent Document 8 to be used for both effects I and II, a hard nitride layer is formed on the surface of a steel material, and further, Ti, Zr, Hf, V, Nb, Ta, Cr, W are formed thereon.
  • Patent Document 8 discloses a hardened steel member in which an inorganic compound layer containing at least one metal oxide selected from the group consisting of Mo, Al and Al is formed.
  • Patent Documents 7 and 8 describe a steel material that combines a deep hardening depth and a nitrogen-containing compound layer by covering a protective film so that the compound layer is not oxidized or decomposed during induction hardening after forming a nitrogen compound layer by nitriding treatment. Although both of these methods are to be manufactured, both methods are to coat the protective film from the treatment liquid by coating or dipping, and are not good at uniform coating on complicated shapes such as gear tooth surfaces. There has been a problem that the compound layer may be lost without being oxidized after quenching.
  • Patent No. 3193320 Japanese Patent No. 3327386 Japanese Patent No. 3145517 JP-A-7-90364 JP 2007-154254 A JP 2007-77411 A JP 58-96815 Heat treatment Vol.16 No.44P206 Showa 51 JP 2008-038220
  • the present invention ensures that the nitrogen compound layer remains uniformly even for complicated shapes such as gear tooth surfaces (for example, machine structural parts) and also ensures the formation of fine martensite. It is an object of the present invention to provide a means capable of imparting mechanical strength such as excellent surface pressure strength, wear resistance and bending fatigue strength to the complicated shape after quenching.
  • the present invention provides a dense oxide layer as a compound layer protective film having a function of preventing oxidative deterioration of a nitrogen compound layer that occurs during induction hardening in a surface layer as a method for uniformly leaving a nitrogen compound layer in advance. It is formed on the top. This ensures that an oxide layer having antioxidation ability is uniformly formed on the nitrogen compound layer regardless of the part shape, and as a result, ensures that the nitrogen-containing compound layer obtained after high-frequency heating remains uniform. Can do. Furthermore, since the thickness of the formed oxide layer is 0.1 to 5 ⁇ m, a sufficient cooling rate can be achieved at the time of quenching, thereby ensuring the formation of fine martensite.
  • the oxide layer is formed at 600 ° C. or lower, it is possible to prevent the nitrogen compound layer from thermally decomposing at the same time as the oxidation and desorbing nitrogen into the gas phase atmosphere and affecting the crystal structure of the nitrogen compound layer. it can.
  • a nitrogen compound layer formed by nitriding with a hardness of HV550 or more and having a thickness of 1 ⁇ m or more remains on the surface layer, and the hardness exceeds HV550 including a fine martensite structure containing nitrogen below the layer. It is possible to obtain a steel material having a distribution region of 200 ⁇ m or more in distance from the surface.
  • the invention is as follows.
  • the present invention (1) is a method for subjecting a steel material to a combined composite heat treatment of nitriding treatment and induction hardening treatment, on the nitrogen compound layer formed on the steel by nitriding treatment before the induction hardening treatment after nitriding treatment.
  • the condition is such that a nitrogen compound layer having a hardness of HV550 or more and 1 ⁇ m or more remains on the surface of the steel material.
  • induction hardening is performed.
  • the present invention (2) is the method according to the invention (1), characterized in that the treatment time in the induction hardening process is 5 seconds or less and the maximum temperature reached is 750 to 860 ° C.
  • Particularly suitable steel materials under these conditions are carbon steel materials for machine structures (S20C to S58C, especially S45C, S40C, S50C) and chromium molybdenum steel materials (SCM415 to 445, 822, especially SCM435, SCM440, SCM445). .
  • the oxide layer is oxidized in an aqueous solution, immersed in an oxidizing molten salt bath, oxidized in an oxidizing gas atmosphere, and a nitrogen compound layer and an oxide layer are simultaneously formed.
  • a nitrogen compound layer having a hardness of HV550 or more and 1 ⁇ m or more obtained by the method of any one of the inventions (1) to (3) remains on the surface layer, and nitrogen is contained below the layer.
  • the steel member is characterized in that a hardness distribution region exceeding HV550 including a fine martensite structure is present at a distance of 200 ⁇ m or more from the surface.
  • a dense oxide layer as a compound layer protective film having a function of preventing oxidative deterioration of a compound layer that occurs during induction quenching on the surface layer as a method of leaving the nitrogen compound layer uniformly is previously formed on the nitrogen compound.
  • the film it is possible to effectively suppress oxidative decomposition of the nitrogen compound layer due to subsequent induction hardening.
  • the thickness of the formed oxide layer is 0.1 to 5 ⁇ m, a sufficient cooling rate can be achieved at the time of quenching, thereby ensuring the formation of fine martensite. be able to.
  • the oxide layer is formed at 600 ° C. or lower, the desorption of nitrogen into the gas phase atmosphere due to the thermal decomposition of the nitrogen compound layer that occurs simultaneously with the oxidation or the crystal of the nitrogen compound layer The influence on the structure can also be prevented.
  • a nitrogen compound layer having a hardness of HV550 or more and a thickness of 1 ⁇ m or more formed by nitriding remains on the surface layer, and a HV550 including a fine martensite structure containing nitrogen is formed below the layer.
  • processing temperature quenching temperature
  • the treatment method for further forming the oxide layer oxidation treatment in an aqueous solution after nitriding treatment, immersion treatment in an oxidizing molten salt bath, oxidation treatment in an oxidizing gas atmosphere , Oxynitridation oxynitride simultaneous treatment in which a nitrogen compound layer and an oxide layer are formed simultaneously
  • the oxidation treatment consisting of the group consisting of the above is selected, the surface layer side of the nitrogen compound layer is transferred to an oxide layer containing magnetite and / or lithium iron oxide.
  • the oxide layer containing magnetite and / or lithium iron oxide has high thermal stability, good adhesion to the nitrogen compound layer, and is dense and uniform. It has the effect of preventing the oxidation of nitrogen compounds.
  • steel members whose hardenability is improved by the diffused nitrogen can obtain a deep hardening depth and high hardness by induction hardening, so that the surface pressure strength, wear resistance, and bending fatigue strength are high. It can be suitably used for machine structural parts that require strength.
  • the steel material to which the present invention is applied is not particularly limited, and examples thereof include carbon steel, low alloy steel, medium alloy steel, high alloy steel, cast iron and the like.
  • a preferable material in terms of cost is carbon steel, low alloy steel, or the like.
  • carbon steel for machine structural use (S20C to S58C) is suitable as carbon steel, and nickel chrome steel (SNC 236 to 836), nickel chrome molybdenum steel (SNCM 220 to 815), chrome, etc. as low alloy steel.
  • Molybdenum steel (SCM 415 to 445, 822), chromium steel (SCr 415 to 445), manganese steel for mechanical structure (SMn 420 to 443), manganese chrome steel (SMnC 420, 443) and the like are suitable.
  • a tempered steel material H material
  • a tempered steel material that has not been tempered and remains in a ferrite-pearlite structure
  • alloy steel tends to have higher surface hardness
  • a sufficiently deep hardening depth can be obtained even with carbon steel because of the effect of improving the hardenability of effect II by nitrogen.
  • due to the effect II by nitrogen it is not always necessary to use tempered steel, and sufficient mechanical strength can be obtained even with non-tempered steel having a ferrite-pearlite structure.
  • the nitrogen compound layer on the surface of the steel material is obtained by a surface hardening treatment that diffuses active nitrogen on the surface of the steel material to generate a hard and stable nitride.
  • a nitrogen compound layer it is usually composed mainly of Fe as a base material component, and a nitride containing Ti, Zr, Mo, W, Cr, Mn, Al, Ni, C, B, Si, etc. It is preferable that it is a layer.
  • a nitrogen compound layer having an effect I such as salt bath nitriding treatment such as tuftride treatment, isonite treatment, and pulsonite treatment, gas nitriding, gas soft nitriding treatment, plasma nitriding treatment, and nitrogen immediately below it. Any nitriding method can be used as long as a diffused region is formed.
  • the nitriding heat treatment temperature for forming the nitrogen compound layer for achieving the effect I is preferably 600 ° C. or lower, more preferably 580 ° C. or lower, and further preferably 570 ° C. or lower. Although the thickness of the nitrogen compound layer obtained at a processing temperature exceeding 600 ° C.
  • the thickness of the nitrogen compound layer obtained by nitriding before induction quenching is not particularly limited, but it is usually sufficient if it is formed with a thickness of 1 to 30 ⁇ m, more preferably 3 to 20 ⁇ m, and even more preferably 5 ⁇ 15 ⁇ m.
  • the thickness of the nitrogen compound layer remaining after the oxidation treatment depends on the method and conditions of the subsequent oxidation treatment.
  • a nitriding condition of 1 ⁇ m or more, more preferably 2 ⁇ m or more, and further preferably 3 ⁇ m or more is selected to form a nitrogen compound layer.
  • oxynitriding conditions are selected such that the thickness of the nitrogen compound layer formed after oxynitriding treatment is in the same range as above (1 ⁇ m or more, more preferably 2 ⁇ m or more, and further preferably 3 ⁇ m or more).
  • a nitrogen compound layer is formed.
  • a dense oxide layer as a nitrogen compound layer protective film having a function of preventing oxidative deterioration of the nitrogen compound layer that occurs during induction hardening is preliminarily prior to induction hardening, a nitrogen compound in advance. It forms on the surface layer side.
  • a 0.1 to 5 ⁇ m oxide layer mainly composed of magnetite and / or lithium iron oxide formed at 600 ° C. or lower on the nitrogen compound layer of the present invention is within 5 seconds thereafter.
  • the temperature as oxidation treatment of the nitrogen compound layer performed before induction hardening is 600 ° C. or less, more preferably 590 ° C.
  • the lower limit is not particularly limited, but is preferably, for example, 400 ° C., and the thickness of the oxide film is preferably 0.1 to 5 ⁇ m, more preferably 0.5 to 3 ⁇ m.
  • the thickness of the oxide film When the thickness of the oxide film is less than 0.1 ⁇ m, the ability to prevent oxidation by subsequent induction hardening becomes insufficient. If the thickness of the oxide film exceeds 5 ⁇ m, the hardenability of the steel body by induction hardening is hindered, which is not preferable.
  • the formation of an oxide film at a temperature exceeding 600 ° C. according to the present invention causes the nitrogen compound layer formed simultaneously with oxidation by exceeding the eutectoid temperature (Ac1 transformation point) 590 ° C. in the iron-nitrogen binary alloy system. Desorption of nitrogen into the gas phase atmosphere due to thermal decomposition becomes remarkable, and the crystal structure of the nitrogen compound layer is also affected.
  • the hardness of the nitrogen compound layer is reduced, which is not preferable.
  • the oxide film becomes thicker and the internal stress generated in the film becomes higher.
  • the oxide film exceeds the rupture stress of the oxide, the oxide film is cracked or peeled off.
  • the oxide film as the protective film is exposed to rapid temperature changes such as cooling after the oxidation treatment as the protective film and heating and cooling during the subsequent induction hardening.
  • the film thickness be within 5 ⁇ m as the upper limit of the thickness of the oxide film.
  • this oxide layer is formed on the nitrogen compound layer by, for example, an oxidation treatment in an aqueous solution, an oxidation treatment in an oxidizing gas atmosphere, or an immersion treatment in an oxidizing molten salt bath.
  • the iron oxide is a black oxide film mainly composed of magnetite (Fe 3 O 4 ), and the nitride on the surface layer side becomes an oxide on the iron nitrogen compound layer obtained by nitriding treatment. Formed by.
  • Oxidation treatment in an aqueous solution means oxidation by immersion in an aqueous solution containing an oxidizing agent (for example, sodium nitrate, sodium nitrite, sodium dichromate, sodium peroxide) or an electrochemical potential in the anode direction. Oxidation by operation is mentioned.
  • the main component is a dense magnetite of about 0.1 to 2 ⁇ m on a nitrogen compound by alkali conversion oxidation treatment at 130 to 150 ° C, which is mainly composed of caustic soda and sodium nitrate, which are known as black dyeing of iron.
  • this oxide layer can also be formed on the nitrogen compound layer, and effectively acts as a protective film for preventing oxidative decomposition of the compound layer from induction hardening in the present invention.
  • oxidation treatment in an oxidizing gas atmosphere homotreatment (steam oxidation treatment), oxidation treatment in an oxidizing gas containing carbon dioxide gas, etc. can be applied.
  • the temperature is 450 to 550 ° C.
  • AB1 salt bath (Nihon Parkerizing Technical Bulletin, 1992, page 19) containing sodium nitrate and sodium nitrite as oxidizing agents may be used as the oxidative molten salt bath, at 350 to 450 ° C for 30 seconds to 60 minutes.
  • an oxide layer mainly composed of magnetite having a uniform and dense black appearance within a range of 0.1 to 1 ⁇ m is obtained on the nitrogen compound.
  • the above oxidation method is also used as a method for improving the corrosion resistance and wear resistance of steel, and the obtained oxide film made of magnetite is characterized by good adhesion to the steel substrate and being dense and uniform. is there.
  • the nitrogen compound layer After forming the nitrogen compound layer, it is possible to oxidize the surface of the nitrogen compound layer by heating and holding in the air atmosphere, but the oxidation rate at 600 ° C or lower is slow, and the film thickness of the resulting oxide film Is difficult to control, It is inadequate as a protective layer at the time of induction hardening in the present invention, such as poor adhesion and falling off of the oxide film during rapid cooling.
  • the presence of magnetite in the obtained oxide film can be investigated, for example, by crystal structure analysis by X-ray diffraction. Further, the thickness of the oxide film can be measured from the cross-sectional observation.
  • an oxide layer on the nitrogen compound formed simultaneously with the nitriding treatment that occurs during a specific nitriding treatment can also be used.
  • Isonite LS Nihon Parkerizing Technical Report, page 39, 2003
  • iron oxide containing lithium is about 0.5 to 5 ⁇ m above the nitrogen compound layer. It is formed.
  • this oxide layer is different from magnetite, the iron oxide containing lithium has the same antioxidant ability as magnetite and effectively prevents oxidation of the nitrogen compound layer by subsequent induction hardening. Function as.
  • oxygen compounding for several hours at 500 to 570 ° C. by adding air, water vapor, carbon dioxide gas or the like as an oxidizing gas to gas nitriding, the outermost surface is treated.
  • this oxide layer also functions as a compound layer protective film that prevents oxidation of the nitrogen compound layer by subsequent induction hardening.
  • the oxide layer as the nitrogen compound layer protective film of the present invention is mainly composed of magnetite and / or lithium iron oxide, is dense and has good adhesion, and has a cross-sectional thickness of 0.1 to 5 ⁇ m. And If the thickness is less than 0.1 ⁇ m, the effect is not sufficiently exhibited.In the case of an oxide layer exceeding 5 ⁇ m, the antioxidant effect is saturated and the nitrogen compound layer is excessively transferred to a dense oxide layer. It is not preferable because it loses.
  • the lower limit of the thickness is more preferably 0.2 ⁇ m, still more preferably 0.5 ⁇ m.
  • the upper limit of the thickness of the oxide layer is more preferably 3 ⁇ m and even more preferably 1.5 ⁇ m.
  • the greatest merit of the method of forming an oxide layer for protecting the nitrogen compound layer is that a protective film can be uniformly formed at a low cost by a simple means. As a result, the nitrogen-containing compound layer obtained after high-frequency heating can remain uniformly. However, in the oxidation treatment after the nitriding treatment, the thickness of the nitrogen compound layer corresponding to the formation of the oxide layer is reduced, so that a nitrogen compound layer having a thickness greater than the film thickness lost by the oxidation treatment may be formed in advance by nitriding treatment. Necessary.
  • induction hardening is performed after forming an oxide layer for protecting the nitrogen compound layer.
  • the optimum quenching heating conditions differ depending on the steel material type, the structure before quenching and the mass effect, but even when induction quenching is performed after forming the nitrogen compound layer of the present invention, the optimum quenching heating temperature Is slightly different depending on the steel grade.
  • the quenching temperature can be lowered as compared with normal induction quenching (without nitriding in advance), but the lower limit temperature is 750 ° C., for example.
  • the application upper limit temperature of the quenching temperature is selected to be not less than the upper limit temperature at which the structure of the steel material can be austenitized by heating, and the antioxidant film can protect the nitrogen compound layer (for example, not more than 860 ° C.).
  • the upper limit temperature at which an oxide anti-oxidation film can be applied varies depending on the steel material, and the higher the nitrogen compound layer contains more elements that form stable compounds with N, such as Cr, Al, Mo, V, etc. Can be set.
  • the optimum quenching temperature is selected according to the steel grade of the steel part to be used, the structure before quenching, the size thereof, and the nitrogen concentration of the nitrogen diffusion layer that differs depending on the nitriding treatment conditions. Regardless of the steel material type, the structure before quenching or the size of the member itself, it is not preferable that the heating time during induction quenching exceeds 5 seconds at the maximum. A preferable heating time is 0.3 to 3 seconds, and more preferably 1 to 2 seconds.
  • the induction hardening temperature commonly used in S45C steel exceeds 900 ° C, but the heating temperature during quenching in the present invention can be 860 ° C or less, and the induction hardening heating temperature performed after the nitriding treatment of the present invention Is preferably 750 to 860 ° C, more preferably 780 to 830 ° C.
  • the heating time is more preferably 0.3 to 3 seconds, and further preferably 1 to 2 seconds.
  • heating at an induction quenching temperature of 750 ° C. or lower has a nitrogen diffusion layer, at this temperature, it is not sufficiently austenitized and thus quenching is insufficient.
  • heating at the time of induction hardening exceeds 860 ° C.
  • the nitrogen compound layer is sufficiently suppressed from oxidation and decomposition even when the atmosphere during high-frequency heating is in the air.
  • the atmosphere during high-frequency heating may be a vacuum atmosphere, an inert atmosphere with argon gas or nitrogen gas, a low oxygen atmosphere, a hydrocarbon-based reducing atmosphere, an ammonia gas atmosphere, or the like. it can.
  • the heating temperature applicable to the present invention is higher, and the heating time may be set longer.
  • a multistage temperature raising method including preheating can be appropriately performed. After quenching by high frequency heating, a tempering treatment may be performed under appropriate conditions in the same manner as a normal quenching technique.
  • the oxide layer for the purpose of protecting the compound layer may or may not be removed, and can be selected as necessary.
  • the removal of the oxide layer can be easily performed because the hardness is lower than that of the compound layer, and can be appropriately performed by, for example, lapping treatment, emery paper polishing, buff polishing, shot blasting, shot pinning, grinding polishing, and the like.
  • the nitrogen compound layer remains by the compound layer protective film of the oxide layer of the present invention, but the nitrogen compound layer does not necessarily remain 100% of the compound layer state before the high frequency heating, and the minimum film thickness is 1 ⁇ m. It is sufficient if the above compound layer thickness is secured. More preferably, it is 2 ⁇ m or more, and more preferably 3 ⁇ m or more (the upper limit is not particularly limited, but is, for example, 30 ⁇ m).
  • the upper limit is not particularly limited, but is, for example, 30 ⁇ m.
  • another layer a belt-like layer in which untransformed austenite remains, may be formed between the nitrogen compound layer and the fine martensite layer during induction hardening.
  • This retained austenite-containing layer tends to be thicker as the induction hardening temperature is higher.
  • the induction hardening heating temperature is set to 750 to 860 ° C. for S45C steel
  • the retained austenite-containing layer having a thickness of 0 to 5 ⁇ m is used. Appears.
  • a carbon steel material for mechanical structure (S20C to S58C, especially S45C, S40C, S50C) or a chromium molybdenum steel material (SCM415 to 445, 822, particularly SCM435, SCM440, SCM445) is used as the steel material
  • SCM415 to 445, 822 particularly SCM435, SCM440, SCM445
  • the residual austenite-containing layer may have a hardness of less than HV550, but the presence of this layer does not deteriorate the mechanical properties of the steel member.
  • the reason for this is that the hardness is reduced to HV550 due to the fact that it is thin in the first place and easily undergoes structural transformation under severe load conditions in the high surface pressure and temperature range exceeding 200 ° C, and changes to a bainite or martensite structure. This is because it will surpass.
  • the upper limit of the hardness is not particularly limited because the harder the better, but for example, HV900.
  • the hardness of the nitrogen compound layer is HV630 or higher in terms of Vickers hardness (the upper limit is not particularly limited because the harder is better, but it is, for example, HV1300), and hard including a fine martensite structure It is possible to obtain a steel material having a hardness distribution in which the hardness region (hardened layer depth) exceeding the HV550 of the layer is 200 ⁇ m or more, preferably 400 ⁇ m or more, more preferably 600 ⁇ m or more from the surface.
  • the upper limit is not particularly limited, but is, for example, HV1100.
  • the upper limit is not particularly limited, but is, for example, 5.0 mm.
  • a hardened layer depth of 0.2 to 1.5 mm is usually obtained although it varies slightly depending on the shape and size of the member.
  • the machine part subjected to the treatment of the present invention has high slidability and seizure resistance due to the nitrogen compound layer formed on the outermost surface, and high temper softening resistance due to the nitrogen-containing fine martensite structure. It has crack initiation / crack growth resistance, surface pressure resistance, high fatigue strength, and deep cure depth.
  • the hardening temperature can be lowered as described above due to the effect II.
  • This is extremely advantageous in terms of thermal deformation and cracking, and enables a significant reduction in the post-cutting process for adjusting the dimensional accuracy performed after general induction hardening or carburizing and quenching.
  • the steel material to which the present invention is applied is not necessarily required to use tempered steel because of the effect of improving the hardenability of the effect II by nitrogen, and it is not necessary to use tempered steel. Sufficient mechanical strength can be obtained even with steel.
  • alloy steel tends to have a slightly higher surface hardness
  • a sufficiently deep hardening depth can be obtained even with inexpensive carbon steel due to the effect II of nitrogen.
  • carbon steel for mechanical structures such as S45C is a heat treatment material having a hardness profile with sufficient hardness and sufficient depth.
  • S45C is not necessarily a tempered material, and even if the heat treatment of the present invention is applied to a steel member having a non-tempered ferrite-pearlite structure, sufficient martensitic transformation occurs and sufficient mechanical properties are obtained. It can be a heat-treated machine part with high strength.
  • the application of the present invention improves the mechanical strength of the parts, reduces the cutting process and switches to inexpensive materials, thereby reducing the size and weight of the entire mechanical parts by downsizing the parts, and nitriding and induction hardening. It is possible to reduce the actual cost by surplus to compensate for the cost increase due to the combined processing.
  • the compound layer protection by the oxide layer of the present invention after nitriding treatment When quenching is performed on a part on which a film is formed, the nitride layer is sufficiently protected, and the steel base portion under the layer can obtain a quenched structure corresponding to the used quenching technique.
  • the hardened steel member according to the present invention is suitable for those used in a high load / high surface pressure region.
  • the shape and type of steel members are not particularly limited, and examples include shafts, gears, pistons, shafts, cams, engine valves, valve lifters, plungers, etc. It is also suitable for train parts.
  • Example 1 As a base material, an SCM440 tempered material having a diameter of 8 mm and a length of 50 mm that was sufficiently degreased and washed was used. Salt bath soft nitriding treatment (Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.) was performed in a molten salt bath at 560 ° C. for 1 hour. Thereafter, treatment was performed for 30 minutes in an AB1 salt bath (manufactured by Nihon Parkerizing Co., Ltd.) at 400 ° C. as an oxidation treatment.
  • Salt bath soft nitriding treatment Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.
  • AB1 salt bath manufactured by Nihon Parkerizing Co., Ltd.
  • Example 2 As a base material, an S45C tempered material having a diameter of 8 mm and a length of 50 mm that was sufficiently degreased and washed was used. Salt bath soft nitriding treatment (Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.) was performed in a molten salt bath at 560 ° C. for 2 hours. Thereafter, treatment was performed for 30 minutes in an AB1 salt bath (manufactured by Nihon Parkerizing Co., Ltd.) at 400 ° C. as an oxidation treatment.
  • Salt bath soft nitriding treatment Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.
  • AB1 salt bath manufactured by Nihon Parkerizing Co., Ltd.
  • a dense magnetite layer having a thickness of 1.0 ⁇ m was formed on the outermost surface, and a nitrogen compound layer mainly composed of iron nitride having a thickness of 12.4 ⁇ m was formed directly below the dense magnetite layer.
  • a nitrogen compound layer mainly composed of iron nitride having a thickness of 12.4 ⁇ m was formed directly below the dense magnetite layer.
  • Example 3 As a base material, an S45C tempered material having a diameter of 8 mm and a length of 50 mm that was sufficiently degreased and washed was used. A salt bath soft nitriding treatment (Isonite TF-1 treatment: Nippon Parkerizing Co., Ltd.) was performed in a molten salt bath at 570 ° C. for 1 hour. Thereafter, treatment was performed for 30 minutes in an AB1 salt bath (manufactured by Nihon Parkerizing Co., Ltd.) at 400 ° C. as an oxidation treatment.
  • Isonite TF-1 treatment Nippon Parkerizing Co., Ltd.
  • a dense magnetite layer having a thickness of 0.8 ⁇ m was formed on the outermost surface, and a nitrogen compound layer mainly composed of iron nitride having a thickness of 7.5 ⁇ m was formed directly below the dense magnetite layer.
  • a nitrogen compound layer mainly composed of iron nitride having a thickness of 7.5 ⁇ m was formed directly below the dense magnetite layer.
  • Example 4 As a base material, an S45C non-heat treated material (ferrite / pearlite structure) having a diameter of 8 mm and a length of 50 mm, which was sufficiently degreased and washed, was used. After performing a salt bath soft nitriding treatment (Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.) at 560 ° C. for 1 hour in a molten salt bath, the treatment was performed in a steam atmosphere at 500 ° C. for 60 minutes as an oxidation treatment.
  • a salt bath soft nitriding treatment Isonite NS-2 treatment: Nippon Parkerizing Co., Ltd.
  • Example 5 As a base material, an SCM435 tempered material having a diameter of 8 mm and a length of 50 mm that was sufficiently degreased and washed was used. After salt bath soft nitriding treatment (Isonite NS-2 treatment: Nihon Parkerizing Co., Ltd.) at 570 ° C. for 1 hour in a molten salt bath, it was oxidized in an alkali conversion treatment solution for black dyeing at 140 ° C. for 15 hours. Treated for minutes.
  • salt bath soft nitriding treatment Isonite NS-2 treatment: Nihon Parkerizing Co., Ltd.
  • a dense magnetite layer having a thickness of 0.5 ⁇ m was formed on the outermost surface, and a nitrogen compound layer mainly composed of iron nitride having a thickness of 8.2 ⁇ m was formed directly below the dense magnetite layer.
  • a nitrogen compound layer mainly composed of iron nitride having a thickness of 8.2 ⁇ m was formed directly below the dense magnetite layer.
  • Example 6 As a base material, an S45C tempered material having a diameter of 8 mm and a length of 50 mm that was sufficiently degreased and washed was used. Using a salt bath (Isonite LS treatment: Nippon Parkerizing Co., Ltd.) capable of performing nitriding treatment and oxidation treatment simultaneously, salt bath soft nitriding oxidation treatment was performed at 560 ° C. for 2 hours. In the steel material thus treated, a dense lithium-containing magnetite layer having a thickness of 3.5 ⁇ m was formed on the outermost surface, and a nitrogen compound layer mainly composed of 8.6 ⁇ m thick iron nitride was formed immediately below. On the other hand, using an induction hardening apparatus in the air atmosphere, after reaching 820 ° C. by heating for 1 second, quenching was performed immediately by water cooling.
  • a salt bath Isonite LS treatment: Nippon Parkerizing Co., Ltd.
  • Table 1 shows a list of evaluation results.
  • the effective curing depth in the table is the depth (mm) from the surface of the portion having a hardness of Hv550 or higher.
  • FIG. 1, FIG. 2, and FIG. 3 show cross-sectional photographs of Example 2, Example 6, and Comparative Example 1, respectively.
  • FIG. 4 shows the cross-sectional hardness distribution of Example 4.

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Abstract

L'invention a pour but de proposer un moyen qui permet à une couche d'un composé de l'azote de rester uniformément même sur un objet ayant une forme complexe, tel qu'une surface de dent d'engrenage (par exemple, une pièce structurale mécanique) et assure également la formation d'une martensite fine, et peut donc conférer une excellente résistance mécanique comprenant la résistance à l'écrasement, la résistance à l'usure et la résistance à la fatigue au pliage à l'objet ayant une forme complexe après un durcissement à haute fréquence. À cet effet, selon l'invention, il est proposé un procédé consistant à soumettre un matériau fer/acier à un traitement thermique combiné d'un traitement de nitruration et d'un traitement de durcissement à haute fréquence, qui est caractérisé en ce qu'avant le traitement de durcissement à haute fréquence après le traitement de nitruration, on réalise de façon supplémentaire une étape de traitement pour former une couche d'oxyde ayant une épaisseur de 0,1 à 5 µm sur le côté surface sur une couche de composé de l'azote formée sur un fer/acier par le traitement de nitruration à 600°C ou au-dessous, et est également caractérisé en ce que le traitement de durcissement à haute fréquence est effectué dans des conditions telles que la couche du composé de l'azote ayant une dureté de HV 550 ou plus et une épaisseur de 1 µm ou plus est restée sur la couche de surface du matériau fer/acier.
PCT/JP2011/067425 2010-09-14 2011-07-29 Élément fer/acier ayant une couche d'un composé de l'azote et son procédé de fabrication WO2012035900A1 (fr)

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JP2014005501A (ja) * 2012-06-25 2014-01-16 Jfe Steel Corp 鉄鋼材料およびその製造方法
JP2015530479A (ja) * 2012-07-09 2015-10-15 スタックポール インターナショナル パウダー メタル，ユーエルシーＳｔａｃｋｐｏｌｅ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｐｏｗｄｅｒ Ｍｅｔａｌ，Ｕｌｃ 燃料セルインターコネクタ及び燃料セルインターコネクタの製造方法
CN109536916A (zh) * 2018-12-27 2019-03-29 合肥百思新材料研究院有限公司 一种可以自由升降的真空气氛淬火cvd***及其工作方法
WO2020175453A1 (fr) * 2019-02-26 2020-09-03 パーカー熱処理工業株式会社 Élément en acier de nitruration, et procédé et dispositif de fabrication d'élément en acier de nitruration
CN115612972A (zh) * 2022-09-27 2023-01-17 南京丰东热处理工程有限公司 钢表面层厚可控的含氮马氏体复合改性层及其工艺方法

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WO2021070344A1 (fr) * 2019-10-10 2021-04-15 パーカー熱処理工業株式会社 Matrice et procédé de production de matrice
JP7262376B2 (ja) * 2019-11-26 2023-04-21 日野自動車株式会社 鉄鋼材料

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JP2014005501A (ja) * 2012-06-25 2014-01-16 Jfe Steel Corp 鉄鋼材料およびその製造方法
JP2015530479A (ja) * 2012-07-09 2015-10-15 スタックポール インターナショナル パウダー メタル，ユーエルシーＳｔａｃｋｐｏｌｅ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｐｏｗｄｅｒ Ｍｅｔａｌ，Ｕｌｃ 燃料セルインターコネクタ及び燃料セルインターコネクタの製造方法
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CN109536916A (zh) * 2018-12-27 2019-03-29 合肥百思新材料研究院有限公司 一种可以自由升降的真空气氛淬火cvd***及其工作方法
WO2020175453A1 (fr) * 2019-02-26 2020-09-03 パーカー熱処理工業株式会社 Élément en acier de nitruration, et procédé et dispositif de fabrication d'élément en acier de nitruration
CN115612972A (zh) * 2022-09-27 2023-01-17 南京丰东热处理工程有限公司 钢表面层厚可控的含氮马氏体复合改性层及其工艺方法

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