WO2020045266A1 - 表面硬化材料の製造方法 - Google Patents

表面硬化材料の製造方法 Download PDF

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Publication number
WO2020045266A1
WO2020045266A1 PCT/JP2019/032980 JP2019032980W WO2020045266A1 WO 2020045266 A1 WO2020045266 A1 WO 2020045266A1 JP 2019032980 W JP2019032980 W JP 2019032980W WO 2020045266 A1 WO2020045266 A1 WO 2020045266A1
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Prior art keywords
steel material
nitrogen
producing
cooling
less
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PCT/JP2019/032980
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English (en)
French (fr)
Inventor
中島　隆
伊藤　太郎
竜也 松川
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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Application filed by 日本パーカライジング株式会社 filed Critical 日本パーカライジング株式会社
Priority to MX2021001758A priority Critical patent/MX2021001758A/es
Priority to US17/270,960 priority patent/US11332818B2/en
Priority to EP19853464.6A priority patent/EP3825438A4/en
Priority to CN201980040442.XA priority patent/CN112469842A/zh
Publication of WO2020045266A1 publication Critical patent/WO2020045266A1/ja

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    • 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
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    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
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    • 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
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    • 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
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    • C23C8/22—Carburising of ferrous surfaces
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    • 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
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    • 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
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    • 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
    • C23C8/34—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 more than one step
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    • 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
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    • C23C8/36—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 using ionised gases, e.g. ionitriding
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    • 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
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    • 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
    • C23C8/60—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 solids, e.g. powders, pastes
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    • 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
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    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • the present invention relates to a method for producing a surface-hardened material hardened to a deep position by performing a predetermined treatment on a steel material having a solid solution of nitrogen on the surface.
  • Patent Literature 1 discloses a method in which a steel is subjected to a soft nitriding treatment, a nitride layer having a predetermined thickness is formed on the surface, and then heated at 1000 to 1200 ° C. for 30 to 120 minutes. Further, in Patent Document 2, the surface of a mold material is heated after nitriding treatment, and is performed at a cooling rate of 30 ° C./sec or less to a martensitic transformation start temperature or less at a critical cooling rate of martensitic transformation. There is disclosed a method of cooling to reduce or eliminate nitrogen compounds on the surface and diffuse and solid-dissolve nitrogen therein to make the surface hardened layer deeper than the nitriding treatment alone.
  • an object of the present invention is to solve the above-mentioned problem, and to provide a method for producing a surface hardened material having a hard surface up to a deep position.
  • the present invention includes the following. (1) an immersion step of immersing a steel material having a solid solution of nitrogen on the surface thereof in a melt containing chloride at a temperature of 650 ° C. to 900 ° C. A cooling step of cooling the immersed steel material at a cooling rate equal to or higher than the lower critical cooling rate at which martensitic transformation starts, to a martensitic transformation start temperature or lower, A method for producing a surface-hardened material, comprising: (2) The method for producing a surface-hardened material according to (1) above, wherein the steel material in which nitrogen is dissolved in the surface further includes an iron-nitrogen compound layer as a surface layer; (3) The method for producing a surface-hardened material according to the above (1) or (2), wherein the steel material in which nitrogen is dissolved in the surface has carbon also dissolved in the surface; (4) The method for producing a surface-hardened material according to the above (1) or (2), further comprising a nitriding treatment step in which nitrogen is dissolved in the surface by
  • the steel material which forms a solid solution of nitrogen on the surface (performs the nitriding treatment) is C is 0.01% or more and 1.5% or less, 3% or less of Si, Mn of 2% or less, 5% or less in total of Cr, Mo, Cu and Ni, 1% or less of Nb, Ti, V and B in total; P is 0.1% or less, S is 0.05% or less,
  • the method for producing a surface-hardened material according to the present invention comprises: a dipping step of dipping a steel material having a solid solution of nitrogen on the surface in a molten material containing chloride at a temperature of 650 ° C. to 900 ° C .; Cooling the material at a cooling rate equal to or higher than the lower critical cooling rate at which martensitic transformation starts, to a temperature equal to or lower than the martensitic transformation start temperature.
  • a specific description will be given.
  • Steel material with a solid solution of nitrogen on the surface means a material in which nitrogen is in a solid solution state on the surface of the steel material.
  • the steel material for dissolving nitrogen on the surface is not particularly limited as long as it contains at least iron and carbon and contains 70% by mass or more (preferably 80% by mass or more) of iron.
  • rolled steel for general structure, cold rolled steel and steel strip, carbon steel for machine structure, alloy steel for machine structure, carbon tool steel, high speed tool steel, spring steel, high carbon chromium Bearing steel materials and the like are included.
  • a steel material having a plating film having the same composition as that of the steel material may be a target. In this case, the steel material and the plating film may have the same composition or may have different compositions.
  • the steel material may include other elements in addition to iron and carbon.
  • the other elements include Si, Mn, Cr, Mo, Cu, Ni, Nb, Ti, V, B, P, S, and O. One or more of these may be included in the steel material, or all may be included in the steel material.
  • the content of each element contained in the steel material will be described.
  • the content of C (carbon) is generally in the range of 0.01% by mass to 1.5% by mass, and preferably in the range of 0.4% by mass to 1.0% by mass.
  • the content of Si (silicon) is usually 3% by mass or less, preferably 1% by mass or less.
  • the content of Mn (manganese) is usually 2% by mass or less, preferably 0.6% by mass or less.
  • the total content of Cr (chromium), Mo (molybdenum), Cu (copper), Ni (nickel) and the like is usually 5% by mass or less.
  • the total content of Nb (niobium), Ti (titanium), V (vanadium), B (boron) and the like may be 1% by mass or less, but is preferably at an impurity level.
  • the content of P (phosphorus) is usually 0.1% by mass or less, preferably 0.05% by mass or less.
  • the content of S (sulfur) is usually 0.05% by mass or less, and preferably 0.03% by mass or less.
  • the content of O (oxygen) is preferably at the impurity level.
  • preferred steel materials include C in the range of 0.01% by mass or more and 1.5% by mass or less; Si 3% by mass or less; Mn 2% by mass or less; Cr, Mo, Cu, and Ni is 5% by mass or less; Nb, Ti, V and B are 1% by mass or less; P is 0.1% by mass or less; S is 0.05% by mass or less; and Fe is 70.0% by mass. % Or more and 99.5% by mass or less, or the balance includes Fe and inevitable impurities.
  • JIS steel types include SPCC, S10C, S45C, S55C, SK65 (SK7), SK105 (SK3), SUJ2, SCM420, SCM440, and the like. These steel materials may have been previously subjected to annealing or spheroidizing annealing.
  • a nitriding treatment on the steel material for example, a nitriding treatment on the steel material can be mentioned.
  • the method for producing a surface hardened material according to the present invention may further include a “nitriding step of dissolving nitrogen in the surface by nitriding the steel material before the dipping step”. Further, after the nitriding treatment step and before the immersion step described below, the steel material having a solid solution of nitrogen on the surface is cooled, or the steel material having a solid solution of nitrogen on the surface is cooled and then washed. Or you may.
  • the nitriding of the steel material is not particularly limited as long as it is a conventionally known method.
  • Examples thereof include gas nitriding, gas nitrocarburizing, plasma nitriding, and salt bath nitrocarburizing. it can.
  • a carbonitriding process may be performed as a nitriding process. By performing these nitriding treatments, on the surface of the steel material, a nitrogen diffusion layer in which nitrogen is dissolved, or a composite layer of the nitrogen diffusion layer and an iron-nitrogen compound layer formed on the nitrogen diffusion layer is formed. It is formed.
  • the nitrogen in the nitrogen diffusion layer is usually 0.05% by mass or more, but is not limited to this value.
  • the iron-nitrogen compound in the iron-nitrogen compound layer is, for example, ⁇ -Fe 2-3 N; ⁇ ′-Fe 4 N; Fex (N, C) [x is an arbitrary numerical value. ]; CrN, Cr 2 N, TiN, Si 3 N 4, MxN of VN such [M: a metal element contained in the steel material, for example, Cr, Ti, Si, V, etc., x is is any numerical value . ].
  • the thickness of the iron-nitrogen compound layer is usually formed in the range of 1 ⁇ m or more and 50 ⁇ m or less.
  • the conditions of the nitriding treatment vary depending on the type of the steel material, the treatment method, and the like. And within a range of 5 minutes to 120 minutes. More specifically, in the case of the salt bath nitrocarburizing treatment, the temperature is preferably in the range of 550 ° C to 600 ° C, more preferably in the range of 570 ° C to 590 ° C.
  • the processing time is preferably in the range of 60 minutes to 120 minutes.
  • the thickness of the iron-nitrogen compound layer can be measured by a light microscope or a scanning electron microscope on a cross section of a steel material having a surface in which nitrogen is dissolved, which is obtained by nitriding the steel material.
  • the composition of the iron-nitrogen compound layer can be measured by EPMA (Electron Beam Microanalyzer) analysis.
  • the thickness of the nitrogen diffusion layer may be a layer in which nitrogen is simply dissolved in iron, a composite layer in which nitrides of alloy elements (Cr, V, Nb, Ti, Al) are dispersed and precipitated in a matrix in which nitrogen is dissolved, Can be measured by EPMA (Electron Beam Microanalyzer) analysis.
  • the method for producing a surface-hardened material according to the present invention may further include a “carburizing treatment step of performing a carburizing treatment on a steel material” before the dipping step, more specifically, before the nitriding treatment step.
  • a “carburizing treatment step of performing a carburizing treatment on a steel material” before the dipping step, more specifically, before the nitriding treatment step.
  • examples of the carburizing treatment include solid carburizing treatment; liquid carburizing treatment such as salt bath carburizing treatment; gas carburizing treatment; vacuum carburizing treatment (vacuum gas carburizing treatment); plasma carburizing treatment (ion carburizing treatment);
  • the present invention is not limited to these.
  • the conditions of the carburizing treatment such as the temperature and the time, vary depending on the type of the steel material, the treatment method, the depth of the carbon penetration, and the like, but are appropriately set so that the carbon is solid-dissolved on the surface of the steel material.
  • the method for producing a surface-hardened material according to the present invention includes a step of performing quenching, tempering, and the like under suitable conditions to improve the surface hardness of the steel material after the carburizing step and before the nitriding step. May be further performed.
  • the steel material in which nitrogen is dissolved in the surface of the immersion step is then immersed in a melt containing chloride.
  • a melt containing chloride By this immersion step, more nitrogen dissolved in the surface can be penetrated deeply, and the surface layer can be prevented from being oxidized. Strength can also be improved.
  • the chloride contained in the melt include, but are not limited to, NaCl, KCl, BaCl 2 and the like. These chlorides may be used alone or in a combination of two or more.
  • the melt may contain a metal nitrate and / or a metal carbonate such as Na, K, Ba, etc., but may not contain it.
  • the temperature for immersion in the melt (immersion temperature) is usually in the range of 650 ° C to 900 ° C.
  • the reason for limiting to this temperature range is that the surface hardness of the surface hardened material cannot be sufficiently increased to a deep position unless it is immersed in this temperature range.
  • the time for immersion in the melt varies depending on the type of steel material for dissolving nitrogen on the surface, the immersion temperature, etc., but is usually 5 minutes to 60 minutes, preferably 5 minutes to 30 minutes. .
  • the condition of cooling is not particularly limited as long as the cooling speed is equal to or higher than the lower critical cooling speed at which martensitic transformation starts (occurs). preferable.
  • the lower critical cooling rate and the upper critical cooling rate vary depending on the composition of the steel material to be immersed, but are generally 20 ° C./sec to 30 ° C./sec or more.
  • the cooling temperature is not particularly limited as long as it is equal to or lower than the martensite transformation start temperature.
  • the method of cooling is not particularly limited, but it is preferable to immerse in a cooling medium such as water, salt water, aqueous polymer dispersion, oil, salt bath, and lead bath.
  • a cooling medium such as water, salt water, aqueous polymer dispersion, oil, salt bath, and lead bath.
  • the cooled steel material may be washed with water, or may be further tempered after washing with water.
  • Tempering can be performed under the conditions usually performed.
  • the conditions such as the tempering temperature and time vary depending on the composition of the cooled steel material and the intended use. For example, the temperature is in the range of 150 ° C. or more and 180 ° C. or less, and in the range of 60 minutes or more and 90 minutes or less. And the like.
  • test piece 1 A test piece 1 was prepared by annealing carbon steel S45C for machine structure at 850 ° C. for 4 hours and forming it into a diameter of 20 mm ⁇ a length of 50 mm by machining.
  • Test piece 2 A test piece 2 was prepared by cutting a 1 mm-thick ultra mild steel sheet for automobiles SPCC into 70 mm x 150 mm.
  • Test piece 3 S10C was annealed at 900 ° C.
  • Test piece 4 S55C was annealed at 850 ° C. for 4 hours, and was machined to form a test piece 4 having a diameter of 20 mm and a length of 50 mm.
  • Test piece 5 and test piece 6 The SCM420 was annealed at 850 ° C. for 4 hours, and formed into a diameter of 20 mm and a length of 50 mm by machining to prepare a test piece 5. This test piece was carburized at 930 ° C. for 180 minutes in a carburizing furnace while injecting a propane modified gas (RX gas) and a propane enriched gas.
  • RX gas propane modified gas
  • propane enriched gas propane enriched gas
  • test piece 6 was formed to a size of 50 mm and provided with a carburized layer on the surface.
  • the effective hardened layer depth was measured based on “Method for measuring the depth of carburized hardened layer of steel” in JIS G 0557: 2006. (6)
  • Test piece 7 The SCM440 was spheroidized and annealed and machined to form a test piece having a diameter of 20 mm and a length of 50 mm.
  • Test pieces 1 for producing evaluation materials 1 to 5 were immersed in a salt bath nitrocarburizing agent (manufactured by Parker Heat Treatment Industry; NS-2), and subjected to a salt bath nitrocarburizing treatment at 570 ° C. for 120 minutes.
  • a salt bath nitrocarburizing agent manufactured by Parker Heat Treatment Industry; NS-2
  • the iron-nitrogen compound layer was about 15 ⁇ m thick from the surface, and the nitrogen diffusion layer was about 200 ⁇ m below the iron-nitrogen compound layer. It was confirmed that a composite layer was formed at a thickness of.
  • the test piece 1 subjected to the salt bath nitrocarburizing treatment was immersed in a salt bath agent containing a chloride metal salt, and heated in a salt bath at 600 to 1000 ° C. for 30 minutes.
  • a salt bath agent GS540 (melting point: 540 ° C.) manufactured by Parker Heat Treatment Industry is used when heating at 600 ° C. or 650 ° C.
  • GS660 melting point: Parking Heat Treatment Industry
  • the test piece 1 was immersed in a 5% aqueous NaCl solution at 20 to 30 ° C. and cooled (hereinafter referred to as “water cooling”). Evaluation materials 1 to 5 were produced. The cooling rate at this time was approximately 170 ° C./sec.
  • test specimens 1 prepared for the evaluation materials 6 to 10 were subjected to the plasma nitriding treatment, and the specimens 1 subjected to the plasma nitriding treatment were observed by an optical microscope and EPMA analysis.
  • the plasma nitriding treatment was performed at 570 ° C. for 6 hours while adjusting the volume ratio of N 2 gas and H 2 gas in the furnace to be 1: 4, reducing the pressure to 3 torr.
  • the iron-nitrogen compound layer was formed discontinuously on the surface, and that the nitrogen diffusion layer was formed with a thickness of about 200 ⁇ m below or from the surface of the iron-nitrogen compound layer. .
  • the surface of the test piece 1 subjected to the plasma nitriding treatment was mechanically polished to remove a slight iron-nitrogen compound layer formed discontinuously on the surface, and immersed in a salt bath and water-cooled as described above. No. Evaluation materials of 6 to 10 were produced.
  • Characteristic evaluation No The characteristics (surface oxidation, cross-sectional hardness) of the evaluation materials 1 to 10 were evaluated.
  • the surface oxidation includes the presence or absence of peeling or falling off of oxides and the like from the surface of the test piece 1 during water cooling, and the thickness of the oxide scale on the surface when a cross section of each evaluation material is observed with a metallographic microscope (observation magnification: 500 times). Was confirmed and evaluated.
  • observation magnification 500 times
  • the surface oxidation was evaluated as “Yes”.
  • the section hardness is mirror-finished by mechanical polishing, and then the depth from the surface is measured using a micro hardness tester (Micro Vickers) at a measurement load of 0.3 kgf.
  • the microhardness (HV) at a position of 300 ⁇ m was measured. Table 2 shows the results.
  • Evaluation materials 11 and 12 were produced.
  • the cooling rate at this time was approximately 100 ° C./sec.
  • the test piece 1 or 6 subjected to the salt bath nitrocarburizing treatment was heated in an electric furnace at 800 ° C. for 5 minutes or 30 minutes (electric furnace heating). After heating, the test piece 1 or 6 was cooled with water or oil. 13 to 15 evaluation materials were produced.
  • the test piece 6 subjected to the salt bath nitrocarburizing treatment was heated at 800 ° C. for 0.5 to 5 minutes using a high frequency power supply (maximum output: 30 kW, frequency: 70 kHz) (IH). After heating, the test piece 6 was oil-cooled. 16 to 18 evaluation materials were produced. No. Properties of 11 to 18 evaluation materials were evaluated in the same manner as described above. Table 3 shows the results.
  • test piece 6 subjected to the salt bath nitrocarburizing treatment was heated in a salt bath at 850 ° C. for 5 minutes, left in a room at 20 ° C., cooled to 20 ° C. Twenty evaluation materials were produced. The cooling rate at this time was about 10 ° C./sec. No. The characteristics of the evaluation materials 19 to 26 were evaluated in the same manner as described above. Table 4 shows the results.

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Abstract

表面に窒素が固溶された鉄鋼材料を、塩化物を含む溶融物に６５０℃～９００℃の範囲内で浸漬する浸漬ステップと、浸漬した前記鉄鋼材料を、マルテンサイト変態が開始する下部臨界冷却速度以上の冷却速度にて、マルテンサイト変態開始温度以下まで冷却する冷却ステップと、を含む、表面硬化材料の製造方法。

Description

表面硬化材料の製造方法
　本発明は、表面に窒素が固溶された鉄鋼材料に所定の処理を施すことにより、深い位置まで硬化させた表面硬化材料の製造方法に関する。
　鉄鋼材料の表面硬化処理法として、従来、様々な方法が開発されている。例えば、特許文献１には、鋼に軟窒化処理を施し、表面に所定の厚さの窒化物層を形成し、次いで、１０００～１２００℃で３０～１２０分加熱する方法が開示されている。また、特許文献２には、金型材に対して窒化処理を行った後に表面の加熱を行い、マルテンサイト変態の臨界冷却速度以上３０℃／ｓｅｃ以下の冷却速度にてマルテンサイト変態開始温度以下まで冷却し、表面の窒素化合物を減少ないしは消滅させかつ内部に窒素を拡散・固溶させ、表面硬化層を窒化処理単独に比べて深くする方法が開示されている。
特開２０１５－５９２４８号公報 特開平７－１３８７３３号公報
　しかし、特許文献１及び２に記載の方法では、表面に窒素が固溶された鉄鋼材料に対し、多くの窒素を深くまで浸透させることができなかったり、表層が酸化したりして、深い位置まで硬質な表面を形成できない場合があった。そこで、本発明の目的は、上記問題を解決するものであり、深い位置まで硬質な表面を有する表面硬化材料を製造する方法を提供することである。
　すなわち、本発明は、以下のものを含む。
（１）表面に窒素が固溶された鉄鋼材料を、塩化物を含む溶融物に６５０℃～９００℃の範囲内で浸漬する浸漬ステップと、
　浸漬した前記鉄鋼材料を、マルテンサイト変態が開始する下部臨界冷却速度以上の冷却速度にて、マルテンサイト変態開始温度以下まで冷却する冷却ステップと、
を含む、表面硬化材料の製造方法；
（２）表面に窒素が固溶された鉄鋼材料は、表層として鉄窒素化合物層を更に含む、上記（１）に記載の表面硬化材料の製造方法；
（３）表面に窒素が固溶された鉄鋼材料は、表面に炭素も固溶されている、上記（１）又は（２）に記載の表面硬化材料の製造方法；
（４）鉄鋼材料を窒化処理することにより、表面に窒素を固溶する窒化処理ステップを更に含む、上記（１）又は（２）に記載の表面硬化材料の製造方法；
（５）前記窒化処理が、ガス窒化処理、ガス軟窒化処理、プラズマ窒化処理、又は塩浴軟窒化処理である、上記（４）に記載の表面硬化材料の製造方法；
（６）前記窒化処理ステップの前に、鉄鋼材料に浸炭処理を施す浸炭処理ステップを更に含む、上記（４）又は（５）に記載の表面硬化材料の製造方法；
（７）表面に窒素を固溶する（前記窒化処理を行う）鉄鋼材料が、質量％で、
　Ｃを０．０１％以上１．５％以下、
　Ｓｉを３％以下、
　Ｍｎを２％以下、
　Ｃｒ、Ｍｏ、Ｃｕ及びＮｉを合計で５％以下、
　Ｎｂ、Ｔｉ、Ｖ及びＢを合計で１％以下、
　Ｐを０．１％以下、
　Ｓを０．０５％以下、
　Ｆｅを７０．０％以上９９．５％以下
の範囲内で含む、上記（１）～（６）のいずれかに記載の表面硬化材料の製造方法；
（８）表面に窒素を固溶する（前記窒化処理を行う）鉄鋼材料が、質量％で、
　Ｃを０．０１％以上１．５％以下、
　Ｓｉを３％以下、
　Ｍｎを２％以下、   
　Ｃｒ、Ｍｏ、Ｃｕ及びＮｉを合計で５％以下、
　Ｎｂ、Ｔｉ、Ｖ及びＢを合計で１％以下、
　Ｐを０．１％以下、
　Ｓを０．０５％以下
の範囲内で含み、Ｆｅおよび不可避不純物を残部として更に含む、上記（１）～（６）のいずれかに記載の表面硬化材料の製造方法。
　本発明によれば、深い位置まで硬質な表面を有する表面硬化材料を製造する方法を提供することができる。
　本発明に係る表面硬化材料の製造方法は、表面に窒素が固溶された鉄鋼材料を、塩化物を含む溶融物に６５０℃～９００℃の範囲内で浸漬する浸漬ステップと、浸漬した前記鉄鋼材料を、マルテンサイト変態が開始する下部臨界冷却速度以上の冷却速度にて、マルテンサイト変態開始温度以下まで冷却する冷却ステップと、を含む。以下、具体的に説明する。
　表面に窒素が固溶された鉄鋼材料とは、鉄鋼材料の表面において窒素が固溶状態にあるものを意味する。表面に窒素を固溶するための鉄鋼材料としては、少なくとも鉄と炭素を含み、鉄が７０質量％以上（好ましくは８０質量％以上）含まれるものであれば特に制限されるものではなく、具体的には、一般構造用圧延鋼材、冷間圧延鋼材及び鋼帯、機械構造用炭素鋼鋼材、機械構造用合金鋼鋼材、炭素工具鋼鋼材、高速度工具鋼鋼材、ばね鋼鋼材、高炭素クロム軸受鋼鋼材などが挙げられる。なお、鉄鋼材料と同様の組成で構成されているめっき被膜を有する鉄鋼材料も対象となり得る。この場合、鉄鋼材料とめっき被膜は同一組成からなるものであっても、異なる組成からなるものであってもよい。また、鉄鋼材料は、鉄及び炭素以外に他の元素を含むものであってもよい。他の元素としては、例えば、Ｓｉ、Ｍｎ、Ｃｒ、Ｍｏ、Ｃｕ、Ｎｉ、Ｎｂ、Ｔｉ、Ｖ、Ｂ、Ｐ、Ｓ、Ｏ等が挙げられる。これらのうち、１種又は２種以上が鉄鋼材料に含まれていてもよいし、全部が鉄鋼材料に含まれていてもよい。
　鉄鋼材料に含まれる各元素の含有量について説明する。Ｃ（炭素）の含有量は、通常０．０１質量％以上１．５質量％以下の範囲内であり、好ましくは０．４質量％以上１．０質量％以下の範囲内である。Ｓｉ（ケイ素）の含有量は、通常３質量％以下であり、好ましくは１質量％以下である。Ｍｎ（マンガン）の含有量は、通常２質量％以下であり、好ましくは０．６質量％以下である。Ｃｒ（クロム）、Ｍｏ（モリブデン）、Ｃｕ（銅）、Ｎｉ（ニッケル）等の合計含有量は、通常５質量％以下である。Ｎｂ（ニオブ）、Ｔｉ（チタン）、Ｖ（バナジウム）、Ｂ（ホウ素）等の合計含有量は、１質量％以下であればよいが、不純物レベルであることが好ましい。Ｐ（燐）の含有量は、通常０．１質量％以下であり、好ましくは０．０５質量％以下である。Ｓ（硫黄）の含有量は、通常０．０５質量％以下であり、好ましくは０．０３質量％以下である。Ｏ（酸素）の含有量は、不純物レベルであることが好ましい。
　本実施の形態において、好ましい鉄鋼材料としては、Ｃを０．０１質量％以上１．５質量％以下の範囲内；Ｓｉを３質量％以下；Ｍｎを２質量％以下；Ｃｒ、Ｍｏ、Ｃｕ及びＮｉを合計で５質量％以下；Ｎｂ、Ｔｉ、Ｖ及びＢを合計で１質量％以下；Ｐを０．１質量％以下；Ｓを０．０５質量％以下；および、Ｆｅを７０．０質量％以上９９．５質量％以下、または、残部としてＦｅおよび不可避不純物；を含むものである。具体的には、ＪＩＳ鋼種でいえば、ＳＰＣＣ、Ｓ１０Ｃ、Ｓ４５Ｃ、Ｓ５５Ｃ、ＳＫ６５（ＳＫ７）、ＳＫ１０５（ＳＫ３）、ＳＵＪ２、ＳＣＭ４２０、ＳＣＭ４４０などが挙げられる。これらの鉄鋼材料は、予め焼鈍や球状化焼鈍が施されたものであってもよい。
　鉄鋼材料の表面に窒素を固溶する方法としては、例えば、鉄鋼材料に対する窒化処理を挙げることができる。本発明に係る表面硬化材料の製造方法は、「浸漬ステップの前に、鉄鋼材料を窒化処理することにより、表面に窒素を固溶する窒化処理ステップ」を更に含んでもよい。また、窒化処理ステップの後であって、後述の浸漬ステップの前に、表面に窒素が固溶された鉄鋼材料を冷却したり、表面に窒素が固溶された鉄鋼材料を冷却した後洗浄したりしてもよい。鉄鋼材料に対する窒化処理としては、従来知られている方法であれば特に制限されるものではなく、例えば、ガス窒化処理、ガス軟窒化処理、プラズマ窒化処理、塩浴軟窒化処理等を挙げることができる。また、後述の浸炭処理ステップを行う場合には、窒化処理として浸炭窒化処理を行ってもよい。これらの窒化処理を行うことにより、鉄鋼材料の表面において、窒素が固溶された窒素拡散層、あるいは、その窒素拡散層と該窒素拡散層上に形成される鉄窒素化合物層との複合層が形成される。
　上記窒素拡散層中の窒素は、通常０．０５質量％以上であるが、この値に限定されるものではない。また、鉄窒素化合物層中の鉄窒素化合物は、例えば、ε－Ｆｅ２-３Ｎ；γ’－Ｆｅ４Ｎ；Ｆｅｘ（Ｎ，Ｃ）［ｘは任意の数値である。］；ＣｒＮ、Ｃｒ２Ｎ、ＴｉＮ、Ｓｉ３Ｎ４、ＶＮ等のＭｘＮ［Ｍ：鉄鋼材料に含まれる金属元素、例えば、Ｃｒ、Ｔｉ、Ｓｉ、Ｖ等であり、ｘは任意の数値である。］などである。鉄窒素化合物層の厚さは、通常１μｍ以上５０μｍ以下の範囲内で形成される。窒化処理の、温度及び時間等の条件は、鉄鋼材料の種類、処理の方法等によって異なるが、一般的には、Ａ１変態点以下の温度で所定時間行われ、例えば、３００℃以上６００℃以下の範囲内で、かつ、５分間以上１２０分間以下の範囲内で行われる。より具体的には、塩浴軟窒化処理の場合、温度は、５５０℃以上６００℃以下の範囲内であることが好ましく、５７０℃以上５９０℃以下の範囲内であることがより好ましい。処理時間は、６０分間以上１２０分間以下の範囲内であることが好ましい。
　鉄窒素化合物層の厚さは、鉄鋼材料を窒化処理することにより得られる、表面に窒素が固溶された鉄鋼材料、の断面を光学顕微鏡または走査型電子顕微鏡により測定できる。鉄窒素化合物層の組成はＥＰＭＡ（電子線マイクロアナライザ）分析により測定できる。窒素拡散層の厚さは、鉄に窒素が単に固溶した層、あるいは窒素を固溶した母相に合金元素（Ｃｒ、Ｖ、Ｎｂ、Ｔｉ、Ａｌ）の窒化物を分散析出した複合層、の厚さとして、ＥＰＭＡ（電子線マイクロアナライザ）分析により測定できる。
　本発明に係る表面硬化材料の製造方法は、浸漬ステップの前、より具体的には、上記窒化処理ステップの前に、「鉄鋼材料に浸炭処理を施す浸炭処理ステップ」を更に含んでもよい。この浸炭処理ステップを行うことにより、鉄鋼材料の表面に炭素を固溶することができる。また、この浸炭処理ステップと窒化処理ステップを行うことにより、表面に炭素と窒素が固溶化された鉄鋼材料を得ることができる。ここで、浸炭処理としては、例えば、固体浸炭処理；塩浴浸炭処理等の液体浸炭処理；ガス浸炭処理；真空浸炭処理（真空ガス浸炭処理）；プラズマ浸炭処理（イオン浸炭処理）；等を挙げることができるが、これらに限定されるものではない。浸炭処理の、温度及び時間等の条件は、鉄鋼材料の種類、処理の方法、炭素を浸透させる深さ等によって異なるが、鉄鋼材料の表面に炭素が固溶されるように適宜設定される。なお、本発明に係る表面硬化材料の製造方法は、浸炭処理ステップを行った後、窒化処理ステップ前に、鉄鋼材料の表面硬さを向上させるため、適した条件下で、焼入れ、焼き戻し等の処理を更に行ってもよい。
浸漬ステップ
　表面に窒素が固溶された鉄鋼材料は、次に塩化物を含む溶融物に浸漬される。この浸漬ステップにより、より多くの、表面に固溶された窒素を深くまで浸透させることができ、かつ、表層が酸化されるのを防ぐことができるため、後述の冷却ステップにより、深い位置まで表面強度も向上させることができるようになる。溶融物に含まれる塩化物としては、例えば、ＮａＣｌ、ＫＣｌ、ＢａＣｌ２等を挙げることができるがこれらに限定されるものではない。これらの塩化物は、１種を単独で用いてもよいが、２種以上を混合して用いてもよい。溶融物には、Ｎａ、Ｋ、Ｂａ等の、硝酸金属塩および／または炭酸金属塩が含まれていてもよいが、含まれていなくてもよい。溶融物に浸漬する温度（浸漬温度）は、通常、６５０℃以上９００℃以下の範囲内である。この温度範囲に限定した理由は、この温度範囲で浸漬しないと、表面硬化材料における表面硬度を深い位置まで十分に高めることができないからである。溶融物に浸漬する時間は、表面に窒素を固溶するための鉄鋼材料の種類、浸漬温度等によって異なるが、通常、５分間以上６０分間以下であり、好ましくは５分間以上３０分間以下である。
冷却ステップ
　浸漬ステップで浸漬した上記鉄鋼材料を急冷することにより、表面部にマルテンサイト変態を生じさせ、深い位置まで硬質な表面を有する表面硬化材料を製造することができる。冷却（急冷）の条件としては、マルテンサイト変態が開始する（生じる）下部臨界冷却速度以上の冷却速度であれば特に制限されるものではないが、上部臨界冷却速度以上の冷却速度であることが好ましい。下部臨界冷却速度及び上部臨界冷却速度は、浸漬する上記鉄鋼材料の組成によって異なるが、一般的に、２０℃／秒～３０℃／秒以上である。なお、冷却する温度としては、マルテンサイト変態開始温度以下であれば特に制限されるものではない。また、冷却（急冷）方法は、特に制限されるものではないが、水、塩水、ポリマー分散水溶液、油、塩浴、鉛浴などの冷却媒体に浸漬することが好ましい。冷却ステップを行った後、冷却した上記鉄鋼材料に対し、水洗したり、水洗後さらに焼き戻しを行ったりしてもよい。焼き戻しを行うことにより、靭性を向上させた表面硬化材料を製造することが可能となる。焼き戻しは、通常行われる条件で行うことができる。焼き戻しの温度及び時間等の条件は、冷却した上記鉄鋼材料の組成や使用用途により異なるが、例えば、１５０℃以上１８０℃以下の範囲内の温度、及び、６０分間以上９０分間以下の範囲内の時間等を挙げることができる。
　本発明による製造方法の効果を確認するために、７種類の試験片を作製した。なお、試験片の作製に用いた各ＪＩＳ鋼種の成分組成を表１に示す。残部は鉄および不純物、単位は質量％である。
（１）試験片１
　機械構造用炭素鋼鋼材Ｓ４５Ｃを８５０℃にて４時間の焼鈍を行い、機械加工により、直径２０ｍｍ×長さ５０ｍｍに成形し、試験片１を作製した。
（２）試験片２
　板厚１ｍｍの自動車用極軟鋼薄鋼板ＳＰＣＣを７０ｍｍ×１５０ｍｍに切断し、試験片２を作製した。
（３）試験片３
　Ｓ１０Ｃを９００℃で４時間の焼鈍を行い、機械加工により、直径２０ｍｍ×長さ５０ｍｍに成形し、試験片３を作製した。
（４）試験片４
　Ｓ５５Ｃを８５０℃で４時間の焼鈍を行い、機械加工により、直径２０ｍｍ×長さ５０ｍｍに成形し、試験片４を作製した。
（５）試験片５及び試験片６
　ＳＣＭ４２０を８５０℃で４時間の焼鈍を行い、機械加工により、直径２０ｍｍ×長さ５０ｍｍに成形し、試験片５を作製した。この試験片を、プロパン変成ガス（ＲＸガス）及びプロパンエンリッチガスを注入しながら浸炭炉内にて、９３０℃で１８０分間浸炭処理を行った。その後、８５０℃まで温度を下げてから油冷（焼入れ）を行い、有効硬化層深さ（５５０ＨＶ）が０．８ｍｍとなるように焼き戻しを行い、表面を機械研磨して直径２０ｍｍ×長さ５０ｍｍに成形し、表面に浸炭層を備えた試験片６を作製した。なお、有効硬化層深さは、ＪＩＳ　Ｇ　０５５７：２００６における「鋼の浸炭硬化層深さ測定方法」に基づき測定した。
（６）試験片７
　ＳＣＭ４４０を球状化焼鈍し、機械加工により、直径２０ｍｍ×長さ５０ｍｍに成形し、試験片を作製した。
Figure JPOXMLDOC01-appb-T000001
Ｎｏ．１～５の評価材料の作製
　試験片１を塩浴軟窒化剤（パーカー熱処理工業製；ＮＳ－２）に浸漬し、５７０℃で１２０分間塩浴軟窒化処理を行った。塩浴軟窒化処理を行った試験片１を、光学顕微鏡及びＥＰＭＡ分析により観察したところ、鉄窒素化合物層が表面から約１５μｍの厚さで、鉄窒素化合物層の下に窒素拡散層が約２００μｍの厚さで、複合層が形成されているのが確認できた。塩浴軟窒化処理を行った試験片１を、塩化物金属塩を含む塩浴剤に浸漬し、６００℃～１０００℃で３０分間塩浴加熱を行った。塩浴剤としては、６００℃又は６５０℃で加熱する場合には、パーカー熱処理工業製ＧＳ５４０（融点５４０℃）を使用し、８００～１０００℃で加熱する場合には、パーカー熱処理工業製ＧＳ６６０（融点６６０℃）を使用した。塩浴加熱を行った後、試験片１を２０～３０℃の５％ＮａＣｌ水溶液中に浸漬して冷却し（以下、「水冷」という）、Ｎｏ．１～５の評価材料を作製した。この際の冷却速度は、概ね１７０℃／秒であった。
Ｎｏ．６～１０の評価材料の作製
　試験片１に対してプラズマ窒化処理を行い、プラズマ窒化処理を行った試験片１を、光学顕微鏡及びＥＰＭＡ分析により観察した。なお、プラズマ窒化処理は、炉内のＮ２ガスとＨ２ガスの体積比が１：４となるように調整し、３ｔｏｒｒに減圧して５７０℃で６時間行った。光学顕微鏡の観察の結果、鉄窒素化合物層が表面において不連続に形成し、また、窒素拡散層が鉄窒素化合物層の下あるいは表面から約２００μｍの厚さで形成されているのが確認できた。プラズマ窒化処理を行った試験片１の表面を機械研磨して、表面に不連続に形成した僅かな鉄窒素化合物層を除去し、上述と同様に、塩浴剤への浸漬及び水冷を行い、Ｎｏ．６～１０の評価材料を作製した。
特性評価
　Ｎｏ．１～１０の評価材料の特性（表面酸化、断面硬さ）を評価した。表面酸化は、水冷時に試験片１の表面から酸化物等の剥離や脱落の有無と、各評価材料を金属顕微鏡により断面観察（観察倍率５００倍）した場合における、表面の酸化スケールの厚さと、を確認し、評価した。剥離や脱落がなく、酸化スケールの厚さが２μｍ未満である場合は実用化レベルと判断し、表面酸化が「無」と評価した。その他の場合、すなわち、剥離や脱落が確認された場合、又は酸化スケールの厚さが２μｍ以上である場合は、表面酸化が「有」と評価した。
　断面硬さは、各評価材料を切断した後、断面を機械研磨により鏡面仕上げし、続いて、微小硬さ試験機（マイクロビッカース）を用いて、測定荷重０．３ｋｇｆにて、表面から深さ３００μｍの位置における微小硬さ（ＨＶ）を測定した。
　これらの結果を表２に示す。
Figure JPOXMLDOC01-appb-T000002
Ｎｏ．１１～１８の評価材料の作製
　上述と同様に塩浴軟窒化処理を行った試験片１又は６を、光学顕微鏡及びＥＰＭＡ分析により観察した。光学顕微鏡の観察の結果、鉄窒素化合物層が表面から約１５μｍの厚さで、鉄窒素化合物層の下に窒素拡散層が約２００μｍの厚さで形成されているのが確認できた。
　塩浴軟窒化処理を行った試験片６に対し、８００℃で５分間または３０分間塩浴加熱を行った後、３０～４０℃のコールドクエンチ油（出光製；ダフニーマスタークエンチＡ）中に浸漬して冷却し（以下、「油冷」という）、Ｎｏ．１１及び１２の評価材料を作製した。この際の冷却速度は、概ね約１００℃／秒であった。
　また、塩浴軟窒化処理を行った試験片１又は６を、電気炉内において８００℃で５分間または３０分間加熱した（電気炉加熱）。加熱後、試験片１又は６を水冷または油冷し、Ｎｏ．１３～１５の評価材料を作製した。
　塩浴軟窒化処理した試験片６を、高周波電源装置（最大出力：３０ｋＷ、周波数：７０ｋＨｚ）を用いて８００℃で０．５～５分間加熱した（ＩＨ）。加熱後、試験片６を油冷し、Ｎｏ．１６～１８の評価材料を作製した。
　Ｎｏ．１１～１８の評価材料に対し、上述の同様に特性の評価を行った。その結果を表３に示す。
Figure JPOXMLDOC01-appb-T000003
Ｎｏ．１９～２６の評価材料の作製
　上述と同様に、塩浴軟窒化処理を行った試験片１～７を、光学顕微鏡及びＥＰＭＡ分析により観察した。光学顕微鏡の観察の結果、鉄窒素化合物層が表面から約１５μｍの厚さで、鉄窒素化合物層の下に窒素拡散層が約２００μｍの厚さで形成されているのが確認できた。塩浴軟窒化処理を行った試験片１～７に対し、８５０℃で５分間塩浴加熱を行った後、水冷又は油冷し、Ｎｏ．１９及びＮｏ．２１～２６の評価材料を作製した。また、塩浴軟窒化処理を行った試験片６に対し、８５０℃で５分間塩浴加熱を行った後、２０℃の部屋に放置し、２０℃になるまで冷却し、Ｎｏ．２０の評価材料を作製した。この際の冷却速度は、概ね約１０℃／秒であった。Ｎｏ．１９～２６の評価材料に対し、上述の同様に特性の評価を行った。その結果を表４に示す。
Figure JPOXMLDOC01-appb-T000004
 

Claims (5)

  1. 　表面に窒素が固溶された鉄鋼材料を、塩化物を含む溶融物に６５０℃～９００℃の範囲内で浸漬する浸漬ステップと、
    　浸漬した前記鉄鋼材料を、マルテンサイト変態が開始する下部臨界冷却速度以上の冷却速度にて、マルテンサイト変態開始温度以下まで冷却する冷却ステップと、
    を含む、表面硬化材料の製造方法。
  2. 　表面に窒素が固溶された鉄鋼材料は、表層として鉄窒素化合物層を更に含む、請求項１に記載の表面硬化材料の製造方法。
  3. 　鉄鋼材料を窒化処理することにより、表面に窒素を固溶する窒化処理ステップを更に含む、請求項１又は２に記載の表面硬化材料の製造方法。
  4. 　表面に窒素が固溶された鉄鋼材料は、表面に炭素も固溶されている、請求項１又は２に記載の表面硬化材料の製造方法。
  5. 　前記窒化処理ステップの前に、鉄鋼材料に浸炭処理を施す浸炭処理ステップを更に含む、請求項３に記載の表面硬化材料の製造方法。
     
PCT/JP2019/032980 2018-08-31 2019-08-23 表面硬化材料の製造方法 WO2020045266A1 (ja)

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