WO2020175453A1 - Élément en acier de nitruration, et procédé et dispositif de fabrication d'élément en acier de nitruration - Google Patents

Élément en acier de nitruration, et procédé et dispositif de fabrication d'élément en acier de nitruration Download PDF

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WO2020175453A1
WO2020175453A1 PCT/JP2020/007395 JP2020007395W WO2020175453A1 WO 2020175453 A1 WO2020175453 A1 WO 2020175453A1 JP 2020007395 W JP2020007395 W JP 2020007395W WO 2020175453 A1 WO2020175453 A1 WO 2020175453A1
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Prior art keywords
phase
steel member
compound layer
nitride compound
furnace
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Japanese (ja)
Inventor
泰 平岡
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Parker Netsushori Kogyo KK
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Parker Netsushori Kogyo KK
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    • 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
    • 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
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/30—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for crankshafts; for camshafts
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/32—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for gear wheels, worm wheels, or the like
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C3/00—Shafts; Axles; Cranks; Eccentrics
    • F16C3/04—Crankshafts, eccentric-shafts; Cranks, eccentrics
    • F16C3/06—Crankshafts
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H55/00—Elements with teeth or friction surfaces for conveying motion; Worms, pulleys or sheaves for gearing mechanisms
    • F16H55/02—Toothed members; Worms
    • F16H55/06—Use of materials; Use of treatments of toothed members or worms to affect their intrinsic material properties

Definitions

  • Nitride steel member and method and device for manufacturing nitrided steel member Nitride steel member and method and device for manufacturing nitrided steel member
  • the present invention relates to a nitrided steel member, and a method and an apparatus for manufacturing the nitrided steel member. More specifically, the present invention relates to a nitrided steel member having excellent wear resistance, which is useful for gears for automobile transmissions, crankshafts, and the like, and a manufacturing method and a manufacturing device for the nitrided steel member.
  • the nitriding treatment which is a low heat treatment strain treatment, is high in number, and recently, the atmosphere control technology of the gas nitriding treatment has been particularly interested.
  • a compound layer which is an iron nitride is formed on the surface and a hardened layer called a diffusion layer is formed inside.
  • the hardened layer is usually made of an alloy nitride such as 3 or 0 ", which is a base material component.
  • Non-Patent Document 1 it is known that the fatigue resistance is improved by forming the phase' rather than the phase.
  • Patent Document 1 a nitrided steel member having improved bending fatigue strength and surface fatigue by forming a ⁇ phase is also provided.
  • Patent Document 1 ⁇ 2020/175453 2 ⁇ (: 170? 2020/007395
  • Non-Patent Document 2 As a nitriding method for forming a compound layer containing a large amount of s phase on the surface, a soft nitriding treatment is known, which is performed by mixing a small amount of carburizing gas into an ammonia atmosphere.
  • the nitriding treatment when the nitriding treatment is performed at a temperature higher than the eutectoid transformation point (about 590°C) of the Fe_N binary alloy, a compound layer is formed on the surface, and if it is then rapidly cooled, nitrogen is formed below it. A hardened layer containing the contained martensitic structure is formed.
  • the nitriding treatment in this temperature range is called an nitriding treatment (A u s t e n i t i c N i t r i d i n g) in distinction from the conventional nitriding process (N i t r i d i n g).
  • STKM- 13C mechanical structure carbon steel pipe defined in JIS G 3445
  • nitriding treatment at 640°C for 90 m in
  • further nitriding treatment at 660°C for 40 min
  • Subsequent reheating at 9Om in at 280°C cures the near surface surface to 800-900 HV.
  • Non-Patent Document 3 The compound layer on the surface at this time is reported to be in the s phase.
  • Patent Document 1 Japanese Patent Laid-Open No. 201 3-22 1 203
  • Patent Document 2 JP 201 4-25 1 61 Publication
  • Non-Patent Document 1 Yasushi Hiraoka, Yoichi Watanabe, Akitake Ishida: Heat Treatment, Volume 55, No. 1, 1 _ 2 ⁇ 2020/175 453 3 (: 170? 2020 /007395
  • Non-Patent Document 2 Dietary Toke et al.: Nitriding and nitrocarburizing of iron, Agne Technology Center —, 2 0 1 3 years, page 8 4
  • Non-Patent Document 3 Kawai _ Ki, Toru Kidate: Summary of the 81st Spring Lecture Meeting of Japan Heat Treatment Technology Association, pp. 2 9-30
  • Friction loss in mechanical parts, such as camshafts, piston rings, crankshafts, etc., inside automobile engines is as high as 10% or more.
  • Surface treatment such as nitriding has already been applied to some mechanical parts, but further reduction of friction loss is desired.
  • Non-Patent Document 3 since the nitriding temperature is 700°C, which is relatively high, the hardness of the base material and the diffusion layer may be reduced.
  • the compound layer formed by the soft nitriding treatment has insufficient surface hardness (see the comparative example in Fig. 11 described later) and has insufficient abrasion resistance (see Table 1 described below). See comparative example).
  • the inventors of the present invention have conducted sufficient studies and various experiments, and have maintained a sufficient hardness by controlling the temperature and nitriding potential of the nitriding treatment with high accuracy while limiting the configuration of the treatment furnace. Manufacturing of nitrided steel members with improved wear resistance ⁇ 2020/175 453 4 ⁇ (: 170? 2020 /007395
  • the present invention was created based on the above findings.
  • the purpose of the present invention is
  • a nitride steel member having improved wear resistance in the surface layer region and a manufacturing method and manufacturing apparatus for manufacturing such a nitrided steel member.
  • the present invention is a nitrided steel member having a carbon steel or low alloy steel as a mother phase, comprising a nitride compound layer on the surface, and a hardened layer having an austenite structure under the nitride compound layer.
  • a diffusion layer in which nitrogen is diffused in the matrix is provided below the hardened layer, and the nitride compound layer has a phase distribution in the order of £ phase, a′ phase, and £ phase.
  • the volume ratio of the phase' in the nitride compound layer is 20% or more, and the nitride compound layer is 5 to 5% from the surface of the nitrided steel member.
  • a nitrided steel member having a thickness of 50 having a thickness of 50.
  • the nitride compound layer on the surface has a phase distribution of the order of £ phase, ⁇ phase, and £ phase, and has a thickness of 50! Since the volume ratio of the phase' in the nitride compound layer is 20% or more (such a structure was first realized by the nitriding method described later), it has sufficient hardness as a nitrided steel member. It is possible to improve wear resistance while providing
  • the upper limit of 50 for the thickness of the nitride compound layer is because that value is the maximum thickness confirmed by the inventor of the present application up to the time of filing of the present application (see Using the mold treatment furnace, adopt the nitrogen treatment conditions of 350 (3 steels as mother phase, treatment temperature: 640° ⁇ , nitriding potential: 0.6, treatment time: 2 hours). Has been confirmed to be obtained by).
  • the lower limit of 5 is set as a condition for forming the nitride compound layer on the entire surface of the nitrided steel member (there is no case where the nitride compound layer is not locally formed). It has a value.
  • the present invention is a nitrided steel member having a carbon steel or a low alloy steel as a parent phase, comprising a nitride compound layer on the surface, and a hardening having an austenitic structure under the nitride compound layer. A layer, and nitrogen spreads in the matrix below the hardened layer. ⁇ 2020/175 453 5 ⁇ (: 170? 2020 /007395
  • the nitride compound layer has a phase distribution of A′ phase and £ phase, and the volume ratio of the A′ phase in the nitride compound layer is 30% or more.
  • the nitride compound layer is 5 to 5 from the surface of the nitrided steel member.
  • a nitrided steel member having a thickness of 30 A nitrided steel member having a thickness of 30.
  • the nitride compound layer on the surface has a phase distribution in the order of A′ phase and £ phase, and Due to the volume ratio of the A'phase in the nitride compound layer being 30% or more (such a structure was first realized by the nitriding method described later), sufficient hardness as a nitrided steel member was obtained. It is possible to improve wear resistance while providing
  • the thickness of the nitride compound layer is set as a condition for forming the nitride compound layer on the entire surface of the nitrided steel member (the nitride compound layer may not be locally formed). , 5 are the lower limits.
  • carbon steel having a carbon content of not less than 0.1% in mass% can be used as the parent phase.
  • the present invention can also be recognized as a method for manufacturing a nitrided steel member. That is, the present invention is a method for producing a nitrided steel member having a carbon steel or a low alloy steel as a mother phase, using a circulation type processing furnace equipped with a guide cylinder and a stirring fan, wherein during the nitriding processing, The temperature range in the circulation-type treatment furnace is controlled to 610 ° to 660 ° ⁇ , and at the time of the nitriding treatment, the nitriding potential in the circulation-type treatment furnace is 0.
  • the method for producing a nitrided steel member is characterized in that the nitriding treatment is controlled within the range of .6, the nitriding treatment is followed by rapid cooling, and then reheating treatment. ⁇ 2020/175 453 6 ⁇ (: 170? 2020 /007395
  • a diffusion layer in which nitrogen is diffused in the parent phase is provided below the layer, and the nitride compound layer has a phase distribution in the order of £ phase, a′ phase, and £ phase.
  • the volume ratio of phase in the layer is 20% or more, and the nitride compound layer has a thickness of 5 to 50 from the surface of the nitrided steel member.
  • a diffusion layer in which nitrogen is diffused in the parent phase is provided below the layer, and the nitride compound layer has a phase distribution in the order of ′′ phase and £ phase.
  • the volume ratio of the ′′ phase is 30% or more, and the nitride compound layer has a thickness of 50° to 300°! from the surface of the nitrided steel member.
  • the present invention can also be recognized as an apparatus for manufacturing a nitrided steel member. That is, the present invention comprises a recycling processing furnace having a stirring fan and the guide tube, at the time of nitriding treatment, the temperature range of the recycling process furnace, controlled 6 1 0 ° ⁇ _ ⁇ 6 6 0 ° ⁇
  • a nitrided steel member is introduced such that ammonia gas and ammonia decomposition gas are introduced into the circulation type treatment furnace in order to control the nitriding potential in the circulation type treatment furnace.
  • the nitriding potential in the circulation-type treatment furnace is such that the amount of ammonia decomposition gas introduced into the furnace is constant and the amount of ammonia gas introduced into the furnace is changed. It is a device for manufacturing nitrided steel members, which is controlled to a target nitriding potential in the range of to 0.6. ⁇ 2020/175 453 7 ⁇ (: 170? 2020/007395
  • a diffusion layer in which nitrogen is diffused in the parent phase is provided below the layer, and the nitride compound layer has a phase distribution in the order of £ phase, a′ phase, and £ phase.
  • the volume ratio of phase in the layer is 20% or more, and the nitride compound layer has a thickness of 5 to 50 from the surface of the nitrided steel member.
  • a diffusion layer in which nitrogen is diffused in the parent phase is provided below the layer, and the nitride compound layer has a phase distribution in the order of ′′ phase and £ phase.
  • the volume ratio of the ′′ phase is 30% or more, and the nitride compound layer has a thickness of 50° to 300°! from the surface of the nitrided steel member.
  • the nitrided steel member of the present invention it is possible to improve wear resistance while providing sufficient hardness as the nitrided steel member.
  • a nitrided steel member having sufficient hardness and wear resistance can be manufactured.
  • a nitrided steel member having sufficient hardness and wear resistance can be manufactured.
  • FIG. 1 A cross-sectional micrograph of a nitrided steel member according to a first embodiment of the present invention.
  • Fig. 2 is a diagram showing an analysis result of the nitrided steel member of Fig. 1 by the Mitsumi three-port method. ⁇ 2020/175 453 8 ⁇ (: 170? 2020 /007395
  • FIG. 3 is a cross-sectional photomicrograph of the nitrided steel member according to the first embodiment of the present invention before being reheated.
  • Fig. 4 is a diagram showing the results of analysis of the nitrided steel member of Fig. 3 by the Mitsumi three-port method.
  • FIG. 5 A cross-sectional micrograph of a nitrided steel member according to a second embodiment of the present invention.
  • Fig. 6 is a diagram showing the results of analysis of the nitrided steel member of Fig. 5 by the Mitsumi three-port method.
  • FIG. 7 A cross-sectional micrograph of a nitrided steel member according to a second embodiment of the present invention before being reheated.
  • Fig. 8 is a diagram showing the results of analysis of the nitrided steel member of Fig. 7 by the Mitsumi three-neck method.
  • FIG. 9 A cross-sectional micrograph of a nitrided steel member as a comparative example.
  • Fig. 10 is a diagram showing an analysis result of the nitrided steel member of Fig. 9 by the Mitsumi three-port method.
  • FIG. 11 A graph showing the measurement results of hardness.
  • FIG. 12 is a schematic view of an apparatus for manufacturing a nitrided steel member according to an embodiment of the present invention.
  • FIG. 13 is a schematic cross-sectional view of a circulation type processing furnace (horizontal gas nitriding furnace).
  • FIG. 14 is a graph showing an example of gas introduction control.
  • FIG. 148 is a graph showing an example of gas introduction control.
  • FIG. 15 is a perspective view of a test piece used for a friction and wear test.
  • FIG. 16 A perspective view of a 3 V tester used for a friction and wear test.
  • FIG. 1 is a cross-sectional micrograph of a nitrided steel member 110 according to the first embodiment of the present invention.
  • the nitrided steel member 1100 of the present embodiment has a nitride compound layer 1111 formed on the surface thereof, and will be described below below the nitride compound layer 1111.
  • a hardened layer 1 12 having such an austenite structure is provided, and a diffusion layer 1 13 in which nitrogen is diffused in a matrix is provided below the hardened layer 1 12.
  • the matrix phase (matrix) of this embodiment is carbon steel having a carbon content of 0.45% by mass. ⁇ 2020/175 453 9 ⁇ (: 170? 2020 /007395
  • Fig. 1 the lower part of the nitride compound layer 1 11 and the hardened layer 1 12 appear black because they were strongly corroded by the corrosive liquid for observing the structure. Also visible above the surface is the polishing plate, not the constituent elements of the nitrided steel member.
  • the phase distribution of the nitrided steel member 110 is It can be analyzed by using together with X-ray diffraction. Specifically, as shown in Figure 2, By the 0 method, from the surface side, £ phase, The crystalline phase) and the £ phase are distributed in the order. Then, by using X-ray diffraction together, the curing layer 1 1 2 is dried. It is confirmed that the crystalline phase is the talent-stainite phase (a phase).
  • the nitride compound layer 1 11 has a thickness of about 30 from the surface of the nitrided steel member 1 10, which is 5 The thickness is within the range of ⁇ 50.
  • the surface phase is several 111 thick.
  • the volume ratio of the phase' in the nitride compound layer 1 1 1 is
  • Nitride compound layer 1 1 It can be measured based on the number of counts of'phase' and £ phase in it. Alternatively, it may be calculated by image analysis from the obtained image of FIG. In the case of the nitride compound layer 1 11 of the present embodiment, it is 41%.
  • the hardened layer 1 12 was expected to be transformed into a martensite structure by the reheating treatment.
  • the result was that most of the stratum 1 12 was the talent-phase (phase a). Therefore, the present inventor believes that the hardened layer 1 12 is strictly a mixed structure of talent and martensite.
  • the possibility that more than one type of microstructure such as a bainite structure or brownite structure may be included is not excluded.
  • the nitrided steel member 110 of the present embodiment was processed by using a circulation type processing furnace described later, processing temperature: 640°°, nitriding potential: 0.4, processing time: 2 hours. Nitrogen treatment was performed under the conditions, followed by rapid cooling, and further treatment temperature: 250 ° ⁇ , treatment time: ⁇ 2020/175 453 10 ⁇ (: 170? 2020 /007395
  • It can be manufactured by being reheated under the processing condition of 2 hours.
  • the nitrided steel member 110 as described above has a sufficient hardness for practical use because the volume ratio of the phase' in the nitride compound layer 1 11 is 41% (20% or more). (See Example 1_30 in FIG. 11 below) and wear resistance is also improved (see Example 1_30 in Table 1 below).
  • FIG. 3 For reference, a cross-sectional micrograph of the nitrided steel member 110 before reheating is shown in Fig. 3.
  • FIG. 4 is a diagram showing an analysis result of the nitrided steel member 160 of FIG. 3 by the Mimi 30 method.
  • FIG. 5 is a cross-sectional photomicrograph of the nitrided steel member 120 according to the second embodiment of the present invention.
  • the nitrided steel member 120 of the present embodiment has a nitride compound layer 1 21 formed on the surface thereof, which will be described below below the nitride compound layer 1 21.
  • the hardened layer 1 2 2 having such an austenite structure is provided, and the diffusion layer 1 2 3 in which nitrogen is diffused in the matrix is provided below the hardened layer 1 2 2.
  • the matrix phase (matrix) of the present embodiment is carbon steel having a carbon content of 0.45% by mass.
  • the lower part of the nitride compound layer 1 2 1 and the hardened layer 1 2 2 appear black because they are strongly corroded by the corrosive liquid for observing the structure. Further, what is visible above the surface is the polishing plate, not the constituent elements of the nitrided steel member.
  • the phase distribution of the nitrided steel member 120 can be analyzed by using the Mimi 30 method and X-ray diffraction in combination. Specifically, as shown in Figure 6, By the 0 method, the phase The crystalline phase) and the £ phase are distributed in this order. Then, the X-ray diffraction is also used, so that the dried crystal phase of the hardened layer 1 2 2 is stable. ⁇ 2020/175 453 1 1 ⁇ (: 170? 2020/007395
  • phase a It is confirmed that it is a night phase (phase a).
  • the nitride compound layer 1 2 1 has a thickness of about 1 2 from the surface of the nitrided steel member 1 2 0. The thickness is within the range. The surface phase is several 111 thick.
  • the volume ratio of the phase' in the nitride compound layer 1 2 1 is
  • nitride compound layer It can be measured based on the number of counts of'phase' and £ phase in it. Alternatively, it may be calculated by image analysis from the obtained image of FIG. In the case of the nitride compound layer 1 2 1 of this embodiment, it is 5 2%.
  • the hardened layer 122 was expected to be transformed into a martensite structure by the reheating treatment. However, the results of Mimi 30 shown in Fig. 6 and the X-ray diffraction method described above were used. It was confirmed by crystal structure analysis that in the hardened layer 122, a large amount of talented regions partially remained. However, depending on the steel material size after nitriding treatment, cooling conditions, and reheating conditions, the possibility of including multiple types of microstructures such as a bainite structure and brownite structure cannot be ruled out.
  • the nitrided steel member 120 of the present embodiment was treated by using a circulation type treatment furnace described later, treatment temperature: 640°°, nitriding potential: 0.2, treatment time: 2 hours. After being subjected to the nitriding treatment under the conditions, it is rapidly cooled, and then it is reheated under the treatment conditions of the treatment temperature: 250 ° C. and the treatment time: 2 hours, whereby it can be produced.
  • the nitrided steel member 120 as described above has sufficient hardness for practical use because the volume ratio of the ⁇ phase in the nitride compound layer 1 21 is 52% (30% or more). (See Example 2 _ 12 in Figure 11 below) and wear resistance is also improved (see Example 2-12 in Table 1 below).
  • FIG. 7 For reference, a cross-sectional micrograph of the nitrided steel member 120 before reheating is shown in Fig. 7.
  • FIG. 8 is a diagram showing an analysis result of the nitrided steel member 170 shown in FIG. 7 by the Mimi 30 method.
  • FIG. 9 is a cross-sectional micrograph of a nitrided steel member 300 of Comparative Example.
  • the nitrided steel member 300 of the comparative example has a nitride compound layer 3001 formed on the surface thereof, and nitrogen is present in the matrix below the nitride compound layer 301. It has a diffusion layer 303 that is diffused.
  • the parent phase (base material) of the comparative example is also carbon steel having a carbon content of 0.45% by mass.
  • the surface side of the compound layer obtained by the conventional general nitriding treatment is porous.
  • the upper part of the nitride compound layer 301 appears black because there are many fine voids in this region. Further, what is seen above the surface is the polishing plate, not the constituent elements of the nitrided steel member.
  • the phase distribution of the nitrided steel member 300 can also be analyzed by using the Mimi 30 method and X-ray diffraction in combination. Specifically, as shown in FIG. By the 0 method, it can be seen that most of the nitride compound layer 301 is in the phase.
  • the nitride compound layer 3001 has a thickness of about 17 from the surface of the nitrided steel member 300.
  • the nitrided steel member 300 of the comparative example was processed using a circulation type processing furnace described below, with a processing temperature of 5800°, a nitriding potential of 2.5, and a processing time of 2 hours. After the soft nitriding process is performed (atmosphere gas is ammonia, nitrogen gas and carbon dioxide gas), it can be rapidly cooled to be manufactured. It has been confirmed that the nitride compound layer 301 of the comparative example does not cure even if it is subjected to the reheating treatment (probably because the temperature during the soft nitriding treatment is relatively low).
  • nitrided steel member 300 As described above, most of the nitride compound layer 3001 is the ⁇ phase, and conventionally, this hard phase was used to improve the wear resistance.
  • the surface hardness was insufficient as compared with the compound layer formed by the nitriding treatment of the present invention (see the comparative example in Fig. 11 described later), which adversely affects the wear resistance and the wear resistance. Abrasion is also insufficient (see Comparative Example in Table 1 below). ⁇ 2020/175 453 13 ⁇ (: 170? 2020 /007395
  • voids which appear black in Fig. 9 are formed on the surface side of the nitride compound layer 3001. To be done. Since the void (porous) can be the starting point of crack initiation, its presence is not preferable.
  • Figure 11 is a graph showing the results of hardness measurement.
  • the nitride compound layer was used.
  • the hardness in the vicinity of the surface is slightly lower than 8 0 0 1 to 1 V, which is not sufficient. ..
  • the hardness decreases toward the inside, but the hardness near the surface is sufficiently high.
  • the hardness in the vicinity of the surface has a 6 0 0 1 - about 1 V, not sufficient.
  • the thickness of the nitride compound layer 1 11 of the nitrided steel member 110 according to the first embodiment generally, the thicker the thickness, the larger the allowable wear amount, and therefore the more preferable.
  • the thickness of 11 was 50 (see Example 1_50 in Table 1 below). Therefore, the maximum value of the thickness of the nitride compound layer 1 11 which can be recognized by those skilled in the art as solving the problem of the present invention is set to 50
  • the inventors of the present invention have confirmed that the thickness of the nitride compound layer 1 11 tends to increase when the nitriding potential during the nitriding treatment is high.
  • the thickness of the nitride compound layer 1 21 of the nitrided steel member 120 of the second embodiment generally, it can be said that the thicker the thickness, the larger the allowable wear amount, which is preferable.
  • the present inventor has a tendency that the carbon compound steel generally used for gears has a low carbon content (specifically, for example, 3 15 (3 steel), the nitride compound layer 1 2 1 tends to be thick. . confirmed direction and, specifically, 3 1 5 (3 steel processing temperature: 6 5 0 ° ⁇ , nitriding potential:. 0 2, treatment time: to nitriding treatment for 2 hours, and quenched
  • the treatment temperature was 250° C. and the treatment time was 2 hours
  • the nitride compound layer 1 21 had a thickness of 30 (see Examples 2 to 30 in Table 1 below). Therefore, the maximum value of the thickness of the nitride compound layer 1 11 which can be recognized by those skilled in the art as solving the problem of the present invention is set to 30
  • the present inventor has confirmed that the thickness of the nitride compound layer 1 2 1 also tends to increase when the nitriding potential during the nitriding treatment is high.
  • the inventor of the present invention has confirmed that a larger volume ratio of phases in the nitride compound layer 1 1 1 is preferable for increasing hardness.
  • the minimum value concretely, 3500 steel is treated at a treatment temperature of 6400°, a nitriding potential of 0.6, and a treatment time of 2 hours.
  • the volume ratio of the ⁇ phase in the nitride compound layer 11 was 20% (Example 1_ in Table 1 below). See 50). Therefore, the minimum value of the volume ratio of the phase in the nitride compound layer 1 11 which can be recognized by those skilled in the art as solving the problem of the present invention is set to 20%.
  • the present inventor has confirmed that the larger the volume ratio of the ⁇ phase in the nitride compound layer 1 21 is, the better it is to increase the hardness.
  • the nitriding potential% is defined by the following equation (2).
  • the nitriding potential is known as an index showing the nitriding ability of the atmosphere in the gas nitriding furnace.
  • the nitriding potential can be calculated. That is, the hydrogen and nitrogen generated are 1.5 mol and 0.5 mol, respectively, from 1 mol of ammonia. Therefore, measuring the ammonia concentration in the furnace also reveals the hydrogen concentration in the furnace, and It can be calculated. Alternatively, if the hydrogen concentration in the furnace is measured, the ammonia concentration in the furnace can be known, and the nitriding potential can also be calculated.
  • the ammonia gas flown in the gas nitriding furnace is circulated in the furnace and then discharged to the outside of the furnace. That is, in the gas nitriding process, the fresh (new) ammonia gas constantly flows into the furnace with respect to the existing gas in the furnace, so that the existing gas is continuously discharged outside the furnace (pushed out by the supply pressure). ..
  • Fig. 12 is a schematic diagram showing a manufacturing apparatus for manufacturing a nitrided steel member according to an embodiment of the present invention.
  • the manufacturing apparatus 1 of the present embodiment is provided with a circulation type treatment furnace 2, and only two types of gas, ammonia and ammonia decomposition gas, are introduced into the circulation type treatment furnace 2. I am using.
  • Ammonia decomposition gas also called 8X gas, is a mixed gas consisting of nitrogen and hydrogen in a ratio of 1:3.
  • FIG. 13 shows an example of a cross-sectional structure of the circulation type processing furnace 2.
  • a cylinder 20 2 called a retort is arranged in a furnace wall (also called a bell) 201, and a cylinder 20 4 called an inner retort is arranged inside the cylinder.
  • a furnace wall also called a bell
  • the introduction gas supplied from the gas introduction pipe 205 passes through the periphery of the object to be treated as shown by the arrow in the figure, and then the two stirring cylinders 2 0 2 and 2 2 are operated by the stirring fan 2 0 3. It circulates through the space between 0 and 4.
  • Reference numeral 206 is a gas hood with flare, 207 is a thermocouple, 208 is a lid for cooling work, and 209 is a fan for cooling work.
  • the circulation type processing furnace 2 is also called a horizontal gas nitriding furnace, and its structure itself is known.
  • the object to be treated 3 is carbon steel or low alloy steel, and is, for example, a crankshaft, a gear or the like which is an automobile part.
  • the processing furnace 2 of the surface hardening processing apparatus 1 of the present embodiment includes a furnace opening/closing lid 7, a stirring fan 8, a stirring fan drive motor 9, and an atmosphere gas concentration.
  • a detector 3, a nitriding potential controller 4, a programmable logic controller 31 and an in-furnace introduced gas supply unit 20 are provided.
  • the stirring fan 8 is arranged in the processing furnace 2 and rotates in the processing furnace 2 to stir the atmosphere in the processing furnace 2.
  • the stirring fan drive motor 9 is connected to the stirring fan 8 so as to rotate the stirring fan 8 at an arbitrary rotation speed.
  • the atmosphere gas concentration detecting device 3 is composed of a sensor capable of detecting the hydrogen concentration or the ammonia concentration in the processing furnace 2 as the atmosphere gas concentration in the furnace.
  • the main body of detection of the sensor communicates with the inside of the processing furnace 2 through an atmospheric gas pipe 12.
  • the atmospheric gas pipe 12 is formed in a path that directly connects the sensor main body of the atmospheric gas concentration detection device 3 and the processing furnace 2, and is connected to the exhaust gas combustion decomposition device 41 on the way. Furnace gas disposal pipe 40 is connected. As a result, the atmospheric gas is distributed between the discarded gas and the gas supplied to the atmospheric gas concentration detection device 3.
  • the atmospheric gas concentration detecting device 3 is configured to detect the atmospheric gas concentration in the furnace and then output an information signal including the detected concentration to the nitriding potential controller 4.
  • the nitriding potential controller 4 includes an in-furnace nitriding potential computing device 13 ⁇ 2020/175 453 18 ⁇ (: 170? 2020 /007395
  • the programmable logic controller 31 has a gas introduction amount control device 14 and a parameter setting device 15.
  • the in-furnace nitriding potential calculation device 13 is configured to calculate the nitriding potential in the processing furnace 2 based on the hydrogen concentration or the ammonia concentration detected by the in-furnace atmosphere gas concentration detection device 3. .. Specifically, a formula for calculating the nitriding potential programmed according to the actual gas introduced in the furnace is incorporated, and the nitriding potential is calculated from the value of the atmospheric gas concentration in the furnace.
  • the parameter setting device 15 is composed of, for example, a touch panel, and can set and input the total flow rate of gas introduced into the furnace, the gas type, the processing temperature, the target nitriding potential, and the like. Each setting parameter value input by setting is transmitted to the gas flow rate output adjusting device 30.
  • the gas flow rate output adjusting device 30 is connected to the in-reactor nitriding potential calculating device 1
  • Control is performed with the nitriding potential calculated in step 3 as the output value, the target nitriding potential (set nitriding potential) as the target value, and the input amounts of ammonia gas and ammonia decomposition gas as input values. It has become. More specifically, it is possible to control the amount of ammonia decomposition gas introduced into the furnace to be constant and to change the amount of ammonia gas introduced into the furnace.
  • the output value of the gas flow rate output adjusting device 30 is transmitted to the gas introduction amount control device 14.
  • the gas introduction amount control device 14 includes a first supply amount control device 2 2 for ammonia gas and a second supply amount control device 26 for ammonia decomposition gas so as to realize the introduction amount of each gas. Each is designed to send a control signal.
  • the in-furnace introduced gas supply unit 20 of the present embodiment includes a first in-reactor introduced gas supply unit 21 for ammonia gas, a first supply amount control device 2 2 and a first supply valve 2 3 And a first flow meter.
  • the in-reactor introduction gas supply unit 20 of the present embodiment includes a second in-reactor introduction gas supply unit 25 for ammonia decomposition gas (eight gas), ⁇ 2020/175 453 19 ⁇ (: 170? 2020 /007395
  • It has a supply amount control device 26, a second supply valve 27, and a second flow meter.
  • the ammonia gas and the ammonia decomposition gas are adapted to be mixed in the furnace introduction gas introduction pipe 29 before entering the processing furnace 2.
  • the first-reactor-introduced-gas supply unit 21 is formed of, for example, a tank filled with the first-reactor-introduced gas (in this example, ammonia gas).
  • the first supply amount control device 22 is formed by a mass flow controller and is interposed between the first in-reactor introduced gas supply part 21 and the first supply valve 23.
  • the opening degree of the first supply amount control device 22 changes according to the control signal output from the gas introduction amount control device 14. Further, the first supply amount control device 22 detects the supply amount from the first in-furnace introduced gas supply part 21 to the first supply valve 23, and outputs an information signal including the detected supply amount to the gas introduction amount. It is designed to output to the control unit 14.
  • the control signal can be used for correction of the control by the gas introduction amount control device 14 or the like.
  • the first supply valve 23 is formed by a solenoid valve that switches between open and closed states in accordance with a control signal output from the gas introduction amount control device 14 and is connected to the first supply amount control device 2 2 and the first flow rate. It is installed between the instrument and the instrument.
  • the second-reactor-introduced-gas supply unit 25 is formed by, for example, a tank filled with the second-reactor-introduced gas (in the present example, an ammonia decomposition gas).
  • the second supply amount control device 26 is formed by a mass flow controller and is interposed between the second in-furnace introduced gas supply part 25 and the second supply valve 27.
  • the opening degree of the second supply amount control device 26 changes according to the control signal output from the gas introduction amount control device 14. Further, the second supply amount control device 26 detects the supply amount from the second in-furnace introduced gas supply unit 25 to the second supply valve 27, and outputs an information signal including the detected supply amount to the gas introduction amount. It is designed to output to the control unit 14.
  • the control signal can be used for correction of the control by the gas introduction amount control device 14 or the like.
  • the second supply valve 27 is formed by a solenoid valve that switches between open and closed states in accordance with a control signal output by the gas introduction amount control device 14 and the second supply amount control device 2 ⁇ 0 2020/175453 20 ?01/1?2020/007395
  • the article to be treated 3 is put into the circulation type processing furnace 2 and the circulation type processing furnace 2 is heated to a desired processing temperature.
  • a mixed gas of ammonia gas and ammonia decomposition gas or only ammonia gas is introduced into the processing furnace 2 from the in-furnace introduction gas supply unit 20 at a set initial flow rate.
  • This set initial flow rate can also be set and input in the parameter setting device 15 and is controlled by the first supply amount control device 2 2 and the second supply amount control device 2 6 (both mass flow controllers).
  • the stirring fan drive motor 9 is driven to rotate the stirring fan 8 to stir the atmosphere in the processing furnace 2.
  • the in-reactor nitriding potential calculator 13 of the nitriding potential controller 4 calculates the in-reactor nitriding potential (it is an extremely high value at the beginning (because there is no hydrogen in the furnace), the Decrease as the decomposition (hydrogen generation) progresses), and determine whether it is below the sum of the target nitriding potential and the standard deviation value.
  • This reference deviation value can also be set and input in the parameter setting device 15.
  • the nitriding potential controller 4 causes the in-reactor amount control device 1 Control of the amount of introduced gas is started.
  • the in-furnace nitriding potential calculator 13 of the nitriding potential controller 4 calculates the in-furnace nitriding potential based on the input hydrogen concentration signal or ammonia concentration signal. Then, the gas flow rate output adjusting device 30 sets the nitriding potential calculated by the in-furnace nitriding potential calculating device 13 as an output value, sets the target nitriding potential (set nitriding potential) as the target value, and introduces it into the furnace. Perform I 0 control with the input amount of gas. Specifically, in the I port control, control is performed so that the amount of ammonia decomposition gas introduced into the reactor is constant and the amount of ammonia gas introduced into the reactor is changed. Concerned ⁇ 2020/175 453 21 ⁇ (: 170? 2020 /007395
  • each set parameter value set and input by the parameter setting device 15 is used.
  • this setting parameter value for example, different values are prepared depending on the value of the target nitriding potential.
  • the gas flow rate output control device 30 controls the introduction amount of each of the in-reactor introduced gas as a result of the I port control. Specifically, the gas flow rate output adjusting device 30 determines the flow rate of each gas, and the output value is transmitted to the gas introduction amount control device 14.
  • the gas introduction amount control device 14 includes a first supply amount control device 2 2 for ammonia gas and a second supply amount control device 26 for ammonia decomposition gas in order to realize the introduction amount of each gas. To each of the control signals.
  • the in-furnace nitriding potential can be stably controlled in the vicinity of the target nitriding potential.
  • the amount of ammonia decomposed gas introduced into the furnace is constant, and feedback control is performed in small increments in the vicinity of the amount of ammonia gas introduced into the furnace of 40 ( ⁇ / ⁇ ! ⁇ 11).
  • the nitriding potential is controlled to 0.17 with high accuracy.
  • the manufacturing apparatus 1 can also perform the cooling step after the nitrification treatment.
  • the workpiece 3 is removed from the furnace while the heating temperature is maintained after the nitrification treatment in the manufacturing apparatus 1. It is necessary to transfer to a rapid cooling device (eg oil tank) and then to quench.
  • a rapid cooling device eg oil tank
  • Friction and wear as shown in Fig. 16 was carried out on 345 ⁇ steel (test piece) having the shape ( ⁇ 25 X80101 size) as shown in Fig. 15 under the conditions shown in Table 1 below.
  • the abrasion resistance was evaluated using a tester (Ovitimol, Germany: vibration friction wear tester 3 V 4).
  • a ball of silicon nitride of ⁇ 10 (hardness: about 16001 to 1) is used, and it is used under the condition of dry type (room temperature 25 ° (:, humidity 30%, no lubricant)). Then, reciprocal sliding is repeated while applying a load of 10 (amplitude 1, 501 to 12,
  • 401 is an oscillation block head plate
  • 4023 is a torsion sensor
  • 402 is a test piece fixture
  • 4033 is the upper specimen holder and 404 is the vertical load axis.
  • Example 1_30 in Table 1 corresponds to the nitrided steel member 110 of the first embodiment described with reference to FIGS. 1 and 2.
  • the circulation treatment furnace 2 was used to perform the nitriding treatment under the treatment conditions of treatment temperature: 640°, nitriding potential: 0.4, treatment time: 2 hours. After that, it was rapidly cooled, and then it was reheated under the treatment conditions of treatment temperature: 250 ° ⁇ , treatment time: 2 hours (manufacturing phase: 3 4 5 (3 steel)).
  • phase distribution of the nitride compound layer is in the order of £ phase, ⁇ phase, and £ phase, and the thickness of the nitride compound layer is about 300! From the surface of the nitrided steel member. * ⁇
  • the volume ratio of the' phase was 41%.
  • Example 1_36 is a nitrided steel member manufactured by changing the nitriding potential during nitrification treatment to 0.5 in comparison with Example 1_30.
  • phase distribution of the nitride compound layer is in the order of £ phase, ⁇ phase, and £ phase, and the thickness of the nitride compound layer is approximately 360° from the surface of the nitrided steel member. * ⁇
  • the volume ratio of the' phase was 33%.
  • nitrided steel members of Examples 1 to 36 as described above also provided a sufficient hardness distribution as generally indicated by the black triangle points in Fig. 11 and, as shown in Table 1, It was confirmed to provide low maximum wear (sufficient friction wear properties).
  • Example 1_40 is a nitrided steel member produced by changing the nitriding potential at the time of nitrification treatment to 0.6 in comparison with Example 1_30.
  • phase distribution of the nitride compound layer is in the order of £ phase, ⁇ phase, £ phase, and the thickness of the nitride compound layer is about 4001 from the surface of the nitrided steel member. * ⁇
  • the volume ratio of the' phase was 24%.
  • Example 1-50 was produced by changing the matrix phase to 350 (3 steel) and the nitriding potential during nitrification treatment to 0.6 compared to Example 1-30. It is a nitrided steel member.
  • phase distribution of the nitride compound layer is in the order of £ phase, ⁇ phase, and £ phase, and the thickness of the nitride compound layer is about 500! From the surface of the nitrided steel member. * ⁇
  • the volume ratio of the ‘phase’ was 20%.
  • nitrided steel members of Examples 1 to 50 described above also provided a sufficient hardness distribution as generally indicated by the black triangle points in Fig. 11 and, as shown in Table 1, It was confirmed to provide low maximum wear (sufficient friction wear properties).
  • Example 1_15 is a nitrided steel member produced by changing the nitriding temperature during the nitriding treatment to 6200° as compared with Example 1_30.
  • the phase distribution of the nitride compound layer is in the order of'phase' and £ phase, and the thickness of the nitride compound layer is about 15 from the surface of the nitrided steel member.
  • the volume ratio was 37%.
  • nitrided steel members of Examples 1 to 15 like this also provided a sufficient hardness distribution as indicated by the white circles in Fig. 11 and had a low hardness as shown in Table 1. It was confirmed to provide maximum wear (sufficient friction wear characteristics).
  • Example 1 — 30 Example 1 — 36, and Example 1 — 40
  • the state before the reheating treatment was respectively Reference Example 1 _ 3 0, Reference Example 1 _ 3 6, Reference Example 1 _ 4
  • the hardness and the maximum wear amount were evaluated as 0.
  • Example 2-12 in Table 1 corresponds to the nitrided steel member 120 of the second embodiment described with reference to FIGS. 5 and 6.
  • the Example 2 _ 1 2 was subjected to a nitriding treatment using the above-mentioned circulation type treatment furnace 2 under the treatment conditions of treatment temperature: 640° ⁇ , nitriding potential: 0.2, treatment time: 2 hours. After that, it was rapidly cooled, and then it was reheated under the treatment conditions of treatment temperature: 250 ° ⁇ , treatment time: 2 hours (manufacturing phase: 3 4 5 (3 steel)).
  • the phase distribution of the nitride compound layer is in the order of'phase' and £ phase, and the thickness of the nitride compound layer is about 12 from the surface of the nitrided steel member.
  • the volume ratio of was 52%.
  • Example 2_7 is a nitrided steel member manufactured by changing the nitriding potential at the time of nitrification treatment to 0.18 as compared with Example 2-12.
  • the phase distribution of the nitride compound layer is in the order of'phase' and £ phase, and the thickness of the nitride compound layer is about 7 from the surface of the nitrided steel member.
  • the volume ratio was 60%.
  • the nitrided steel members of Examples 2 to 7 also provided a sufficient hardness distribution as generally indicated by the white circles in Fig. 11 and had a low maximum maximum as shown in Table 1. It was confirmed to provide the amount of wear (sufficient friction and wear characteristics).
  • Example 2 _ 16 is a nitrided steel member manufactured by changing the nitriding temperature at the time of nitrification treatment to 6 3 ⁇ ° ⁇ and the nitriding potential to 0.25 in comparison with Example 2 _ 1 2. is there.
  • phase distribution of the nitride compound layer is in the order of'phase' and £ phase, and the thickness of the nitride compound layer is about 16 from the surface of the nitrided steel member. of ⁇ 2020/175 453 26 ⁇ (: 170? 2020/007395
  • the volume ratio was 45%.
  • Such a nitrided steel member of Example 2 _ 16 also provided a sufficient hardness distribution as generally indicated by the white circles in Fig. 11 and had a low hardness as shown in Table 1. It was confirmed to provide maximum wear (sufficient friction wear characteristics).
  • Example 2-30 is different from Example 2-12 in that the matrix phase is changed to 3 15 (3 steel, and the nitriding temperature at the time of the nitriding treatment is 650°° and the nitriding potential is 0°. It is a nitrided steel member manufactured by changing to .2.
  • the phase distribution of the nitride compound layer is in the order of A'phase and £ phase, and the thickness of the nitride compound layer is about 30 from the surface of the nitrided steel member.
  • the volume ratio of was 30%.
  • the nitrided steel members of Examples 2-30 also provided a sufficient hardness distribution as indicated by the white circles in Fig. 11 and had a low hardness as shown in Table 1. It was confirmed to provide maximum wear (sufficient friction wear characteristics).

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Abstract

La présente invention concerne un élément en acier de nitruration, dans lequel une phase de matrice est composée d'un acier au carbone ou d'un acier faiblement allié, l'élément en acier de nitruration étant caractérisé par une couche de composé de nitrure se situant sur sa surface, une couche durcie présentant une structure d'austénite se situant sous la couche de composé de nitrure, et une couche diffusée, dans laquelle de l'azote est diffusé dans la phase de matrice, se situant sous la couche durcie. La couche de composé de nitrure comporte une distribution de phases dans laquelle une phase ε, une phase γ' et une phase ε sont agencées dans cet ordre, le rapport volumique de la phase γ' dans la couche de composé de nitrure étant supérieure ou égale à 20 %, et la couche de composé de nitrure présente une épaisseur de 5 à 50 µm depuis la surface de l'élément en acier de nitruration.
PCT/JP2020/007395 2019-02-26 2020-02-25 Élément en acier de nitruration, et procédé et dispositif de fabrication d'élément en acier de nitruration Ceased WO2020175453A1 (fr)

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WO2022215526A1 (fr) * 2021-04-09 2022-10-13 パーカー熱処理工業株式会社 Appareil et procédé de traitement de durcissement de surface

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WO2012035900A1 (fr) * 2010-09-14 2012-03-22 日本パーカライジング株式会社 Élément fer/acier ayant une couche d'un composé de l'azote et son procédé de fabrication
JP2014047410A (ja) * 2012-09-03 2014-03-17 Yuki-Koushuha Co Ltd 鉄基合金材及びその製造方法
WO2015136917A1 (fr) * 2014-03-13 2015-09-17 新日鐵住金株式会社 Procédé de nitruration et procédé de fabrication de composé nitruré
WO2019131602A1 (fr) * 2017-12-27 2019-07-04 パーカー熱処理工業株式会社 Élément en acier nitruré, et procédé et appareil de production d'élément en acier nitruré

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WO2012035900A1 (fr) * 2010-09-14 2012-03-22 日本パーカライジング株式会社 Élément fer/acier ayant une couche d'un composé de l'azote et son procédé de fabrication
JP2014047410A (ja) * 2012-09-03 2014-03-17 Yuki-Koushuha Co Ltd 鉄基合金材及びその製造方法
WO2015136917A1 (fr) * 2014-03-13 2015-09-17 新日鐵住金株式会社 Procédé de nitruration et procédé de fabrication de composé nitruré
WO2019131602A1 (fr) * 2017-12-27 2019-07-04 パーカー熱処理工業株式会社 Élément en acier nitruré, et procédé et appareil de production d'élément en acier nitruré

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Publication number Priority date Publication date Assignee Title
WO2022215526A1 (fr) * 2021-04-09 2022-10-13 パーカー熱処理工業株式会社 Appareil et procédé de traitement de durcissement de surface

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