US20240229178A9 - Nitriding treatment method for steel component - Google Patents

Nitriding treatment method for steel component Download PDF

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US20240229178A9
US20240229178A9 US18/546,438 US202218546438A US2024229178A9 US 20240229178 A9 US20240229178 A9 US 20240229178A9 US 202218546438 A US202218546438 A US 202218546438A US 2024229178 A9 US2024229178 A9 US 2024229178A9
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gas
nitriding
nitriding treatment
treatment step
potential
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US20240132985A1 (en
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Yasushi Hiraoka
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Parker Netsushori Kogyo KK
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Parker Netsushori Kogyo KK
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C21D8/0257—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C8/34—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

Definitions

  • JP-A-2013-221203 JP application number 2012-095035 (Patent Document 1) has disclosed that, in order to improve a pitting resistance and/or flexural fatigue strength of a steel component, it is effective to produce an iron nitride compound layer having a ⁇ ′ phase as a main component on a surface of the steel component by a nitriding treatment.
  • JP-B-6378189 has disclosed a nitriding treatment method including a first nitriding treatment step in which a nitriding treatment is performed to a steel component under a nitriding gas atmosphere of a nitriding potential for generating a nitride compound layer of a ⁇ ′ phase or an c phase, and a second nitriding treatment step in which another nitriding treatment is performed to the steel component under another nitriding gas atmosphere of another nitriding potential lower than that of the first nitriding treatment step resulting in deposition of a ⁇ ′ phase in the nitride compound layer, in order to suppress variation in mass production.
  • a gas nitriding treatment performed at a temperature of 600° C. using two types of gases which are an NH 3 gas and an H 2 gas, is described as an example. More specifically, at a temperature of 600° C., a range of 0.6 to 1.51 is adopted for the nitriding potential in the first nitriding treatment step, and a range of 0.16 to 0.25 is adopted for the nitriding potential in the second nitriding treatment step.
  • the action (reaction) in which the ⁇ ′ phase is deposited in the nitride compound layer is affected by both the nitriding potential and the furnace temperature.
  • the nitriding potential at the second nitriding treatment step is set to be 0.25 or less, an a phase which is lower in hardness than the ⁇ ′ phase is also deposited. This results in an insufficient pitting resistance and/or an insufficient bending fatigue strength.
  • the effectiveness of the present invention wherein the first nitriding treatment step is performed at a temperature within a range of 500° C. to 590° C., wherein the second nitriding treatment step is also performed at a temperature within a range of 500° C. to 590° C., wherein the first nitriding potential is a value within a range of 0.300 to 10.000, and wherein the second nitriding potential is lower than the first nitriding potential and is a value within a range of 0.253 to 0.600, has been proved.
  • the effectiveness of the present invention wherein the first nitriding treatment step is performed at a temperature within a range of 500° C. to 590° C., wherein the second nitriding treatment step is also performed at a temperature within a range of 500° C. to 590° C., wherein the first nitriding potential is a value within a range of 0.300 to 10.000, and wherein the second nitriding potential is lower than the first nitriding potential and is a value within a range of 0.253 to 0.600, has been
  • FIG. 5 is a schematic view showing a structure of a horizontal type thermal processing furnace (one-chamber type of thermal processing furnace) to be used for a nitriding treatment method according to the present invention:
  • FIG. 10 is a table showing nitriding conditions and treatment results of examples and comparative examples of the present invention.
  • An inlet hood 22 having an openable and closable door 21 is attached to an inlet side (left side in FIG. 1 ) of the heating chamber 11 .
  • the heating chamber 11 has a retort structure, and an outer periphery of the retort structure is configured to be heated by a heater (not shown) so that a temperature in the furnace (chamber) is controlled to a predetermined temperature.
  • a plurality of types of gases for the nitriding treatment are configured to be introduced into the heating chamber 11 while being controlled as described below.
  • a fan 26 is mounted on a ceiling of the heating chamber 11 to stir the gases introduced into the heating chamber 11 so that a heating temperature for the steel component is made uniform therein.
  • An openable and closable intermediate door 27 is attached to an exit side (right side in FIG. 1 ) of the heating chamber 11 .
  • the case 20 that contains the steel component is loaded into the heating chamber 11 from the loading section 10 by a pusher or the like.
  • the steel component the case that contains the steel component
  • the plurality of types of process gases are introduced into the heating chamber 11 , and the process gases are heated to a predetermined temperature by the heater and stirred by the fan 26 (for example, rotating at 1500 rpm) so that the steel component loaded into the heating chamber 11 is subjected to the nitriding treatment.
  • FIG. 2 is a process diagram of an embodiment of the nitriding treatment method according to the present invention in a case wherein the thermal processing furnace 1 shown in FIG. 1 is used.
  • a steel component (work) is loaded into the heating chamber 11 .
  • the door 21 is opened, and thus the temperature in the heating chamber 11 is temporarily lowered as shown in FIG. 2 . Thereafter, the door 21 is closed and the temperature in the heating chamber 11 is heated again to 550° C.
  • a nitriding potential K N is represented by the following formula using P(NH 3 ) which is a partial pressure of the NH 3 gas and P(H 2 ) which is a partial pressure of the H 2 gas.
  • P(NH 3 ) i.e. a partial pressure of the NH 3 gas in the heating chamber 11 or P(H 2 ) i.e. a partial pressure of the H 2 gas in the heating chamber 11 is measured.
  • the introduction amounts (flow rates) of the process gases are subjected to a feedback control in such a manner that a nitriding potential calculated from the measured value is brought into the vicinity of the first nitriding potential, which is a target nitriding potential.
  • P(H 2 ) i.e. a partial pressure of the H 2 gas in the heating chamber 11 is measured by a heat conduction type H 2 sensor (not shown), the measured value is analyzed online (so that a nitriding potential is calculated from the measured value), and the introduction amounts (flow rates) of the process gases are subjected to a feedback control.
  • the first nitriding treatment step is performed for 240 minutes.
  • a nitride compound layer consisting of a ⁇ ′ phase, or an ⁇ phase, or mixture of a ⁇ ′ phase and an ⁇ phase, is generated in the steel component.
  • a value of 0.300 (an example of a value within a range of 0.253 to 0.600) is employed as a second nitriding potential, and a second nitriding treatment step is performed at a temperature of 550° C.
  • P(H 2 ) i.e. a partial pressure of the H 2 gas in the heating chamber 11 is measured by the heat conduction type H 2 sensor (not shown), the measured value is analyzed online (so that a nitriding potential is calculated from the measured value), and the introduction amounts (flow rates) of the process gases are subjected to a feedback control.
  • the introduction amounts (flow rates) of the NH 3 gas and the AX gas are respectively increased or decreased while keeping the sum (total) amount of the two gases to be 160 (L/min).
  • the second nitriding treatment step is performed for 60 minutes. Thereby, a ⁇ ′ phase is deposited in the nitride compound layer.
  • a cooling step is performed.
  • the cooling step is performed for 15 minutes (the case 20 is held in the oil bath (100° C.) for 15 minutes, the oil bath being provided with a stirrer).
  • the case 20 that contains the steel component is unloaded onto the unloading conveyor 13 .
  • the pit type thermal processing furnace 201 includes a bottomed cylindrical furnace wall 211 and a furnace lid 212 .
  • a fan 213 is provided on a lower (inner) side of the furnace lid 212 .
  • a rotation shaft of the fan 213 passes through the furnace lid 212 , and is connected to a fan motor 214 , which is provided on an upper (outer) side of the furnace lid 212 .
  • a retort 221 is provided inside the furnace wall 211 .
  • a gas guide tube 222 is provided further inside the retort 221 .
  • An outer periphery of the retort 221 is configured to be heated by a heater (not shown) so that a temperature in the furnace (in the retort 221 ) is controlled to a predetermined temperature.
  • a case is configured to be placed into the gas guide tube 222 .
  • a steel component as an object to be processed (work) is configured to be contained in the case 20 .
  • the maximum gross weight to be processed is 700 kg.
  • a plurality of types of gases for the nitriding treatment are configured to be introduced into the retort 221 while being controlled as described below.
  • the outer periphery of the retort 221 has a cooling function by a blower (not shown). When cooled, a temperature of the retort 221 itself is lowered, and thus the temperature in the furnace (in the retort 221 ) is lowered (furnace cooling).
  • the furnace lid 212 is opened, and the case 20 that contains the steel component is loaded into the gas guide tube 222 .
  • the plurality of types of process gases are introduced into the gas guide tube 222 , and the process gases are heated to a predetermined temperature by the heater and stirred by the fan 213 (for example, rotating at 1500 rpm) so that the steel component loaded into the gas guide tube 222 is subjected to the nitriding treatment.
  • FIG. 4 is a process diagram of an embodiment of the nitriding treatment method according to the present invention in a case wherein the thermal processing furnace 201 shown in FIG. 3 is used.
  • the inside of the retort 221 is heated to 550° C.
  • an N 2 gas is introduced at a constant flow rate of 40 (L/min).
  • an NH 3 gas is introduced at a constant flow rate of 40 (L/min).
  • a nitriding potential K N is represented by the following formula using P(NH 3 ) which is a partial pressure of the NH 3 gas and P(H 2 ) which is a partial pressure of the H 2 gas.
  • P(H 2 ) i.e. a partial pressure of the H 2 gas in the gas guide tube 222 is measured by the heat conduction type H 2 sensor (not shown), the measured value is analyzed online (so that a nitriding potential is calculated from the measured value), and the introduction amounts (flow rates) of the process gases are subjected to a feedback control.
  • the introduction amount (flow rate) of the NH 3 gas is increased or decreased while the AX gas is introduced at a constant flow rate of 30 (L/min). In this case, the total amount of the two gases is also increased or decreased.
  • the process diagram shown in FIG. 4 is also applicable in a case wherein the horizontal type thermal processing furnace is used. Specifically, the heating step (introduction manners of the process gases are different between a former half thereof and a latter half thereof), the first nitriding treatment step, the second nitriding treatment step and the cooling step may be performed. After the cooling step has been completed, the furnace lid 212 is opened, and the case 20 that contains the steel component is unloaded from the gas guide tube 222 .
  • the nitriding treatment according to the present invention is performed at a temperature not higher than the austenite transformation temperature, so that an amount of strain is small.
  • a quenching step which is necessary for a carburizing treatment or a nitrocarburizing treatment, can be omitted, so that an amount of strain variation is small. As a result, a high-strength and low-strain nitrided steel member can be obtained.
  • the temperature of each nitriding treatment step is 500° C. to 590° C. It is said that, when the temperature of a nitriding treatment step is higher, the productivity thereof is better. However, according to the inventor's verification, if the temperature of a nitriding treatment step is higher than 590° C., an amount (degree) of hardening is reduced and an austenite layer is formed on the surface. Thus, it is preferable that 590° C. is the upper limit. On the other hand, according to the inventor's verification, if the temperature of a nitriding treatment step is lower than 500° C., a formation speed of the nitride compound layer is slow, which is not cost effective. Thus, it is preferable that 500° C. is the lower limit.
  • a first nitriding treatment step and a second nitriding treatment step were performed in sequence in the same batch type of thermal processing furnace 1 .
  • the comparative examples 1-1 to 1-4 have proved that an a phase which is lower in hardness than the ⁇ ′ phase was deposited, resulting in an insufficient pitting resistance and an insufficient bending fatigue strength.
  • a two-stage nitriding treatment was performed according to the conditions of Table 2 shown in FIG. 7 .
  • a first nitriding treatment step and a second nitriding treatment step were performed in sequence in the same pit type thermal processing furnace 201 .
  • the first nitriding treatment step of each of the examples 2-1 to 2-9 and the comparative examples 2-1 to 2-4 three types of gases, which are an NH 3 gas, an AX gas and an N 2 gas, were used, and a nitriding potential during the first nitriding treatment step was controlled to be close to the first nitriding potential (K N ), which is a target nitriding potential, by changing an introduction amount of each of the NH 3 gas and the AX gas while keeping a total introduction amount of the three types of gases constant.
  • K N is a target nitriding potential
  • the comparative examples 3-1 to 3-4 have proved that an a phase which is lower in hardness than the ⁇ ′ phase was deposited, resulting in an insufficient pitting resistance and an insufficient bending fatigue strength.
  • a two-stage nitriding treatment was performed according to the conditions of Table 4 shown in FIG. 9 .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Articles (AREA)
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WO2018062290A1 (ja) * 2016-09-30 2018-04-05 Ｄｏｗａサーモテック株式会社 連続窒化処理炉および連続窒化処理方法
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US20240132985A1 (en) 2024-04-25
WO2022176878A1 (ja) 2022-08-25
CN116917529A (zh) 2023-10-20
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TW202237866A (zh) 2022-10-01
KR102878198B1 (ko) 2025-10-28

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