EP2085493A1 - Process for producing high-concentration carburized steel - Google Patents

Process for producing high-concentration carburized steel Download PDF

Info

Publication number
EP2085493A1
EP2085493A1 EP07830687A EP07830687A EP2085493A1 EP 2085493 A1 EP2085493 A1 EP 2085493A1 EP 07830687 A EP07830687 A EP 07830687A EP 07830687 A EP07830687 A EP 07830687A EP 2085493 A1 EP2085493 A1 EP 2085493A1
Authority
EP
European Patent Office
Prior art keywords
carburization
temperature
steel material
primary
quenching
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP07830687A
Other languages
German (de)
French (fr)
Other versions
EP2085493A4 (en
Inventor
Toshiyuki Morita
Masaomi Saruyama
Hiroyuki Tsuyuzaki
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Honda Motor Co Ltd
Original Assignee
Honda Motor Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Honda Motor Co Ltd filed Critical Honda Motor Co Ltd
Publication of EP2085493A1 publication Critical patent/EP2085493A1/en
Publication of EP2085493A4 publication Critical patent/EP2085493A4/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/20—Carburising
    • C23C8/22—Carburising of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium

Definitions

  • the present invention relates to a manufacturing method for high-concentration carburized steel and, more particularly, to a manufacturing method for high-concentration carburized steel in which fine and spherical carbides can be precipitated in a large amount in the surface thereof by carburization treatment.
  • Carburization means a treatment of heating steel in a carburizing atmosphere to thereby enhance carbon concentration in the surface.
  • Carburization is generally applied to low-carbon steel, which is quenched after carburization to use.
  • Materials having been subjected to such carburizing-quenching treatment are called case-hardened steel or carburized steel and are commercially used as mechanical members such as shafts, bearings, gear wheels, piston pins, and cams since they have a hard surface and a soft interior.
  • a treatment of enhancing the carbon concentration in the vicinity of the surface of the material to precipitate carbides is specifically called "high-concentration carburization".
  • Materials obtained by the high-concentration carburization contains hard carbides dispersed in their structure, and hence they are characterized in that they have higher abrasion resistance and higher surface fatigue strength than those materials have which are obtained by conventionally performed eutectoid carburization.
  • characteristic properties of the materials having been subjected to the high-concentration carburization treatment are strongly influenced by the dispersion state of carbides, it is necessary to disperse carbides finely in a spherical form in a large amount so as to obtain high strength (see, non-patent document 1). In particular, coarse carbides precipitated at the grain boundaries cause reduction in strength.
  • patent document 1 discloses a method of carburization treatment of steel, which subjecting following steps on a machine structure member made of steel having C:0.05-0.45% :
  • patent document 2 discloses a carburization heat treatment method of a steel member. The method includes:
  • the primary carburization treatment is performed mainly for the purpose of solid-dissolving carbon in a high concentration in the surface so as to precipitate fine carbides in a large amount upon re-heating for performing the secondary carburization treatment.
  • the secondary carburization treatment is performed mainly for the purpose of allowing fine carbides generated upon re-heating to grow. For such purposes, it is desirable that the difference in temperature between the primary carburization treatment and the secondary carburization treatment is large enough.
  • the manufacturing method for high-concentration carburized steel of the invention includes:
  • the difference between the primary carburization temperature T1 and the secondary carburization temperature T2 can be made large enough even when the primary carburization temperature T1 is a comparatively low temperature, by separating the secondary carburization treatment into a secondary carburization initial step of performing carburization at a secondary carburization temperature T2 which is lower than the quenching temperature Tq and a secondary carburization late step of performing carburization at a quenching temperature Tq.
  • fine and spherical carbides can be dispersed in a large amount without shortening the furnace life and generating serious deformation after carburization treatment.
  • a steel material to which the manufacturing method for high-concentration carburized steel of the invention is applied contains alloy elements as described below, and the balance thereof is Fe and unavoidable impurities.
  • Kinds of the alloy elements, ranges of the components, and reasons for restricting the ranges are as follows.
  • the amount of C is preferably 0.15 mass% or more.
  • the amount of C is preferably 0.30 mass% or less.
  • the amount of Si is preferably 0.40 mass% or more.
  • the amount of Si is preferably 0. 80 mass% or less.
  • the amount of Mn is preferably 0.3 mass% or more.
  • the amount of Mn is preferably 0.8 mass% or less.
  • the amount of Cr is small, the amount of generated carbides is reduced, which reduces strength. Also, ferrite is generated in the core portion, which reduces strength. Therefore, the amount of Cr is preferably 1.25 mass% or more. On the other hand, if the amount of Cr is excessive, hardness of the material is enhanced, which reduces productivity (particularly machinability). Therefore, the amount of Cr is 2.00 mass% or less.
  • the manufacturing method for high-concentration carburized steel of the invention includes a primary carburization step, a cooling step, a secondary carburization initial step, a secondary carburization late step, and a quenching step.
  • the primary carburization step is a step of carburizing a steel material having the above-described composition at a primary carburization temperature T1 (°C) so that the surface carbon concentration C becomes Ceu ⁇ C ⁇ C(Acm). It suffices for the primary carburization temperature T1 to be temperature higher than the secondary carburization start temperature T2s to be described hereinafter by 100°C or more. In general, as the primary carburization temperature T1 becomes higher, carburization to a predetermined carbon concentration can be achieved in a shorter time. To be specific, the primary carburization temperature T1 is preferably 900°C or higher.
  • the primary carburization temperature T1 is preferably 1,100°C or lower, more preferably 1,000°C or lower.
  • C of a steel material becomes Ceu ⁇ C ⁇ C (Acm).
  • surface carbon concentration means an average carbon concentration within the region of 10 ⁇ m from the surface.
  • Ceu means an eutectoid carbon concentration of a steel material containing Si, Mn, and Cr in the above-described ranges, respectively. With every above-described steel material, the eutectoid carbon concentration is 0.5 mass% or more.
  • C(Acm) means a carbon concentration corresponding to the Acm line of a steel material containing Si, Mn, and Cr in the above-described ranges, respectively, at the primary carburization temperature T1. To perform carburization till C ⁇ C(Acm) means to perform the primary carburization at temperature at which the surface temperature of the steel material becomes the Acm line or higher (i.e., temperature at which the surface becomes a single phase of ⁇ -phase).
  • the surface carbon concentration C is small, carbides would not be precipitated within the matrix during the temperature-raising procedure in the secondary carburization to be described hereinafter. If carbides are not precipitated within the matrix, coarse carbides would be generated at the grain boundaries during the secondary carburization. Therefore, the primary carburization must be performed so that the surface carbon concentration C can become larger than Ceu. On the other hand, if the carbon concentration C of the surface becomes excessive, carbides would be generated at the grain boundaries during the primary carburization. Since carbides generated in the primary carburization remain as such, generation of coarse carbides must be prevented. Specifically, absence of coarse carbides of 5 ⁇ m or more in long diameter is preferred.
  • the primary carburization must be performed so that the surface carbon concentration C can become C(Acm) or less.
  • C(Acm) becomes from about 1.25 to about 1.4 mass% when the primary carburization temperature T1 is from 950 to 1,000°C.
  • the carburization method upon performing the primary carburization is not particularly limited, and various methods may be employed.
  • gas carburization and vacuum carburization are preferred as the carburization methods since handling is easy and treating period is short.
  • the surface carbon concentration C can be controlled within the above-described range by optimizing the carburizing conditions.
  • gas carburization carburization is performed by heating a steel material in an atmosphere of a carburizing gas.
  • the amount of carburization can be controlled through carbon potential of the carburizing atmosphere. Carbon potential is the surface equilibrium carbon concentration of pure iron equilibrated with the atmosphere and is dependent upon the CO/CO 2 ratio and the amount of H 2 O in the atmosphere.
  • the surface carbon concentration can be increased in a shorter time when the carbon potential becomes higher and/or when the primary carburization temperature T1 becomes higher.
  • carburization can be performed by, for example, reducing the pressure inside the furnace into which a steel material has been introduced to about 1.3 Pa, and then heating to the carburization temperature with introducing thereinto a hydrocarbon gas such as methane or propane.
  • a hydrocarbon gas such as methane or propane.
  • the amount of carburization can be controlled through the time of introducing the hydrocarbon gas.
  • the carbon concentration in the vicinity of the surface may become too high. In such case, it is general to perform diffusion treatment of stopping supply of the hydrocarbon gas after carburization and retaining in the same state.
  • the cooling step is a step of cooling, after completion of the primary carburization step, the steel material at a cooling rate of 1°C/min or more to 700°C or lower. After completion of the primary carburization, the steel material is once cooled to temperature of 700°C or lower.
  • the reason for cooling to temperature of 700°C or lower is that, upon re-heating in the secondary carburization, fine carbides be precipitated within grains. In this case, when the cooling rate is too slow, flake-like, coarse carbides are formed at the grain boundaries during cooling, thus too slow cooling rate is not preferred. The coarse carbides generated during cooling will not disappear in the step to be described hereinafter, and can cause reduction of strength of the steel material. Therefore, the cooling rate of 1°C/min or more is preferred. A faster cooling rate is more preferred.
  • the secondary carburization initial step is a step wherein the temperature of the cooled steel material is raised to the secondary carburization start temperature T2s and the steel material is carburized at the secondary carburization temperature T2.
  • the term "secondary carburization start temperature T2s" means the temperature which satisfies the condition of the following formula (1). Ac ⁇ 1 point °C ⁇ T ⁇ 2 ⁇ s °C ⁇ primary carburization temperature T ⁇ 1 - 100 ⁇ °C ⁇ Acm line temperature °C ⁇ corresponding to the surface carbon concentration of the steel material immediately after initiation of secondary carburization
  • the temperature difference between the secondary carburization start temperature T2s and the primary carburization temperature T1 is preferably 100°C or more.
  • the secondary carburization start temperature T2s must be equal to, or higher than, Ac1 point and must be equal to, or lower than, the Acm line temperature corresponding to the surface carbon concentration of a steel material immediately after initiation of the secondary carburization. This means to initiate the secondary carburization when the surface temperature of the steel material is between Ac1 point and Acm line (i.e., the temperature at which the surface becomes ⁇ +Fe 3 C phase).
  • secondary carburization temperature T2 means the temperature which satisfies the conditions of the following formula (2). T ⁇ 2 ⁇ s ⁇ T ⁇ 2 ⁇ Acm line temperature C corresponding to the surface carbon concentration of the aforesaid steel material
  • the secondary carburization temperature T2 may be the same as the secondary carburization start temperature T2s or may be temperature higher than that. If the secondary carburization temperature T2 is the same as the secondary carburization start temperature T2s, the retaining time at the secondary carburization temperature T2 may be such that, when the temperature is raised to the quenching temperature Tq to be described hereinafter, the surface temperature of the steel material does not exceed the Acm line temperature.
  • the surface carbon concentration increases as the time of retaining at the secondary carburization temperature T2 is prolonged, and hence carburization can be performed with keeping the surface temperature of the steel material at Acm line or less.
  • the retaining time at the secondary carburization temperature T2 is preferably 15 minutes or longer.
  • the secondary carburization temperature T2 may be reached by raising the temperature stepwisely or continuously from the secondary carburization start temperature T2s.
  • stepwisely means to repeat the procedures of retaining the temperature at a definite level for a predetermined time, then raising the temperature with a predetermined temperature width, and retaining the temperature at the predetermined temperature for a predetermined time.
  • stepwisely raising the temperature carburization can be performed with retaining the surface temperature of the steel material at Acm line or less by optimizing the temperature-raising width and the temperature-retaining time.
  • the term “continuously” means to raise the temperature at a predetermined temperature-raising rate. When continuously raising the temperature, carburization can be performed with retaining the surface temperature of the steel material at Acm line or less by optimizing the temperature-raising rate.
  • the secondary carburization late step is a step of subsequently raising, after completion of the secondary carburization initial step, the temperature of the steel material up to the quenching temperature Tq (°C), and further performing carburization at the quenching temperature Tq, provided that Tq ⁇ Acm line temperature (°C) corresponding to the surface carbon concentration of the aforesaid steel material.
  • the secondary carburization late step is a step of not only raising the temperature of the steel material to the quenching temperature Tq but also adjusting the surface carbon concentration to an intended carbon concentration in a short time without precipitation of flake-like, coarse carbides at the grain boundaries. Therefore, the quenching temperature Tq must be equal to, or less than, the Acm line temperature corresponding to the surface carbon concentration of the steel material.
  • the temperature can be raised up to the quenching temperature Tq with retaining the surface temperature of the steel material at Acm line temperature or less.
  • the quenching temperature Tq is preferably equal to, or higher than, the temperature at which the core portion of the steel material becomes an austenite single phase.
  • the time of retaining the temperature at the quenching temperature Tq is not particularly limited, and an optimal time is to be selected depending upon composition of the steel material, quenching temperature Tq, characteristic properties required for the steel material, and the like. In general, as the temperature-retaining time is prolonged, the surface carbon concentration of the steel material can be more increased. In order to obtain high-concentration carburized steel excellent in abrasion resistance and surface fatigue strength, the temperature-retaining time at the quenching temperature Tq (i.e., carburization time) is preferably 15 minutes or longer.
  • quenching may immediately be performed substantially without performing carburization at the quenching temperature Tq after the temperature reaches the quenching temperature Tq as long as a sufficient carburization amount is obtained at the point when the temperature reaches the quenching temperature Tq and when soaking of the steel material is sufficient.
  • the quenching step is a step of quenching the steel material after completion of the secondary carburization late step. Quenching is to be performed for transforming the surface carburized layer and the core portion to martensite. For this, the steel material after completion of the secondary carburization late step is to be preferably quenched.
  • the quenching method there are specifically an oil quenching method and a gas quenching method.
  • Figs. 1A to Fig. 1D are schematic views showing structural changes when performing high-concentration carburization under various conditions. Additionally, phase diagrams are also shown in Figs. 1A to Fig. 1D .
  • the high-concentration carburization it is performed twice in many case, that is, the primary carburization and the secondary carburization.
  • the surface carbon concentration upon completion of the primary carburization is lower than the Acm line concentration corresponding to the carburization temperature as shown in the phase diagram of Fig. 1A .
  • the surface after the completion of the primary carburization is in a state of austenite single phase. Therefore, when the steel material is cooled to 700°C or lower from this state at a predetermined cooling rate, the structure of the steel material becomes the state wherein coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1A .
  • the temperature of the steel material is raised to the secondary carburization temperature, spherical and fine carbides are generated in the course of raising the temperature in the secondary carburization as shown in the middle drawing of Fig. 1A .
  • the secondary carburization is performed at temperature lower than the Acm line temperature corresponding to the surface carbon concentration of the steel material (i.e., the temperature at which the surface becomes ⁇ +Fe 3 phase), and carbon diffusion rate becomes smaller than in the primary carburization, thus carbides being difficultly precipitated in the grain boundaries.
  • the fine carbides generated during temperature-raising procedure act as nuclei to allow growth of carbides as shown in the right drawing of Fig. 1A .
  • the temperature upon completion of the primary carburization must be higher than the Acm line, and the temperature upon initiation of the secondary carburization must be lower than the Acm line. Since produced steel materials are not uniform in composition between lots, the position of the Acm line varies to some extent between individual steel materials. Hence, in order to surely obtain the structure as shown in Fig. 1A , it is necessary to provide a sufficient temperature difference between the primary carburization temperature and the secondary carburization temperature. However, when the primary carburization temperature is raised for the purpose of providing the sufficient temperature difference, durability of the furnace is decreased. On the other hand, when the secondary carburization temperature is decreased in order to avoid this, the carbon diffusion rate in the secondary carburization is reduced, leading to serious decrease in productivity.
  • the two-step carburization treatment with the Acm line being put between the two steps.
  • the primary carburization temperature is above the Acm line while retaining the secondary carburization temperature at the same temperature as in the conventional art and lowering the primary carburization temperature
  • the structure of the steel material after completion of the primary carburization is in the state that coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1B .
  • the structure of the steel material after completion of the primary carburization is in the state that coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1D .
  • the secondary carburization start temperature is lower than the primary carburization temperature by 100°C or more while raising, after cooling the steel material, the temperature to the secondary carburization start temperature, the surface temperature of the steel material can surely be adjusted to temperature lower than the Acm line. Therefore, at the point where the temperature reaches the secondary carburization start temperature, fine carbides are generated within the grains as shown in the middle drawing of Fig. 1D .
  • the primary carburization In order to prevent precipitation of flake-like, coarse carbides at the grain boundaries, the primary carburization must be performed at temperature higher than the Acm line and the secondary carburization must be performed at temperature lower than the Acm line.
  • the manufacturing method for high-concentration carburized steel of the invention can provide a sufficient temperature difference between after completion of the primary carburization and upon initiation of the secondary carburization, and hence generation of flake-like, coarse carbides can surely be suppressed even when steel materials are not uniform in composition between lots. Also, since it is not necessary to raise the temperature of the primary carburization for providing a sufficient temperature difference, durability of the furnace is not reduced. Further, since carburization is continued, after a predetermined time after the temperature reaches the secondary carburization start temperature, by raising the temperature to the quenching temperature, the carbon concentration of the surface can reach the intended concentration in a short time.
  • Carburization is performed with steel materials having various compositions under various conditions. Additionally, every carburization is performed in two steps of the primary carburization and the second carburization. Also, except for Example 15 and Comparative Example 1, the secondary carburization is performed in two steps of the secondary initial step of retaining the temperature for a predetermined time at a definite level (low temperature) and the secondary carburization late step of raising the temperature to the quenching temperature (high temperature) and retaining at the temperature for a predetermined time.
  • a typical carburization treatment pattern is shown in Fig. 2 .
  • the surface carbon concentration after completion of the primary carburization is determined by measuring distribution of cross-sectional carbon concentration through EPMA and calculating an average carbon concentration in the region of 10 ⁇ m from the surface. Also, diameter of carbide after completion of the primary carburization and diameter after quenching are measured by photographing using SEM after corroding the cross-section of the sample with picral, with the maximum value of the particle size of carbides existing in 1 mm 2 being taken as "particle size of carbides”. Further, fatigue strength after quenching is measured by the rotating bending fatigue test (according to JIS Z 2274).
  • Compositions of individual steel materials, carburization conditions, and test results are shown in Table 1.
  • Comparative Example 1 coarse carbides of larger than 10 ⁇ m are generated after quenching. This may be attributed to that, since the secondary carburization initial step is omitted and the secondary carburization late step at 885°C is immediately performed, fine carbides generated in the course of the secondary carburization again undergoes solid dissolution.
  • Comparative Example 2 coarse carbides of larger than 10 ⁇ m are generated after quenching. The reason for this is that the primary carburization is excessive and, at the point of completion of the primary carburization, coarse carbides are already generated.
  • Comparative Example 3 coarse carbides of larger than 6 ⁇ m are generated.
  • the fatigue strength is 700 MPa or more. This may be attributed to that, since the primary carburization, secondary carburization initial procedure, and secondary carburization late procedure are performed under proper conditions, fine and spherical carbides are formed in a large amount within the grains without generating flake-like, coarse carbides at the grain boundaries.
  • the manufacturing method for high-concentration carburized steel of the invention can be used as a manufacturing method for mechanical members such as shafts, bearings, gear wheels, piston pins, and cams.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical 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)

Abstract

The subject of the present invention is to provide a manufacturing method for high-concentration carburized steel which does not cause reduction of life of a furnace, deformation of steel materials, and reduction of working efficiency and which enables dispersion of fine and spherical carbides in a large amount. This subject can be solved by the manufacturing method for high-concentration carburized steel comprises (i) a primary carburization step of carburizing a steel material having a certain composition at a primary carburization temperature T1(°C) till a surface carbon concentration C becomes a certain carbon concentration, (ii) a cooling step of cooling the steel material to Ar1 point or less at a cooling rate of 1°C/min or more after completion of the primary carburization step, (iii) a secondary carburization initial step of raising the temperature of the steel material to a secondary carburization start temperature T2s lower than the primary carburization temperature T1 by 100°C or more to carburize the steel material at a secondary carburization temperature T2, (iv) a secondary carburization later step of raising the temperature, after completion of the secondary carburization initial step, to a quenching temperature Tq to further carburize at the quenching temperature of Tq and perform further carburization of the steel material at the quenching temperature Tq, and (v) a quenching step of quenching the steel material after completion of the secondary carburization.
Figure imgaf001

Description

    Technical Field
  • The present invention relates to a manufacturing method for high-concentration carburized steel and, more particularly, to a manufacturing method for high-concentration carburized steel in which fine and spherical carbides can be precipitated in a large amount in the surface thereof by carburization treatment.
    • Background Art
  • Carburization means a treatment of heating steel in a carburizing atmosphere to thereby enhance carbon concentration in the surface. Carburization is generally applied to low-carbon steel, which is quenched after carburization to use. Materials having been subjected to such carburizing-quenching treatment are called case-hardened steel or carburized steel and are commercially used as mechanical members such as shafts, bearings, gear wheels, piston pins, and cams since they have a hard surface and a soft interior.
    Among carburization treatments, a treatment of enhancing the carbon concentration in the vicinity of the surface of the material to precipitate carbides is specifically called "high-concentration carburization". Materials obtained by the high-concentration carburization contains hard carbides dispersed in their structure, and hence they are characterized in that they have higher abrasion resistance and higher surface fatigue strength than those materials have which are obtained by conventionally performed eutectoid carburization.
    However, since characteristic properties of the materials having been subjected to the high-concentration carburization treatment are strongly influenced by the dispersion state of carbides, it is necessary to disperse carbides finely in a spherical form in a large amount so as to obtain high strength (see, non-patent document 1). In particular, coarse carbides precipitated at the grain boundaries cause reduction in strength.
  • Thus, in order to solve this problem, various proposals have conventionally been made.
    For example, patent document 1 discloses a method of carburization treatment of steel, which subjecting following steps on a machine structure member made of steel having C:0.05-0.45% :
    1. (i) subjecting primary carburization by plasma carburization at temperature of 880°C or higher to enhance the C concentration of the member surface to Acm of the steel or more than that to thereby precipitate carbides in the vicinity of the surface;
    2. (ii) gradually cooling the machine structure member to temperature lower than Ar1 of the steel and, after retaining the temperature at the level, heating it to temperature exceeding Ar1;
    3. (iii) subjecting secondary carburization by plasma carburization again at temperature lower than the temperature of the primary carburization by 10 to 60°C; and
    4. (iv) quenching and tempering immediately or after subjecting a diffusing treatment to thereby obtain a member in which the surface C concentration is 1.5% or more, the shape of the carbides in the carburized layer is approximately spherical, and has excellent abrasion resistance and excellent pitching resistance.
      Also, the same literature discloses following steps which are subjected subsequent to the above-described step (iii):
    5. (v) gradually cooling it again to temperature lower than Ar1 of the steel and, retaining the temperature at the level at once, heating it to temperature exceeding Ar1;
    6. (vi) subjecting third carburization by plasma carburization again at temperature still lower than the temperature of the secondary carburization by 10 to 60°C; and then the step (iv)
      to thereby obtain a member in which the surface C concentration is 1.7% or more, in which the shape of the carbides in the carburized layer is approximately spherical, and which has excellent abrasion resistance and excellent pitching resistance.
  • In the same literature describes followings:
    1. (1) no anxiety about carburization unevenness exists since generation of soot is slight in spite of a high carbon potential when plasma carburization is employed as the carburization treatment method;
    2. (2) carbides can be precipitated in a agglomerate shape at the austenite grain boundaries since carburization in the primary carburization is performed in a high density of C concentration exceeding Acm;
    3. (3) the austenite grain boundary migrates when the temperature is once decreased, after carburization, to temperature lower than Ar1 and is again raised to temperature higher than Ar1 and, as a result, carbides first having existed at the grain boundaries remain within new austenite grains; and
    4. (4) carbides precipitate at the new austenite grain boundaries by further performing the secondary carburization, and a carburized layer having a preferred carbide distribution can be obtained by the newly generated carbides and the above-described residual carbides.
  • Further, patent document 2 discloses a carburization heat treatment method of a steel member. The method includes:
    • cooling a steel member having been subjected to carburization treatment to a degree of 0.8% or more in the surface carbon concentration to temperature of 300°C or lower than that after this carburization treatment at a cooling rate of 0.1°C/sec or more,
    • heating the steel member to temperature range higher than the Ac1 transformation temperature of the steel by 50°C and lower than that by 150°C,
    • retaining the steel member at the same temperature and,
    • further raising the temperature at a heating rate of 10°C/sec to temperature at which the core portion thereof acquires an austenite single phase or an austenite/ferrite dual phase wherein the ferrite area ratio is 30% or less and retaining at the temperature,
    • performing quenching directly or after decreasing the temperature to a predetermined level for quenching.
    • The literature describes that fine carbides can be allowed to grow by retaining the carburized steel member in the temperature range of higher than the Ac1 transformation temperature of the steel by 50°C and lower than that by 150°C.
    • Non-patent document 1: Tetsuya Shimomura, Toshiyuki Morita, and Koichiro Inoue; DENKI-SEIKO (Electric Furnace Steel), vol.77 (2006), p.11
    • Patent document 1: Japanese Patent Examined Publication JP-B-2808621
    • Patent document 2: Japanese Patent unexamined publication JP-A-6-108226
    Disclosure of the Invention Problems that the Invention is to Solve
  • As disclosed in the patent document 2, it is difficult to disperse fine and spherical carbides in a large amount only by one carburization treatment. Therefore, in many of the conventionally performed high-concentration carburization, two carburization treatments of a primary carburization treatment and a secondary carburization treatment are performed. The primary carburization treatment is performed mainly for the purpose of solid-dissolving carbon in a high concentration in the surface so as to precipitate fine carbides in a large amount upon re-heating for performing the secondary carburization treatment. On the other hand, the secondary carburization treatment is performed mainly for the purpose of allowing fine carbides generated upon re-heating to grow. For such purposes, it is desirable that the difference in temperature between the primary carburization treatment and the secondary carburization treatment is large enough.
  • However, if the temperature in the primary carburization treatment is raised in order to enlarge the difference in temperature between the primary carburization treatment and the secondary carburization treatment, the life of the furnace would be shortened. Also, the case-hardened steel is usually used as such without finishing processing, thus, heating it at a higher temperature than is necessary would increase deformation of the material.
    On the other hand, if the temperature of the secondary carburization treatment is decreased simultaneously with decreasing the temperature of the primary carburization treatment in order to solve this problem, the diffusion rate of carbon upon the second carburization treatment would be lowered. Thus, it takes a long time to precipitate a necessary amount of carbides, which reduces working efficiency.
    Further, if only the temperature of the primary carburization treatment is decreased with the temperature of the secondary carburization treatment being kept at a high level, the difference in temperature between the primary carburization treatment and the secondary carburization treatment would become smaller. Thus, flake-like, coarse carbides would be tended to be precipitated at grain boundaries, which reduces reproducibility of the structure.
  • A problem that the invention is to solve is to provide a manufacturing method for high-concentration carburized steel, which enables dispersion of fine and spherical carbides in a large amount without shortening the furnace life.
    Another problem that the invention is to solve is to provide a manufacturing method for high-concentration carburized steel, which does not cause large deformation after carburization treatment.
    A further problem that the invention is to solve is to provide a manufacturing method for high-concentration carburized steel, which enables dispersion of fine and spherical carbides in a large amount without reducing working efficiency.
    A still further problem that the invention is to solve is to provide a manufacturing method for high-concentration carburized steel, in which flake-like, coarse carbides are not precipitated at the grain boundaries, and which provides a high reproducibility of the structure.
    • Means for Solving the Problems
  • In order to solve the above-described problems, the manufacturing method for high-concentration carburized steel of the invention includes:
    1. (i) a primary carburization step of carburizing a steel material having C of 0.15-0.30 mass%, Si of 0.40-0.80 mass%, Mn of 0.3-0.8 mass%, Cr of 1.25-2.00 mass%, and balance of Fe and unavoidable impurities at a primary carburization temperature T1(°c) till the surface carbon concentration C becomes Ceu<C≤C(Acm), wherein Ceu is an eutectoid carbon concentration of the steel material, and C(Acm) is a carbon concentration corresponding to the Acm line of the aforesaid steel material at the primary carburization temperature T1;
    2. (ii) a cooling step of cooling the steel material to 700°C or lower at a cooling rate of 1°C/min or more after completion of the primary carburization step;
    3. (iii) a secondary carburization initial step of raising the temperature of the steel material to a secondary carburization start temperature T2s to carburize the steel material at a secondary carburization temperature T2, wherein Ac1 point (°C) ≤ T2s (°C) ≤ primary carburization temperature T1 - 100°C ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material immediately after initiation of the secondary carburization, and T2s ≤ T2 ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material;
    4. (iv) a secondary carburization late step of raising the temperature, after completion of the secondary carburization initial step, to a quenching temperature Tq (°C) to further carburize at the quenching temperature of Tq, wherein Tq ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material; and
    5. (v) a step of quenching the steel material after completion of the secondary carburization.
    Advantage of the Invention
  • When performing the primary carburization treatment at the primary carburization temperature T1 and further performing the secondary carburization treatment, the difference between the primary carburization temperature T1 and the secondary carburization temperature T2 can be made large enough even when the primary carburization temperature T1 is a comparatively low temperature, by separating the secondary carburization treatment into a secondary carburization initial step of performing carburization at a secondary carburization temperature T2 which is lower than the quenching temperature Tq and a secondary carburization late step of performing carburization at a quenching temperature Tq. Thus, fine and spherical carbides can be dispersed in a large amount without shortening the furnace life and generating serious deformation after carburization treatment. Also, in the secondary carburization late step, carburization is performed at a comparatively high temperature, and hence working efficiency is not reduced. Further, since the difference between the primary carburization temperature T1 and the secondary carburization temperature T2 can be made large enough, precipitation of flake-like, coarse carbides at the grain boundaries can surely be suppressed even when composition is not uniform between steel materials.
    • Brief Description of the Drawings
    • Figs. 1A to 1D are schematic views showing change in structure in the case of performing high-concentration carburization under various conditions, and phase diagrams; and
    • Fig. 2 is a view showing the typical carburization treatment pattern employed in Example.
    Best Mode for Carrying Out the Invention
  • An embodiment of the invention will be described in detail hereinafter.
    First, steel material to which the manufacturing method for high-concentration carburized steel of the invention is applied is described.
    A steel material to which the manufacturing method of the invention is applied contains alloy elements as described below, and the balance thereof is Fe and unavoidable impurities. Kinds of the alloy elements, ranges of the components, and reasons for restricting the ranges are as follows.
    • (1) C: 0.15-0.30 mass%
  • If the amount of C is small, ferrite is generated in the core portion, which reduces strength. Therefore, the amount of C is preferably 0.15 mass% or more.
    On the other hand, if the amount of C is large, hardness of the material is enhanced, which reduces productivity (particularly machinability). Therefore, the amount of C is preferably 0.30 mass% or less.
    • (2) Si: 0.40 to 0.80 mass%
  • If the amount of Si is small, tempered hardness of the matrix is reduced, which reduces strength. Therefore, the amount of Si is preferably 0.40 mass% or more.
    On the other hand, if the amount of Si is excessive, the amount of generated carbides is reduced, which reduces strength. Also, ferrite is generated in the core portion, which reduces strength. Therefore, the amount of Si is preferably 0. 80 mass% or less.
    • (3) Mn: 0.3 to 0.8 mass%
  • If the amount of Mn is small, quenching properties of the matrix are deteriorated, and strength is reduced due to incomplete quenching. Therefore, the amount of Mn is preferably 0.3 mass% or more.
    On the other hand, if the amount of Mn is excessive, hardness of the material is enhanced, which reduces productivity (particularly machinability). Therefore, the amount of Mn is preferably 0.8 mass% or less.
    • (4) Cr: 1.25 to 2.00 mass%
  • If the amount of Cr is small, the amount of generated carbides is reduced, which reduces strength. Also, ferrite is generated in the core portion, which reduces strength. Therefore, the amount of Cr is preferably 1.25 mass% or more.
    On the other hand, if the amount of Cr is excessive, hardness of the material is enhanced, which reduces productivity (particularly machinability). Therefore, the amount of Cr is 2.00 mass% or less.
  • Next, the manufacturing method for high-concentration carburized steel of the invention will be described.
    The manufacturing method for high-concentration carburized steel of the invention includes a primary carburization step, a cooling step, a secondary carburization initial step, a secondary carburization late step, and a quenching step.
  • The primary carburization step is a step of carburizing a steel material having the above-described composition at a primary carburization temperature T1 (°C) so that the surface carbon concentration C becomes Ceu<C≤C(Acm).
    It suffices for the primary carburization temperature T1 to be temperature higher than the secondary carburization start temperature T2s to be described hereinafter by 100°C or more. In general, as the primary carburization temperature T1 becomes higher, carburization to a predetermined carbon concentration can be achieved in a shorter time. To be specific, the primary carburization temperature T1 is preferably 900°C or higher.
    On the other hand, if the primary carburization temperature T1 is too high, the furnace life would be shortened, or deformation of the steel material would occur in some cases. Therefore, to be specific, the primary carburization temperature T1 is preferably 1,100°C or lower, more preferably 1,000°C or lower.
  • Also, carburization is performed so that the surface carbon concentration C of a steel material becomes Ceu<C≤C (Acm). Here, the term "surface carbon concentration" means an average carbon concentration within the region of 10 µm from the surface. Also, "Ceu" means an eutectoid carbon concentration of a steel material containing Si, Mn, and Cr in the above-described ranges, respectively. With every above-described steel material, the eutectoid carbon concentration is 0.5 mass% or more.
    Further, "C(Acm)" means a carbon concentration corresponding to the Acm line of a steel material containing Si, Mn, and Cr in the above-described ranges, respectively, at the primary carburization temperature T1. To perform carburization till C≤C(Acm) means to perform the primary carburization at temperature at which the surface temperature of the steel material becomes the Acm line or higher (i.e., temperature at which the surface becomes a single phase of γ-phase).
  • If the surface carbon concentration C is small, carbides would not be precipitated within the matrix during the temperature-raising procedure in the secondary carburization to be described hereinafter. If carbides are not precipitated within the matrix, coarse carbides would be generated at the grain boundaries during the secondary carburization. Therefore, the primary carburization must be performed so that the surface carbon concentration C can become larger than Ceu.
    On the other hand, if the carbon concentration C of the surface becomes excessive, carbides would be generated at the grain boundaries during the primary carburization. Since carbides generated in the primary carburization remain as such, generation of coarse carbides must be prevented. Specifically, absence of coarse carbides of 5 µm or more in long diameter is preferred. Therefore, the primary carburization must be performed so that the surface carbon concentration C can become C(Acm) or less.
    For example, with the steel material having the above-described composition, C(Acm) becomes from about 1.25 to about 1.4 mass% when the primary carburization temperature T1 is from 950 to 1,000°C.
  • The carburization method upon performing the primary carburization is not particularly limited, and various methods may be employed. In particular, gas carburization and vacuum carburization are preferred as the carburization methods since handling is easy and treating period is short. When employing a particular carburization method, the surface carbon concentration C can be controlled within the above-described range by optimizing the carburizing conditions.
    For example, with gas carburization, carburization is performed by heating a steel material in an atmosphere of a carburizing gas. In this case, the amount of carburization can be controlled through carbon potential of the carburizing atmosphere. Carbon potential is the surface equilibrium carbon concentration of pure iron equilibrated with the atmosphere and is dependent upon the CO/CO2 ratio and the amount of H2O in the atmosphere. In general, the surface carbon concentration can be increased in a shorter time when the carbon potential becomes higher and/or when the primary carburization temperature T1 becomes higher.
    Also, with vacuum carburization, carburization can be performed by, for example, reducing the pressure inside the furnace into which a steel material has been introduced to about 1.3 Pa, and then heating to the carburization temperature with introducing thereinto a hydrocarbon gas such as methane or propane. In this case, the amount of carburization can be controlled through the time of introducing the hydrocarbon gas. Additionally, when vacuum carburization is performed, the carbon concentration in the vicinity of the surface may become too high. In such case, it is general to perform diffusion treatment of stopping supply of the hydrocarbon gas after carburization and retaining in the same state.
  • The cooling step is a step of cooling, after completion of the primary carburization step, the steel material at a cooling rate of 1°C/min or more to 700°C or lower.
    After completion of the primary carburization, the steel material is once cooled to temperature of 700°C or lower. The reason for cooling to temperature of 700°C or lower is that, upon re-heating in the secondary carburization, fine carbides be precipitated within grains. In this case, when the cooling rate is too slow, flake-like, coarse carbides are formed at the grain boundaries during cooling, thus too slow cooling rate is not preferred. The coarse carbides generated during cooling will not disappear in the step to be described hereinafter, and can cause reduction of strength of the steel material. Therefore, the cooling rate of 1°C/min or more is preferred. A faster cooling rate is more preferred.
  • The secondary carburization initial step is a step wherein the temperature of the cooled steel material is raised to the secondary carburization start temperature T2s and the steel material is carburized at the secondary carburization temperature T2.
    The term "secondary carburization start temperature T2s" means the temperature which satisfies the condition of the following formula (1). Ac ⁢ 1 point °C ≤ T ⁢ 2 ⁢ s °C ≤ primary carburization temperature T ⁢ 1 - 100 ⁢ °C ≤ Acm line temperature °C ⁢ corresponding to the surface carbon concentration of the steel material immediately after initiation of secondary carburization
    Figure imgb0001
    The temperature difference between the secondary carburization start temperature T2s and the primary carburization temperature T1 is preferably 100°C or more. If the temperature difference therebetween is less than 100°C, there is the possibility of generation of flake-like, coarse carbides at the grain boundaries. A larger temperature difference therebetween is more preferred.
    Also, the secondary carburization start temperature T2s must be equal to, or higher than, Ac1 point and must be equal to, or lower than, the Acm line temperature corresponding to the surface carbon concentration of a steel material immediately after initiation of the secondary carburization. This means to initiate the secondary carburization when the surface temperature of the steel material is between Ac1 point and Acm line (i.e., the temperature at which the surface becomes γ+Fe3C phase).
  • The term "secondary carburization temperature T2" means the temperature which satisfies the conditions of the following formula (2). T ⁢ 2 ⁢ s ≤ T ⁢ 2 ≤ Acm line temperature C corresponding to the surface carbon concentration of the aforesaid steel material
    Figure imgb0002
    The secondary carburization temperature T2 may be the same as the secondary carburization start temperature T2s or may be temperature higher than that.
    If the secondary carburization temperature T2 is the same as the secondary carburization start temperature T2s, the retaining time at the secondary carburization temperature T2 may be such that, when the temperature is raised to the quenching temperature Tq to be described hereinafter, the surface temperature of the steel material does not exceed the Acm line temperature. In general, the surface carbon concentration increases as the time of retaining at the secondary carburization temperature T2 is prolonged, and hence carburization can be performed with keeping the surface temperature of the steel material at Acm line or less. In order for the surface temperature of the steel material to become Acm line or less when the temperature is raised to the quenching temperature Tq, the retaining time at the secondary carburization temperature T2 is preferably 15 minutes or longer.
  • On the other hand, in the case when the secondary carburization temperature T2 is higher than the secondary carburization start temperature T2s, the secondary carburization temperature T2 may be reached by raising the temperature stepwisely or continuously from the secondary carburization start temperature T2s.
    The term "stepwisely" means to repeat the procedures of retaining the temperature at a definite level for a predetermined time, then raising the temperature with a predetermined temperature width, and retaining the temperature at the predetermined temperature for a predetermined time. When stepwisely raising the temperature, carburization can be performed with retaining the surface temperature of the steel material at Acm line or less by optimizing the temperature-raising width and the temperature-retaining time.
    Also, the term "continuously" means to raise the temperature at a predetermined temperature-raising rate. When continuously raising the temperature, carburization can be performed with retaining the surface temperature of the steel material at Acm line or less by optimizing the temperature-raising rate.
  • The secondary carburization late step is a step of subsequently raising, after completion of the secondary carburization initial step, the temperature of the steel material up to the quenching temperature Tq (°C), and further performing carburization at the quenching temperature Tq, provided that Tq ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the aforesaid steel material.
    The secondary carburization late step is a step of not only raising the temperature of the steel material to the quenching temperature Tq but also adjusting the surface carbon concentration to an intended carbon concentration in a short time without precipitation of flake-like, coarse carbides at the grain boundaries. Therefore, the quenching temperature Tq must be equal to, or less than, the Acm line temperature corresponding to the surface carbon concentration of the steel material. When carburization conditions of the secondary carburization initial step are optimized, the temperature can be raised up to the quenching temperature Tq with retaining the surface temperature of the steel material at Acm line temperature or less.
    In general, as the quenching temperature Tq is lowered, flake-like, coarse carbides are less difficultly generated at the grain boundaries during retaining. However, if the quenching temperature Tq is too low, there result not only reduction of diffusion rate of carbon but also insufficient quenching of the core portion. Therefore, the quenching temperature Tq is preferably equal to, or higher than, the temperature at which the core portion of the steel material becomes an austenite single phase.
  • The time of retaining the temperature at the quenching temperature Tq is not particularly limited, and an optimal time is to be selected depending upon composition of the steel material, quenching temperature Tq, characteristic properties required for the steel material, and the like. In general, as the temperature-retaining time is prolonged, the surface carbon concentration of the steel material can be more increased. In order to obtain high-concentration carburized steel excellent in abrasion resistance and surface fatigue strength, the temperature-retaining time at the quenching temperature Tq (i.e., carburization time) is preferably 15 minutes or longer.
    Additionally, when stepwisely or continuously raising the secondary carburization temperature T2 in the secondary carburization initial step, quenching may immediately be performed substantially without performing carburization at the quenching temperature Tq after the temperature reaches the quenching temperature Tq as long as a sufficient carburization amount is obtained at the point when the temperature reaches the quenching temperature Tq and when soaking of the steel material is sufficient.
  • The quenching step is a step of quenching the steel material after completion of the secondary carburization late step.
    Quenching is to be performed for transforming the surface carburized layer and the core portion to martensite. For this, the steel material after completion of the secondary carburization late step is to be preferably quenched. As the quenching method, there are specifically an oil quenching method and a gas quenching method.
  • Next, effects of the manufacturing method for high-concentration carburized steel of the invention are described below.
    Figs. 1A to Fig. 1D are schematic views showing structural changes when performing high-concentration carburization under various conditions. Additionally, phase diagrams are also shown in Figs. 1A to Fig. 1D.
    In the high-concentration carburization, it is performed twice in many case, that is, the primary carburization and the secondary carburization. In conventional high-concentration carburization of performing carburization in two steps, the surface carbon concentration upon completion of the primary carburization is lower than the Acm line concentration corresponding to the carburization temperature as shown in the phase diagram of Fig. 1A. That is, the surface after the completion of the primary carburization is in a state of austenite single phase. Therefore, when the steel material is cooled to 700°C or lower from this state at a predetermined cooling rate, the structure of the steel material becomes the state wherein coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1A.
    When the temperature of the steel material is raised to the secondary carburization temperature, spherical and fine carbides are generated in the course of raising the temperature in the secondary carburization as shown in the middle drawing of Fig. 1A. This is because the secondary carburization is performed at temperature lower than the Acm line temperature corresponding to the surface carbon concentration of the steel material (i.e., the temperature at which the surface becomes γ+Fe3 phase), and carbon diffusion rate becomes smaller than in the primary carburization, thus carbides being difficultly precipitated in the grain boundaries.
    When the secondary carburization is initiated after the temperature reaches the secondary carburization temperature, the fine carbides generated during temperature-raising procedure act as nuclei to allow growth of carbides as shown in the right drawing of Fig. 1A.
  • In order to obtain the structure as shown in Fig. 1A, the temperature upon completion of the primary carburization must be higher than the Acm line, and the temperature upon initiation of the secondary carburization must be lower than the Acm line. Since produced steel materials are not uniform in composition between lots, the position of the Acm line varies to some extent between individual steel materials. Hence, in order to surely obtain the structure as shown in Fig. 1A, it is necessary to provide a sufficient temperature difference between the primary carburization temperature and the secondary carburization temperature.
    However, when the primary carburization temperature is raised for the purpose of providing the sufficient temperature difference, durability of the furnace is decreased. On the other hand, when the secondary carburization temperature is decreased in order to avoid this, the carbon diffusion rate in the secondary carburization is reduced, leading to serious decrease in productivity.
  • Further, when the temperature difference between the primary carburization temperature and the secondary carburization temperature is reduced for the purpose of obtaining both durability of the furnace and productivity, it becomes difficult to perform, with good reproducibility, the two-step carburization treatment with the Acm line being put between the two steps.
    For example, when the primary carburization temperature is above the Acm line while retaining the secondary carburization temperature at the same temperature as in the conventional art and lowering the primary carburization temperature, the structure of the steel material after completion of the primary carburization is in the state that coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1B. However, when the secondary carburization temperature exceeds the Acm line, fine carbides having been generated within the grains in the course of raising temperature in the secondary carburization again undergoes solid dissolution as shown in the middle drawing of Fig 1B. Thus, nuclei for allowing carbides to grow disappear within the grains, and hence carbides are preferentially generated at the grain boundaries having smaller formation energy. As a result, coarse carbides are generated at the grain boundaries as shown in the right drawing of Fig. 1B.
    On the other hand, when the primary carburization temperature is below the Acm line while retaining the secondary carburization temperature at the same temperature as in the conventional art and lowering the primary carburization temperature, the structure of the steel material after completion of the primary carburization is in the state that flake-like carbides are generated at the grain boundaries as shown in the left drawing of Fig. 1C. When the temperature is raised to the secondary carburization start temperature, fine carbides are generated within the grains in the course of raising temperature as shown in the middle drawing of Fig. 1C. When the secondary carburization is performed from this state, both fine carbides existing within the grains and flake-like carbides generated at the grain boundaries grow as shown in the right drawing of Fig. 1C.
    In both cases of Figs. 1B and 1C, the flake-like, coarse carbides generated at the grain boundaries will be the cause of reducing strength of high-concentration carburized steel.
  • In contrast, when the primary carburization is completed in the state of retaining the primary carburization temperature at the same temperature as in the conventional art or lower than that, the structure of the steel material after completion of the primary carburization is in the state that coarse carbides are not generated at the grain boundaries as shown in the left drawing of Fig. 1D. Also, when the secondary carburization start temperature is lower than the primary carburization temperature by 100°C or more while raising, after cooling the steel material, the temperature to the secondary carburization start temperature, the surface temperature of the steel material can surely be adjusted to temperature lower than the Acm line. Therefore, at the point where the temperature reaches the secondary carburization start temperature, fine carbides are generated within the grains as shown in the middle drawing of Fig. 1D.
    When the temperature is retained, from this state, at the same level as the secondary carburization start temperature or when the temperature is stepwisely or continuously raised from the secondary carburization start temperature to perform carburization for a predetermined time, carbides within the grains grow without generation of carbides at the grain boundaries.
    Also, with the progress of the secondary carburization, the surface carbon concentration increases, and the Acm line temperature of the surface also increases. Therefore, when conditions of the secondary carburization initial step are optimized, the quenching temperature does not exceed the Acm line temperature of the surface even when the temperature of the steel material is raised to the quenching temperature. As a result, as shown in the right drawing of Fig. 1D, carbides in the grains can be allowed to grow without generation of carbides at the grain boundaries.
  • In order to prevent precipitation of flake-like, coarse carbides at the grain boundaries, the primary carburization must be performed at temperature higher than the Acm line and the secondary carburization must be performed at temperature lower than the Acm line. The manufacturing method for high-concentration carburized steel of the invention can provide a sufficient temperature difference between after completion of the primary carburization and upon initiation of the secondary carburization, and hence generation of flake-like, coarse carbides can surely be suppressed even when steel materials are not uniform in composition between lots. Also, since it is not necessary to raise the temperature of the primary carburization for providing a sufficient temperature difference, durability of the furnace is not reduced. Further, since carburization is continued, after a predetermined time after the temperature reaches the secondary carburization start temperature, by raising the temperature to the quenching temperature, the carbon concentration of the surface can reach the intended concentration in a short time.
    • Examples (Examples 1 to 15 and Comparative Examples 1 to 5) [1. Preparation of samples]
  • Carburization is performed with steel materials having various compositions under various conditions. Additionally, every carburization is performed in two steps of the primary carburization and the second carburization. Also, except for Example 15 and Comparative Example 1, the secondary carburization is performed in two steps of the secondary initial step of retaining the temperature for a predetermined time at a definite level (low temperature) and the secondary carburization late step of raising the temperature to the quenching temperature (high temperature) and retaining at the temperature for a predetermined time. A typical carburization treatment pattern is shown in Fig. 2.
  • In all of the primary carburization, secondary initial carburization, and secondary late carburization, these carburizations are performed by repeating the following procedures (1) and (2) for 4 times in total:
    1. (1) performing carburization by flowing a carburizing gas for a time corresponding to 2% of the total carburization time; and
    2. (2) diffusing by vacuum pumping for a time corresponding to 23% of the total carburization time.
      However, in Example 15, the secondary carburization start temperature is set to 750°C, the temperature is raised up to the quenching temperature of 850°C over 40 minutes with performing carburization and, after the temperature reaches the quenching temperature, quenching is immediately performed.
      Also, in the secondary carburization initial step of Comparative Example 2, a procedure of performing carburization by flowing a carburizing gas for a time corresponding to 3% of the total carburization time and a procedure of diffusing by vacuum pumping for a time corresponding to 22% of the total carburization time are repeated for 4 times in total.
      Further, in the secondary carburization initial step of Comparative Example 3, a procedure of performing carburization by flowing a carburizing gas for a time corresponding to 1% of the total carburization time and a procedure of diffusing by vacuum pumping for a time corresponding to 24% of the total carburization time are repeated 4 times in total.
    [2. Testing method]
  • The surface carbon concentration after completion of the primary carburization is determined by measuring distribution of cross-sectional carbon concentration through EPMA and calculating an average carbon concentration in the region of 10 µm from the surface. Also, diameter of carbide after completion of the primary carburization and diameter after quenching are measured by photographing using SEM after corroding the cross-section of the sample with picral, with the maximum value of the particle size of carbides existing in 1 mm2 being taken as "particle size of carbides". Further, fatigue strength after quenching is measured by the rotating bending fatigue test (according to JIS Z 2274).
    • [3. Results]
  • Compositions of individual steel materials, carburization conditions, and test results are shown in Table 1.
    In Comparative Example 1, coarse carbides of larger than 10 µm are generated after quenching. This may be attributed to that, since the secondary carburization initial step is omitted and the secondary carburization late step at 885°C is immediately performed, fine carbides generated in the course of the secondary carburization again undergoes solid dissolution.
    Also, in Comparative Example 2, coarse carbides of larger than 10 µm are generated after quenching. The reason for this is that the primary carburization is excessive and, at the point of completion of the primary carburization, coarse carbides are already generated.
    Also, in Comparative Example 3, coarse carbides of larger than 6 µm are generated. This may be attributed to that, since the primary carburization is insufficient and the surface carbon concentration does not reach the eutectoid carbon concentration, fine carbides are not generated within the grains at the point when the temperature reaches the secondary carburization start temperature.
    Also, in Comparative Example 4, the fatigue strength is low, though coarse carbides do not exist. This may be attributed to that, since the secondary carburization initial temperature is the same as the secondary carburization late temperature and the diffusion rate of carbon is slow, a sufficient amount of carbides are not generated.
    Further, in Comparative Example 5, coarse carbides of larger than 7 µm are generated. This may be attributed to that, since the retaining time of retaining at the secondary carburization initial temperature is short, the surface temperature of the steel material exceeds the Acm line when the temperature is raised to the secondary carburization late temperature.
    Therefore, in all of Comparative Examples 1 to 5, the fatigue strength is less than 700 MPa.
  • In contrast, in all of Examples 1 to 15, the fatigue strength is 700 MPa or more. This may be attributed to that, since the primary carburization, secondary carburization initial procedure, and secondary carburization late procedure are performed under proper conditions, fine and spherical carbides are formed in a large amount within the grains without generating flake-like, coarse carbides at the grain boundaries.
  • [Table 1]
    Composition of Steel material (mass%) Carburizing Gas Primary Carburization Secondary Carburization Results
    C Si Mn Cr Carburization Temp. °C Surface Carbon Concent ration mass% Grain Size of Carbide µm Cooling Rate °C/min Initial Temp. °C Carburization Time min Late Temp. °C Carburization Time min Grain Size of Carbide µm Fatigue Strength MPa
    Example 1 0.18 0.57 0.60 1.93 Acetylene 951 0.73 0.7 140 732 20 872 38 1.7 886
    Example 2 0.17 0.72 0.52 1.34 Acetylene 933 0.53 0.2 245 782 21 840 17 1.3 947
    Example 3 0.20 0.54 0.37 1.57 Acetylene 981 0.72 0.0 268 766 21 848 20 1.1 922
    Example 4 0.15 0.77 0.44 1.92 Propane 978 0.71 0.0 655 757 33 851 33 1.1 925
    Example 5 0.15 0.46 0.68 1.86 Propane 959 0.79 0.0 385 766 42 866 57 1.0 964
    Example 6 0.16 0.61 0.49 1.86 Propane 973 0.51 0.0 413 736 52 887 38 1.1 928
    Example 7 0.24 0.64 0.50 1.69 Acetylene 953 0.70 0.0 162 758 50 854 50 1.2 935
    Example 8 0.15 0.53 0.73 1.38 Acetylene 998 0.53 1.7 265 778 25 857 16 2.8 829
    Example 9 0.21 0.47 0.69 1.44 Propane 983 0.64 0.0 487 751 28 825 52 1.1 932
    Example 10 0.23 0.44 0.59 1.48 Acetylene 943 0.50 1.4 46 783 43 890 34 2.5 830
    Example 11 0.23 0.79 0.55 1.87 Propane 971 0.76 2.2 813 713 29 877 34 3.2 836
    Example 12 0.25 0.53 0.65 1.50 Acetylene 972 0.65 0.0 728 764 30 841 42 1.2 922
    Example 13 0.16 0.43 0.67 1.34 Acetylene 985 0.80 0.0 748 772 51 856 51 1.2 931
    Example 14 0.18 0.49 0.68 1.32 Propane 925 0.61 2.1 517 731 52 841 40 3.2 810
    Example 15 0.24 0.61 0.33 1.29 Acetylene 945 0.77 2.1 10 * 3.3 816
    Comparative Example 1 0.19 0.68 0.66 1.48 Acetylene 978 0.62 0.0 595 - - 885 51 10.1 425
    Comparative Example 2 0.21 0.67 0.62 1.52 Acetylene 945 0.95 10.3 48 810 53 879 34 11.4 404
    Comparative Example 3 0.21 0.73 0.60 1.99 Propane 998 0.45 0.0 11 768 32 856 41 6.2 644
    Comparative Example 4 0.22 0.48 0.31 1.87 Propane 923 0.79 0.0 675 755 34 755 21 1.0 574
    Comparative Example 5 0.16 0.79 0.36 1.70 Propane 980 0.64 0.0 413 723 5 856 30 7.1 661
    *Example 15: Temperature is raised 750 → 850°C in 40 minutes with performing carburization.
    • Industrial Applicability
  • The manufacturing method for high-concentration carburized steel of the invention can be used as a manufacturing method for mechanical members such as shafts, bearings, gear wheels, piston pins, and cams.
  • Although the invention has been described in detail and by reference to particular embodiments, it is apparent to those skilled in the art that various alterations and modifications can be made without departing from the spirits and the scope of the invention. This application is based on Japanese Patent Application filed on Nov. 6, 2006 (Japanese Patent Application No. 2006-299836 ), and the contents thereof are incorporated herein by reference.

Claims (5)

  1. A manufacturing method for high-concentration carburized steel, comprising:
    (i) a primary carburization step of carburizing a steel material having C of 0.15-0.30 mass%, Si of 0.40-0.80 mass%, Mn of 0.3-0.8 mass%, Cr of 1.25-2.00 mass%, and balance of Fe and unavoidable impurities at a primary carburization temperature T1(°c) till a surface carbon concentration C becomes Ceu<C≤C(Acm), wherein Ceu is an eutectoid carbon concentration of the steel material, and C(Acm) is a carbon concentration corresponding to a Acm line of the aforesaid steel material at the primary carburization temperature T1;
    (ii) a cooling step of cooling the steel material to 700°C or lower at a cooling rate of 1°C/min or more after completion of the primary carburization step;
    (iii) a secondary carburization initial step of raising the temperature of the steel material to a secondary carburization start temperature T2s to carburize the steel material at a secondary carburization temperature T2, wherein Ac1 point (°C) ≤ T2s (°C) ≤ primary carburization temperature T1 - 100°C ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material immediately after initiation of the secondary carburization, and T2s ≤ T2 ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material;
    (iv) a secondary carburization late step of raising the temperature, after completion of the secondary carburization initial step, to a quenching temperature Tq (°C) to further carburize at the quenching temperature of Tq, wherein Tq ≤ Acm line temperature (°C) corresponding to the surface carbon concentration of the steel material); and
    (v) a step of quenching the steel material after completion of the secondary carburization.
  2. The manufacturing method for high-concentration carburized steel as set forth in claim 1, wherein the primary carburization temperature T1 is 1,100°C or lower.
  3. The manufacturing method for high-concentration carburized steel as set forth in claim 1 or 2, wherein the secondary carburization initial step is a step of performing the carburization for a period of 15 minutes or longer with retaining the secondary carburization temperature T2 at the secondary carburization start temperature T2s.
  4. The manufacturing method for high-concentration carburized steel as set forth in claim 1 or 2, wherein the secondary carburization initial step is a step of performing the carburization with raising the secondary carburization temperature T2 stepwisely or continuously from the secondary carburization start temperature T2s to the quenching temperature Tq.
  5. The manufacturing method for high-concentration carburized steel as set forth in any one of claims 1 to 4, wherein the secondary carburization late step is a step of performing the carburization for a period of 15 minutes or longer at the quenching temperature Tq.
EP07830687A 2006-11-06 2007-10-26 Process for producing high-concentration carburized steel Withdrawn EP2085493A4 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2006299836A JP4971751B2 (en) 2006-11-06 2006-11-06 Manufacturing method of high-concentration carburized steel
PCT/JP2007/070953 WO2008056552A1 (en) 2006-11-06 2007-10-26 Process for producing high-concentration carburized steel

Publications (2)

Publication Number Publication Date
EP2085493A1 true EP2085493A1 (en) 2009-08-05
EP2085493A4 EP2085493A4 (en) 2009-11-25

Family

ID=39364374

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07830687A Withdrawn EP2085493A4 (en) 2006-11-06 2007-10-26 Process for producing high-concentration carburized steel

Country Status (5)

Country Link
US (1) US20100126632A1 (en)
EP (1) EP2085493A4 (en)
JP (1) JP4971751B2 (en)
CN (1) CN101535522B (en)
WO (1) WO2008056552A1 (en)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120099519A (en) * 2010-01-27 2012-09-10 제이에프이 스틸 가부시키가이샤 Case-hardened steel and carburized material
CN102676983B (en) * 2011-03-11 2014-03-26 青岛德盛机械制造有限公司 Carburization processing method
CN102796852B (en) * 2012-07-16 2014-07-02 鑫光热处理工业(昆山)有限公司 Carburizing reinforced isothermal quenching workpiece and processing method thereof
WO2014034150A1 (en) * 2012-09-03 2014-03-06 新日鐵住金株式会社 Carburized component
CN102877072B (en) * 2012-10-15 2014-08-27 常州市新城光大热处理有限公司 Technology for quickly carburizing gear like parts at variable temperatures and carbon potentials
CN102912282B (en) * 2012-10-24 2017-06-20 哈尔滨东安发动机（集团）有限公司 The secondary carburizing process method of 16Cr3NiWMoVNbE materials
EP3000910A4 (en) * 2013-05-10 2017-01-25 Hitachi, Ltd. Software and method for calculating carbon concentration distribution
JP6337580B2 (en) * 2013-06-26 2018-06-06 大同特殊鋼株式会社 Carburized parts
WO2015098106A1 (en) * 2013-12-27 2015-07-02 新日鐵住金株式会社 Carburized-steel-component production method, and carburized steel component
JP6425025B2 (en) * 2015-02-23 2018-11-21 大同特殊鋼株式会社 Method of manufacturing high concentration carburized steel
CN104726819B (en) * 2015-03-20 2017-09-19 上海人本集团有限公司 Carburizing Heat-Treatment of Steel carburization process
CN104949769B (en) * 2015-06-23 2018-04-03 南车戚墅堰机车有限公司 A kind of method that the change of carburizing temperature field is quickly found not against temp measuring system
CN109201966A (en) * 2018-10-30 2019-01-15 安徽芜湖海螺建筑安装工程有限责任公司 The anti-anchoring piece bending cutter assembly that bursts apart
CN109201967A (en) * 2018-10-30 2019-01-15 安徽芜湖海螺建筑安装工程有限责任公司 Resisting fractre anchoring piece bending cutter assembly
CN109321871A (en) * 2018-10-30 2019-02-12 安徽芜湖海螺建筑安装工程有限责任公司 The anti-anchoring piece bending cutter material and preparation method thereof that bursts apart
CN109207912A (en) * 2018-10-31 2019-01-15 安徽芜湖海螺建筑安装工程有限责任公司 Anti-drag anchoring part and preparation method thereof
CN109338274A (en) * 2018-11-21 2019-02-15 中国航发哈尔滨东安发动机有限公司 A kind of 15Cr14Co12Mo5Ni2WA steel secondary low-voltage vacuum carburization method
CN110923411B (en) * 2019-12-11 2021-07-30 洛阳北方易初摩托车有限公司 Carburizing and quenching tissue refining process method for box type multipurpose furnace
CN111140161B (en) * 2019-12-30 2021-10-22 无锡森亘精密机械有限公司 Drill shank for special equipment for mine and production process thereof
CN111826604B (en) * 2020-07-15 2022-03-01 湖南南方宇航高精传动有限公司 Method for performing differential deep carburization on different parts of same part
CN113943916A (en) * 2021-10-20 2022-01-18 石家庄双剑工具有限公司 File manufacturing process
CN113969389A (en) * 2021-10-28 2022-01-25 惠州市思逸臻实业有限公司 Low-temperature carburizing process for screw production
CN115287584B (en) * 2022-08-08 2024-04-12 重庆齿轮箱有限责任公司 Carburizing and quenching method for medium alloy carburizing steel

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5569252A (en) * 1978-11-20 1980-05-24 Komatsu Ltd Carburizing method for steel
JPH083629A (en) * 1994-06-15 1996-01-09 Sumitomo Metal Ind Ltd Carburizing and quenching method
US20060130935A1 (en) * 2004-12-10 2006-06-22 Daido Stell Co., Ltd. & Honda Moto Co., Ltd. Carburized component and method of manufacturing the same

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2808621B2 (en) 1988-11-28 1998-10-08 大同特殊鋼株式会社 Method of carburizing steel
JPH06108226A (en) * 1992-09-30 1994-04-19 Daido Steel Co Ltd Carburizing heat treatment of steel-made parts
JP3413975B2 (en) * 1994-08-08 2003-06-09 日本精工株式会社 Rolling bearing with excellent wear resistance
JP3894635B2 (en) * 1997-08-11 2007-03-22 株式会社小松製作所 Carburized member, manufacturing method thereof, and carburizing system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5569252A (en) * 1978-11-20 1980-05-24 Komatsu Ltd Carburizing method for steel
JPH083629A (en) * 1994-06-15 1996-01-09 Sumitomo Metal Ind Ltd Carburizing and quenching method
US20060130935A1 (en) * 2004-12-10 2006-06-22 Daido Stell Co., Ltd. & Honda Moto Co., Ltd. Carburized component and method of manufacturing the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO2008056552A1 *

Also Published As

Publication number Publication date
WO2008056552A1 (en) 2008-05-15
CN101535522A (en) 2009-09-16
US20100126632A1 (en) 2010-05-27
CN101535522B (en) 2011-05-18
JP4971751B2 (en) 2012-07-11
EP2085493A4 (en) 2009-11-25
JP2008115427A (en) 2008-05-22

Similar Documents

Publication Publication Date Title
EP2085493A1 (en) Process for producing high-concentration carburized steel
RU2518840C2 (en) Case-hardened steel element and method of its production
EP1847630B1 (en) High-concentration carburized/low-strain quenched member and process for producing the same
EP2796586A1 (en) Steel for mechanical structure for cold working, and method for manufacturing same
EP3276040B1 (en) Nitrided or soft nitrided part with excellent wear resistance and pitting resistance
EP2562283A1 (en) Steel component having excellent temper softening resistance
JP4881577B2 (en) Vacuum carburized parts and manufacturing method thereof
JP4229609B2 (en) Carburized and hardened gear and manufacturing method thereof
JP2005163173A (en) Gear part and method of producing thereof
WO2003056054A1 (en) Carburized and quenched member and method for production thereof
JPWO2019198539A1 (en) Machine parts and their manufacturing methods
JP2008057017A (en) Carburized component or carbo-nitrided component made of steel
EP1847631B1 (en) Carburized component and manufacturing method thereof
JP4501573B2 (en) Gear and gear manufacturing method
JP4073860B2 (en) Manufacturing method of carburized steel with excellent coarsening resistance after high-temperature carburizing
EP2548976A1 (en) Spring steel and surface treatment method for steel material
EP3020841B1 (en) Coil spring, and method for manufacturing same
JP2010222636A (en) Surface treatment method of steel product
JP3644217B2 (en) Induction-hardened parts and manufacturing method thereof
JPH0559527A (en) Production of steel excellent in wear resistance and rolling fatigue characteristic
JP4149576B2 (en) Method for producing high-temperature carburizing steel and high-temperature carburizing steel obtained by the method
JP7010320B2 (en) Rough material for vacuum carburizing and its manufacturing method
KR102177936B1 (en) High-temperature carburizing heat treatment method after Pre-nitriding
JP2636661B2 (en) High-strength steel part with excellent fatigue strength and method of manufacturing the same
JP2021046596A (en) High-concentration carburized gear component

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20090505

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE SI SK TR

A4 Supplementary search report drawn up and despatched

Effective date: 20091026

DAX Request for extension of the european patent (deleted)
17Q First examination report despatched

Effective date: 20100413

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

RTI1 Title (correction)

Free format text: MANUFACTURING METHOD FOR HIGH-CONCENTRATION CARBURIZED STEEL

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20110426