US20050173026A1 - Carburized and quenched member and method for production thereof - Google Patents

Carburized and quenched member and method for production thereof Download PDF

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Publication number
US20050173026A1
US20050173026A1 US10/473,716 US47371604A US2005173026A1 US 20050173026 A1 US20050173026 A1 US 20050173026A1 US 47371604 A US47371604 A US 47371604A US 2005173026 A1 US2005173026 A1 US 2005173026A1
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carburized
quenching
carburizing
steel
cooling
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US10/473,716
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Inventor
Takao Taniguchi
Kazumasa Tsukamoto
Kouji Ohbayashi
Tomoki Hanyuda
Yutaka Kurebayashi
Hideo Kanisawa
Seiji Itoh
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Aisin AW Co Ltd
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Aisin AW Co Ltd
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Assigned to AISIN AW CO., LTD. reassignment AISIN AW CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ITOH, SEIJI, KANISAWA, HIDEO, HANYUDA, TOMOKI, KUREBAYASHI, YUTAKA, OHBAYASHI, KOUJI, TSUKAMOTO, KAZUMASA, TANIGUCHI, TAKAO
Publication of US20050173026A1 publication Critical patent/US20050173026A1/en
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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
    • C23C8/06—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
    • 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

Definitions

  • the present invention relates to a carburized and hardened member that is excellent in fatigue strength and dimensional accuracy, and a production method for the member.
  • carburized and hardened members subjected to a carburizing and quenching process are often used in order to increase the surface hardness and the toughness.
  • Conventional carburized and hardened members are normally produced by forming a case hardening steel (JIS: SCM420H, SCR420H, SNCM220) or the like into a desired shape, and then gas-carburizing the steel in a carburizing atmosphere, and then quenching it in an oil or the like.
  • JIS Japanese Industrial Standard SCM420H, SCR420H, SNCM220
  • the present invention has been accomplished in view of the aforementioned problems of the conventional art. It is an object of the present invention to provide a carburized and hardened member that allows strength enhancement while sufficiently reducing the hardening strain, and a production method for the carburized and hardened member.
  • the aforementioned hardenability J based on an end quenching test is a value acquired by an end quenching test method prescribed in JIS: G0561 (generally termed “Jominy end quench test method”). Furthermore, the indication of (at 12.5 mm) means that the value of hardenability J is a value of hardenability J regarding a position of 12.5 mm from the water cool-side end surface of a rod-like test piece in the Jominy end quench test method.
  • a specific alloy of which the C content and the Si content and the hardenability J are within the specific ranges is used as a raw material.
  • the quenching process is performed so as to fulfill the aforementioned conditions of monotonous cooling and the aforementioned condition of specific severity of quenching H. That is, only after the material characteristics and the production conditions are fulfilled, it becomes possible to provide a carburized and hardened member in which the strength is enhanced while the hardening strain is sufficiently reduced.
  • the setting of the C content within the range of 0.1 to 0.50 wt. % makes it possible to secure an appropriate toughness and an appropriate strength of a non-carburized portion (internal portion) after the carburizing and quenching process. If the C content is less than 0.1 wt. %, the aforementioned effect is not sufficient. If the C content exceeds 0.50 wt. %, the pre-quenching hardness becomes excessively high, thus creating a possibility of increased processing cost and reduced toughness. Furthermore, due to increased structural transformation rate of the interior of the non-carburized portion following the carburizing and quenching process, transformation stress increases, and due to great quenching strain, the component part accuracy may degrade.
  • the Si content is less than 0.50 wt. %, the aforementioned improvement effect is small; in particular, there is a problem of reduction of intergranular oxidation preventative effect at the time of the carburizing process. Conversely, if the Si content is greater than 1.50 wt. %, the improvement effect becomes saturated, and uniform austenitization prior to quenching is difficult. In order to prevent or curb degradations in the plastic processability, the cutting processability and the formability of the material, it is preferable that the Si content be less than or equal to 0.70 wt. %. Therefore, a preferable range of the Si content is a range greater than 0.50 wt. % and less than or equal to 0.70 wt. %.
  • the hardenability J of the material is limited within the range of 35 to 50 (at 12.5 mm). Therefore, excellent hardening effect can be achieved even if the range of the severity of quenching H is limited to the aforementioned range. If the hardenability J is less than 35, it becomes impossible to achieve sufficient hardening effect on the carburized layer and the non-carburized portion (internal portion) in the quenching process following the carburizing process, and it is therefore impossible to achieve a desired strength enhancement. Therefore, it is preferable that the hardenability J be greater than or equal to 38. If the hardenability J exceeds 50, the structural transformation rate of the internal portion, that is, the non-carburized portion, rises, so that the transformation stress increases and the hardening strain becomes more likely.
  • hardenability J If the hardenability J is higher, the hardness prior to the carburizing and quenching process is correspondingly higher, so that processability, such as the plastic processability prior to the carburizing process, the cutting processability, etc., degrades. Therefore, in order to prevent such degradation of workability, it is preferable that hardenability J be less than or equal to 45.
  • the severity of quenching H is less than 0.01 (cm ⁇ 1 ), it is impossible to achieve sufficient hardening effect on the carburized layer and the non-carburized portion (internal portion) in a hardening process following the carburizing process as in the case where the hardenability J is less than 35. Therefore, desired strength enhancement cannot be accomplished. If the severity of quenching H is greater than 0.08 (cm ⁇ 1 ), the transformation stress increases due to, particularly, increased structural transformation rate of the internal portion, that is, the non-carburized portion, and therefore the hardening strain is likely to occur, as in the case where the hardenability J is greater than 50.
  • the quenching process is performed under the condition that the cooling monotonously occurs from the A1 point to the Ms point, in addition to the condition of the range of severity of quenching H.
  • the term “monotonously” herein means that re-heating is not performed during the cooling process, that is, there is no rise of the material temperature during the cooling. Therefore, examples of the case where the condition of monotonous cooling is fulfilled include a case where the material temperature continues to fall, and a case where if the temperature stops falling during the process, the temperature remains constant and never rises, and then starts falling again. Furthermore, changes in the cooling rate are allowable.
  • the monotonous cooling condition it is possible to select a cooling condition such that the cooling does not enter a region of a nose of an S curve indicated in an isothermal transformation diagram within the carburized portion. This selection secures sufficient martensite transformation.
  • the present invention provides a carburized and hardened member in which the strength is enhanced while the hardening strain is sufficiently reduced, as the invention comprises the aforementioned C content, the Si content, the hardenability J, the carburizing process in an oxidation inhibitive atmosphere, and the quenching process that fulfills the condition of the monotonous cooling and the condition of the specific severity of quenching H. If any one of these elements is absent, the intended object cannot be achieved.
  • the present inventors have discovered this through many experiments.
  • a second aspect of the present invention is a carburized and hardened member produced by the above-described production method, characterized in that a surface hardness of the carburized layer is in a range of 700 to 900 Hv, and an internal hardness of a non-carburized portion located inward of the carburized layer is in a range of 250 to 450 Hv.
  • the surface hardness of the carburized layer is less than 700 Hv, a conceivable problem is that strength cannot be secure corresponding to the stress concentration adjacent to the surfaces of the member. Another conceivable problem is insufficient abrasion resistance in outermost surface. If the surface hardness is greater than 900 Hv, production of carbide, such as cementite and the like, in the surface layer is conceivable. Therefore, a conceivable problem is insufficient strength and, more particularly, reduced toughness.
  • the internal hardness of the non-carburized portion is less than 250 Hv, the problem of insufficient strength and, more particularly, insufficient static strength, can be considered. If the internal hardness is greater than 450 Hv, the following problem is possible, taking the rate of transformation of structure into consideration. That is, when a hardening process is performed so as to secure 450 Hv, a great transformation stress occurs, which causes a great hardening strain and therefore makes a factor of degradation in component parts accuracy.
  • FIG. 1 is an illustration of a rotating bending fatigue test piece.
  • the carburizing process be performed in a reduced-pressure atmosphere having a reduced pressure of 1 to 30 hPa. Therefore, it becomes possible to easily provide the oxidation inhibitive atmosphere through pressure reduction, and therefore sufficiently prevent intergranular oxidation at the time of carburization.
  • the value of the reduced pressure of the reduced-pressure atmosphere being less than 1 hPa is excessive for substantial prevention of oxidation. If such value of the reduced pressure is required, the device for the pressure reduction needs to have high capability for pressure reduction, and creates a problem of cost increase. If the value of the reduced pressure is higher than 30 hPa, the oxidation preventing effect degrades, and furthermore, other problems, such as production of soot in the carburizing furnace, and the like, occur.
  • the carburizing process be performed so that a surface carbon amount in the carburized layer becomes 0.6 to 1.5 wt. % (claim 4 ).
  • the surface carbon concentration in the carburized layer affects the surface hardness of the carburized and hardened member. If the surface carbon amount in the carburized layer is less than 0.6 wt. %, there occurs a problem of insufficient surface hardness. If the surface carbon amount is greater than 1.5 wt. %, the precipitation of carbide becomes great so that the hardenability of the base remarkably degrades and the surface hardness becomes insufficient.
  • the intergranular strength decreases if an intergranular oxide (portion) is produced. Therefore, if intergranular oxidation reaches a depth beyond 3 ⁇ m, there is a danger of reduced abrasion resistance due to insufficient strength of the member, reduced hardness, etc. Furthermore, at the time of intergranular oxidation, surrounding alloy elements are also taken up into the intergranular oxide due to chemical reactions. Therefore, the hardenability-improving elements in the carburized and hardened layer around intergranular oxides are taken up and consumed by the intergranular oxides, thereby forming regions where additives are depleted, around the intergranular oxide layer. Therefore, the hardenability of the carburized and hardened layer becomes insufficient. Hence; there is a danger of causing insufficient hardness and insufficient strength.
  • the surface compression residual stress can be produced by forming the martensite via the quenching process of the carburized layer, and creating a compression stress field due to volume expansion involved in the transformation.
  • the amount of martensite produced is small, that is, if the amount of retained austenite is great, or if the troostite structure is great in amount, it is impossible to form a sufficient compression residual stress field. Therefore, the reduction of the retained austenite (specifically, to 25% or less) and the reduction of the troostite structure (specifically, to 10% or less) are effective in view of enhancement of compression residual stress effect.
  • the absorption of volume expansion at the time of martensite transformation does not considerably contribute to enhancement of the surface compression residual stress if the amount of martensite is small.
  • the compression residual stress can be increased by performing a surface process, such as shot peening, after the quenching process.
  • a surface process such as shot peening
  • turning the retained austenite into martensite by the shot peening process is more advantageous in increasing the compression residual stress.
  • quenching be performed with the severity of quenching H being in said range during a transition from a temperature in an austenite region to 300° C. Therefore, sufficient quenching effect can be achieved. If the severity of quenching H in a cooling process from the temperature of the austenite region to 300° C. is less than 0.01 (cm ⁇ 1 ), the quenching will be insufficient. Thus, desired hardened structure and characteristic cannot be achieved, and the strength of the member will be insufficient. If the severity of quenching H in a cooling process from the temperature of the austenite region to 300° C. is greater than 0.08 (cm ⁇ 1 ), the quenching will be excessive, so that the structure transformation stress and the thermal stress will increase. Therefore, there is a possibility of increased hardening strain and degraded component part accuracy.
  • quenching be accomplished by gas cooling. Therefore, it becomes relatively easy to secure the aforementioned severity of quenching H.
  • the quenching by gas cooling use an inert gas. Therefore, a safety can be secured during the quenching.
  • the inert gas be a nitrogen gas.
  • the adoption of nitrogen gas as the aforementioned inert gas is preferable in view of cost, ease of handling, availability at the time of mass-production operation, etc.
  • a retained austenite area rate of the carburized layer preferably is at most 25%. If the retained austenite area rate is greater than 25%, structural transformation from retained austenite into martensite occurs in association with changes in temperature and operating stress during a working process after the carburizing and quenching process, or during the use of the member. Due to the stress of the transformation, strain occurs, and the component parts accuracy will likely degrade. It is more preferable that the retained austenite area rate be 20% or less.
  • the retained austenite area rate can be reduced by other manners. For example, the area rate can be reduced by forcibly turning the retained austenite into martensite via shot peening or the like.
  • a troostite structure area rate of a surface layer of the carburized layer be at most 10%.
  • the troostite is a slack-quenched structure formed in the carburized layer after the carburizing and quenching process, and has a low hardness. Therefore, if the troostite structure area rate is greater than 10%, low-strength troostite will reduce the strength of the component part.
  • an internal structure of the carburized and hardened member be bainite. More-specifically, it is desirable that the area rate of bainite in a sectional structure be at least 50%. Unlike the case of martensite, transformation of bainite progresses while iron atoms forming a lattice partially diffuse. Therefore, the strain associated with transformation is less in bainite than in martensite. Furthermore, bainite has a greater hardness than pearlite, which is produced if the cooling rate is lower. Thus, bainite appropriately enhances the strength of the internal non-carburized layer.
  • the carburized and hardened member be a carburized toothed gear.
  • the toothed gears require various strict conditions. The excellent characteristics achieved by the above-described production method are very effective for the toothed gears.
  • Step 11 to Steel 14 having chemical compositions shown in Table 1, after being melt-formed in an arc furnace, were hot-rolled into round bars having a diameter of 150 mm and a diameter of 32 mm.
  • the round bars were normalized by keeping them at 925° C. for an hour and then air-cooling them.
  • Steel 11 and Steel 12 are steel grades having new compositions developed in the example.
  • Steel 13 and Steel 14 are steel grades corresponding to case hardening steels SCM420 and SNCM 815 according to JIS.
  • a hardenability J was determined by conducting a Jominy end quenching method according to JIS: G0561.
  • test spur gears 4 Normalized materials of 150 mm in diameter were machined into test spur gears 4 having a pitch radius of 54 mm, 27 teeth, a module of 4, a facewidth of 9 mm, a shaft hole radius of 35 mm (an equivalent round bar diameter of 10.5 mm ⁇ ) as shown in FIG. 2 .
  • the severity of quenching H after the carburization is 0.05 (cm ⁇ 1 ) as shown in Table 2, and the elements of the production method of the present invention are included.
  • a hardness distribution (internal hardness) of a cross section was investigated using a Vickers hardness meter.
  • the surface layer hardness (surface hardness) of each carburized member was measured at a position of 0.02 mm from the surface.
  • the troostite area rate was measured by image analysis of scanning electron micrographs.
  • the surface carbon concentration was measured at a position of 50 ⁇ m from the surface via an X-ray macroanalyzer.
  • an internal layer portion can be provided with a structure in which bainite is major if the cooling rate is set at 0.1 to 1° C./sec. It is particularly desirable to select such a composition that the cooling at 3° C./sec. will provide a structure mainly formed by bainite.
  • steels indicated in Table 6 (Steels 21 to 24 and Steels 31 to 38) were melted and formed into ingots, which were bloom-rolled and bar-rolled to produce round bars of 70 mm in diameter.
  • Process 4 is characterized by vacuum carburization and gas cooling. In this process, steel is carburized and quenched and then tempered in the manner of heating at 930° C. for 5 hours ⁇ diffusion at 850° C. for 1 hour ⁇ nitrogen gas cooling ⁇ tempering at 180° C. for 1 hour.
  • the severity of quenching H in this case is 0.05 (cm ⁇ 1 ).
  • Process 5 is similar to Process 4, except that the nitrogen gas cooling in Process 4 is changed to oil quenching at 130° C.
  • the severity of quenching H in this case is 0.15 (cm ⁇ 1 ).
  • test pieces and the gears processed by the above-described process were subjected to measurements, tests, and the like as in Example 1.
  • Steel Grades 31 to 34 had a slack quenched structure due to intergranular oxidation formation at the time of gas carburization, and therefore exhibited low surface hardness and low strengths. Furthermore, since oil cooling causes rapider quenching and greater non-uniformity in cooling than gas cooling, the variation in precision due to hardening strain increased.
  • each of Steel Grades 21 to 24 exhibited a high surface hardness and an appropriate value of internal hardness, and reduced strain. Thus, it is apparent that high strengths and low strains were achieved.
  • this example also indicates that it is possible to increase the strength while sufficiently reducing the hardening strain in the members if a specific alloy steel having a C content, an Si content and hardenability J within the aforementioned specific ranges is used as a raw material, and is subjected to a carburizing process in an oxidation inhibitive atmosphere, thereby forming a carburized layer, and then the steel is quenched under the condition of the specific severity of quenching H.
  • at least one species selected from the group consisting of at most 0.01% by weigh of Ca, at most 0.01% by weight of Mg, at most 0.05% by weight of Zr and at most 0.1% by weight of Te may be contained.

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  • Engineering & Computer Science (AREA)
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JP2001-392410 2001-12-25
JP2001392410 2001-12-25
PCT/JP2002/013561 WO2003056054A1 (fr) 2001-12-25 2002-12-25 Element carbure et trempe et son procede de production

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EP (1) EP1550736A4 (fr)
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KR (1) KR20040088016A (fr)
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WO (1) WO2003056054A1 (fr)

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US20060137766A1 (en) * 2004-12-27 2006-06-29 Nippon Steel Corporation And Honda Motor Co., Ltd. Case-hardening steel superior in tooth surface fatigue strength, gear using the same, and method of production of the same
US20090301608A1 (en) * 2005-04-28 2009-12-10 Aisin Aw Co., Ltd. Carburized and induction-hardened component
US20120312425A1 (en) * 2010-12-08 2012-12-13 Tatsuya Koyama Gas-carburized steel part excellent in surface fatigue strength, steel product for gas carburizing, and manufacturing method of gas-carburized steel part
CN105525252A (zh) * 2015-12-22 2016-04-27 中车戚墅堰机车车辆工艺研究所有限公司 一种盘类渗碳淬火齿轮的变形矫正方法及其专用工装
US9340233B2 (en) 2010-10-15 2016-05-17 Benteler Automobiltechnik Gmbh Method for producing a hot-formed and press-hardened metal component
US9389155B1 (en) * 2013-03-12 2016-07-12 United Technologies Corporation Fatigue test specimen
US10889870B2 (en) 2016-03-08 2021-01-12 Aisin Aw Co., Ltd. Steel component, gear component, and producing method for steel component
CN113926962A (zh) * 2021-10-13 2022-01-14 宿迁弘益工贸有限公司 一种高强度水泥钉生产方法

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WO2004059029A1 (fr) * 2002-12-25 2004-07-15 Aisin Aw Co., Ltd. Élément cémenté et trempé et son procédé de fabrication
JP4876668B2 (ja) * 2006-03-29 2012-02-15 アイシン精機株式会社 鋼部材の熱処理方法
US7550048B2 (en) * 2006-12-15 2009-06-23 Tenneco Automotive Operating Company Inc. Method of manufacture using heat forming
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JP5305820B2 (ja) * 2008-10-08 2013-10-02 アイシン・エィ・ダブリュ株式会社 浸炭部品の製造方法及び鋼部品
US9212416B2 (en) 2009-08-07 2015-12-15 Swagelok Company Low temperature carburization under soft vacuum
US9617632B2 (en) 2012-01-20 2017-04-11 Swagelok Company Concurrent flow of activating gas in low temperature carburization
KR101185060B1 (ko) 2012-03-13 2012-09-21 동우에이치에스티 주식회사 자동변속기용 에뉼러스 기어 열처리 방법
CN104384887A (zh) * 2014-09-19 2015-03-04 马鞍山邦斯科自动化科技有限公司 一种提高铰刀使用寿命的铰刀制造方法
JP6191630B2 (ja) * 2015-01-15 2017-09-06 トヨタ自動車株式会社 ワークの製造方法

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060137766A1 (en) * 2004-12-27 2006-06-29 Nippon Steel Corporation And Honda Motor Co., Ltd. Case-hardening steel superior in tooth surface fatigue strength, gear using the same, and method of production of the same
DE102005061946B4 (de) * 2004-12-27 2013-03-21 Nippon Steel Corp. Einsatzgehärteter Stahl mit hervorragender Zahnoberflächendauerfestigkeit, diesen verwendendes Zahnrad, und Verfahren zur Herstellung desselben
US20090301608A1 (en) * 2005-04-28 2009-12-10 Aisin Aw Co., Ltd. Carburized and induction-hardened component
US8430974B2 (en) 2005-04-28 2013-04-30 Aisin Aw Co., Ltd. Carburized and induction-hardened component
US9340233B2 (en) 2010-10-15 2016-05-17 Benteler Automobiltechnik Gmbh Method for producing a hot-formed and press-hardened metal component
US20120312425A1 (en) * 2010-12-08 2012-12-13 Tatsuya Koyama Gas-carburized steel part excellent in surface fatigue strength, steel product for gas carburizing, and manufacturing method of gas-carburized steel part
US9506137B2 (en) * 2010-12-08 2016-11-29 Nippon Steel & Sumitomo Metal Corporation Gas-carburized steel part excellent in surface fatigue strength, steel product for gas carburizing, and manufacturing method of gas-carburized steel part
US9389155B1 (en) * 2013-03-12 2016-07-12 United Technologies Corporation Fatigue test specimen
CN105525252A (zh) * 2015-12-22 2016-04-27 中车戚墅堰机车车辆工艺研究所有限公司 一种盘类渗碳淬火齿轮的变形矫正方法及其专用工装
US10889870B2 (en) 2016-03-08 2021-01-12 Aisin Aw Co., Ltd. Steel component, gear component, and producing method for steel component
CN113926962A (zh) * 2021-10-13 2022-01-14 宿迁弘益工贸有限公司 一种高强度水泥钉生产方法

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EP1550736A1 (fr) 2005-07-06
EP1550736A4 (fr) 2005-07-06
WO2003056054A1 (fr) 2003-07-10
JPWO2003056054A1 (ja) 2005-05-12
JP4354277B2 (ja) 2009-10-28

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