JP6552209B2 - Method and apparatus for manufacturing metal spring - Google Patents

Method and apparatus for manufacturing metal spring Download PDF

Info

Publication number
JP6552209B2
JP6552209B2 JP2015024398A JP2015024398A JP6552209B2 JP 6552209 B2 JP6552209 B2 JP 6552209B2 JP 2015024398 A JP2015024398 A JP 2015024398A JP 2015024398 A JP2015024398 A JP 2015024398A JP 6552209 B2 JP6552209 B2 JP 6552209B2
Authority
JP
Japan
Prior art keywords
nitriding
furnace
temperature
metal spring
predetermined
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.)
Active
Application number
JP2015024398A
Other languages
Japanese (ja)
Other versions
JP2016148068A (en
Inventor
苅谷　良一
良一 苅谷
寺床　圭一郎
圭一郎 寺床
均 椛澤
均 椛澤
勇 高瀬
勇 高瀬
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.)
SANCALL CORPORATION
Original Assignee
SANCALL CORPORATION
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 SANCALL CORPORATION filed Critical SANCALL CORPORATION
Priority to JP2015024398A priority Critical patent/JP6552209B2/en
Priority to PCT/JP2016/051374 priority patent/WO2016129333A1/en
Publication of JP2016148068A publication Critical patent/JP2016148068A/en
Application granted granted Critical
Publication of JP6552209B2 publication Critical patent/JP6552209B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—Surface hardening
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
    • C21D7/04—Modifying the physical properties of iron or steel by deformation by cold working of the surface
    • C21D7/06—Modifying the physical properties of iron or steel by deformation by cold working of the surface by shot-peening or the like
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/02—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for springs
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16F—SPRINGS; SHOCK-ABSORBERS; MEANS FOR DAMPING VIBRATION
    • F16F1/00—Springs
    • F16F1/02—Springs made of steel or other material having low internal friction; Wound, torsion, leaf, cup, ring or the like springs, the material of the spring not being relevant

Description

本発明は、窒化層が形成された弁ばね等の金属製ばねの製造方法及び製造装置に関する。   The present invention relates to a method and apparatus for manufacturing a metal spring such as a valve spring in which a nitride layer is formed.

鋼材等の金属体の機械的強度を向上させる方法として、処理対象金属体に対して窒化処理を行うことが広く利用されている。   As a method for improving the mechanical strength of a metal body such as a steel material, performing nitriding treatment on a metal body to be treated is widely used.

この窒化処理においては、処理対象金属体の表面に窒化層を形成しつつ化合物層の発生を防止乃至は低減することが重要となる。   In this nitriding treatment, it is important to prevent or reduce the generation of the compound layer while forming a nitride layer on the surface of the metal object to be treated.

即ち、処理対象金属体の表面に化合物層が生成されてしまうと、前記金属体表面近傍の粒界に窒化物や炭窒化物が生じことになる。   That is, when a compound layer is formed on the surface of the metal object to be treated, nitrides and carbonitrides are generated at grain boundaries in the vicinity of the surface of the metal body.

従って、一旦、窒化処理によって化合物層が生成されると、たとえ化合物層を除去したとしても、粒界に生じた窒化物や炭窒化物は残ったままとなり、処理対象金属体の機械的強度を十分には向上できない。
特に、弁ばね等の繰り返し荷重を受ける部材が処理対象金属体とされる場合には、耐久性の観点で問題となる。 Therefore, once a compound layer is formed by nitriding, even if the compound layer is removed, nitrides and carbonitrides formed at grain boundaries remain, and the mechanical strength of the metal object to be treated is reduced. It cannot be improved sufficiently.
In particular, in the case where a member such as a valve spring that receives repeated load is used as the metal object to be treated, this is a problem in terms of durability.

この点に関し、下記特許文献１には、弁ばねの製造方法として、第１の濃度範囲の窒化ガス雰囲気で窒化処理を施し、その後、それよりも低濃度である第２の濃度範囲の窒化ガス雰囲気で窒化処理を施す方法が開示されている。   In this regard, in Patent Document 1 below, as a method of manufacturing a valve spring, nitriding is performed in a nitriding gas atmosphere in a first concentration range, and then a nitriding gas in a second concentration range having a lower concentration than that. A method of nitriding in an atmosphere is disclosed.

詳しくは、前記特許文献１には、窒化ガスの濃度が高い（窒化ポテンシャルが高い）場合には、弁ばね表面の窒素濃度が高まり、弁ばね表面に窒化鉄の化合物層が形成され、一旦、このように表面に窒化鉄の化合物層が形成された後に、窒化ガスの濃度を低濃度とすると、弁ばねの表面においては新規な窒化鉄の化合物層の形成が抑制されると共に、既存の窒化鉄の化合物層が溶解して窒素が弁ばねの内部に拡散する旨の説明がなされている。   Specifically, in Patent Document 1, when the concentration of nitriding gas is high (nitriding potential is high), the nitrogen concentration on the valve spring surface is increased, and a compound layer of iron nitride is formed on the valve spring surface. Thus, after the formation of the compound layer of iron nitride on the surface, if the concentration of the nitriding gas is low, formation of a new compound layer of iron nitride is suppressed on the surface of the valve spring and the existing nitriding There is an explanation that the iron compound layer dissolves and nitrogen diffuses into the valve spring.

しかしながら、実際の窒化処理において、一旦、弁ばね表面に窒化鉄の化合物層が形成された後に、この化合物層を低濃度の窒化ガス雰囲気での窒化処理によって溶解させることは困難である。   However, in an actual nitriding process, once a compound layer of iron nitride is formed on the valve spring surface, it is difficult to dissolve the compound layer by the nitriding process in a low concentration nitriding gas atmosphere.

また、下記特許文献２には、窒化処理の前に、処理対象金属体に対してフッ化処理を行うことにより、窒化処理時に化合物層が生成されることを防止乃至は低減する方法が開示されている。   Patent Document 2 listed below discloses a method for preventing or reducing the formation of a compound layer during nitriding by performing fluorination on the metal object to be treated before nitriding. ing.

しかしながら、この方法では、窒化処理とは別にフッ化処理が必要であり、処理コストの高騰を招くと共に、処理に相当な時間を要するという問題がある。   However, in this method, the fluorination treatment is required separately from the nitriding treatment, which causes the cost of the treatment to rise, and the treatment takes a considerable time.

特開２００４−１８３０９９号公報JP 2004-183099 A 特開２００６−２４９４８６号公報JP, 2006-249486, A

本発明は、斯かる従来技術に鑑みなされたものであり、化合物層の発生を有効に防止しつつ、深い窒化層が形成された金属製ばねを製造する為の製造方法及び製造装置の提供を目的とする。   The present invention has been made in view of such prior art, and provides a manufacturing method and a manufacturing apparatus for manufacturing a metal spring having a deep nitrided layer formed while effectively preventing the generation of a compound layer. To aim.

本発明は、前記目的を達成するために、表面に窒化層が形成された金属製ばねの製造方法であって、所定のばね形状に形成された金属製ばね本体を気密性雰囲気炉内に配置させた状態で炉内温度を所定窒化処理温度まで上昇させる昇温工程と、炉内温度を前記所定窒化処理温度に保持しつつ、前記炉内の窒化ポテンシャルが所定の高レベル値となるようにアンモニアガスを供給する第１窒化工程と、炉内温度を前記所定窒化処理温度に保持しつつ、前記炉内へのアンモニアガスの供給を停止し且つ前記炉内に水素ガス及び窒素ガスを３：１の割合で供給して、前記炉内の窒化ポテンシャルを前記金属製ばね本体に化合物層が生成しない低レベル値まで低下させる窒化ポテンシャル低下工程と、炉内温度を前記所定窒化処理温度に保持し且つ前記炉内の窒化ポテンシャルを前記低レベル値に保持する第２窒化工程とを含み、前記第１窒化工程における窒化ポテンシャルの前記高レベル値は、当該第１窒化工程を所定時間以上に亘って継続すると前記金属製ばね本体に化合物層の生成を招く濃度とされており、前記第１窒化工程の処理時間は化合物層の生成を招く前記所定時間より短く且つ前記所定時間の６０％以上の時間とされている金属製ばねの製造方法を提供する。 The present invention is a method of manufacturing a metal spring having a nitrided layer formed on its surface, in which the metal spring main body formed in a predetermined spring shape is disposed in an airtight atmosphere furnace. In the heated state, the temperature in the furnace is raised to a predetermined nitriding treatment temperature, and while maintaining the temperature in the furnace at the predetermined nitriding treatment temperature, the nitriding potential in the furnace becomes a predetermined high level value A first nitriding step for supplying ammonia gas; and while maintaining the furnace temperature at the predetermined nitriding temperature, supply of ammonia gas to the furnace is stopped and hydrogen gas and nitrogen gas are supplied into the furnace at 3: A nitriding potential reducing step of supplying at a ratio of 1 to reduce the nitriding potential in the furnace to a low level value that does not form a compound layer on the metal spring body, and keeping the temperature in the furnace at the predetermined nitriding treatment temperature And before And a second nitriding step for maintaining the nitriding potential in the furnace at the low level value, wherein the high level value of the nitriding potential in the first nitriding step is to continue the first nitriding step for a predetermined time or more. are the concentrations lead to formation of the compound layer on the metallic spring body, the processing time of the first nitriding step and more than 60% of the time tank and the predetermined time than the predetermined time lead to formation of compound layer The present invention provides a method of manufacturing a metal spring.

好ましくは、前記第１窒化工程の処理時間は、化合物層の生成を招く前記所定時間より短く且つ前記所定時間の８０％以上の時間とされる。 Preferably, the processing time of the first nitriding step is shorter than the predetermined time leading to the formation of the compound layer and is 80% or more of the predetermined time .

好ましくは、前記昇温工程は、前記炉内にアンモニアガスを供給しつつ行われる。   Preferably, the temperature raising step is performed while supplying ammonia gas into the furnace.

好ましくは、本発明に係る前記金属製ばねの製造方法は、前記昇温工程の前に、前記金属製ばね本体に対してショットブラストを行う前処理工程を含み得る。   Preferably, the method for manufacturing a metal spring according to the present invention may include a pretreatment step of performing shot blasting on the metal spring body before the temperature raising step.

好ましくは、本発明に係る前記金属製ばねの製造方法は、前記第２窒化工程の後に、前記金属製ばね本体に対してショットブラスト又はショットピーニングを行う後処理工程を含み得る。   Preferably, the method for manufacturing a metal spring according to the present invention may include a post-processing step of performing shot blasting or shot peening on the metal spring body after the second nitriding step.

また、本発明は、気密性雰囲気炉と、前記雰囲気炉内を加熱する加熱手段と、前記雰囲気炉へのアンモニアガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能なアンモニアガス供給手段と、前記雰囲気炉への水素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な水素ガス供給手段と、前記雰囲気炉への窒素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な窒素ガス供給手段と、前記雰囲気炉内の窒化ポテンシャルを検出する窒化ポテンシャルセンサと、前記雰囲気炉内の温度を検出する温度センサと、制御装置とを備えた金属製ばねの製造装置を提供する。   Further, the present invention can switch between an airtight atmosphere furnace, a heating means for heating the inside of the atmosphere furnace, and supply and stop of supply of ammonia gas to the atmosphere furnace, and the supply amount can be adjusted at the time of supply. Ammonia gas supply means can be switched between supply and stop of hydrogen gas to the atmosphere furnace, and hydrogen gas supply means capable of adjusting the supply amount at the time of supply, supply and supply of nitrogen gas to the atmosphere furnace The nitrogen gas supply means capable of switching the stop and adjusting the supply amount at the time of supply, the nitriding potential sensor for detecting the nitriding potential in the atmosphere furnace, and the temperature sensor for detecting the temperature in the atmosphere furnace An apparatus for manufacturing a metal spring having a control device is provided.

本発明に係る前記製造装置において、前記制御装置には、事前試験に基づき予め設定された制御モードが記憶される。
前記制御モードは、被処理体である金属製ばね本体が前記炉内に配置された状態で前記温度センサによって検出される炉内温度が事前試験に応じて予め設定された所定窒化処理温度まで上昇するように前記加熱手段を制御する昇温工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが事前試験に応じて予め設定された所定の高レベル値となるように前記アンモニアガス供給手段を制御する第１窒化工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが事前試験に応じて予め設定された所定の低レベル値まで低下するように、前記アンモニアガス供給手段を停止制御させて前記炉内へのアンモニアガスの供給を停止させ且つ前記水素ガス供給手段及び前記窒素ガス供給手段を供給制御させて前記炉内に水素ガス及び窒素ガスを３：１の割合で供給させる窒化ポテンシャル低下工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが前記低レベル値に保持されるように、前記アンモニアガス供給手段、前記水素ガス供給手段及び前記窒素ガス供給手段の作動制御を行う第２窒化工程とを含むものとされる。 In the manufacturing apparatus according to the present invention, a control mode set in advance based on a preliminary test is stored in the control device.
In the control mode, the furnace temperature detected by the temperature sensor rises to a predetermined nitriding temperature set in advance according to a preliminary test in a state where the metal spring body as the object to be processed is arranged in the furnace. Based on the nitriding potential sensor while controlling the heating means to control the heating means so that the temperature in the furnace detected by the temperature sensor is maintained at the predetermined nitriding treatment temperature. A first nitriding step for controlling the ammonia gas supply means so that a nitriding potential in the furnace becomes a predetermined high level value set in advance according to a preliminary test; and an in-furnace temperature detected by the temperature sensor While controlling the heating means to be maintained at the predetermined nitriding temperature, the nitriding potential in the furnace based on the nitriding potential sensor is preliminarily tested. The ammonia gas supply means is controlled to stop to stop the supply of ammonia gas into the furnace, and the hydrogen gas supply means and the nitrogen gas so as to decrease to a predetermined low level value set in advance according to A nitriding potential lowering step of supplying hydrogen gas and nitrogen gas into the furnace at a ratio of 3: 1 by supplying the supply means and maintaining the furnace temperature detected by the temperature sensor at the predetermined nitriding temperature. The ammonia gas supply means, the hydrogen gas supply means, and the nitrogen gas are controlled so that the nitriding potential in the furnace based on the nitriding potential sensor is maintained at the low level value while controlling the heating means. And a second nitriding step for controlling the operation of the supply means.

ここで、窒化ポテンシャルの前記高レベル値は、前記所定窒化処理温度での窒化処理を所定時間以上に亘って継続すると前記金属製ばね本体に化合物層の生成を招く濃度とされ、前記第１窒化工程の処理時間は化合物層の生成を招く前記所定時間より短く且つ前記所定時間の６０％以上の時間とされ、窒化ポテンシャルの前記低レベル値は、前記所定窒化処理温度での窒化処理を行っても前記金属製ばね本体に化合物層を生成させない濃度とされる。 Here, the high level value of the nitriding potential, is a concentration which leads to generation of said predetermined nitriding nitriding treatment at treatment temperatures to be continued for more than a predetermined time said metallic spring body to the compound layer, the first nitride processing time of step is 60% or more of the time tank and the predetermined time than the predetermined time lead to formation of the compound layer, the low-level value of the nitriding potential, performing nitriding treatment at the predetermined nitriding temperature However, the concentration is such that the metal spring body does not form a compound layer.

好ましくは、本発明に係る金属製ばねの製造装置は、さらに、前記雰囲気炉のガスの排出及び排出停止を切り換えるガス排出手段と、前記炉内の圧力を検出する圧力センサとを備え得る。
この場合、前記制御装置は、前記圧力センサの検出信号に基づき前記炉内の圧力が負圧とならないように前記ガス排出手段の作動制御を行うものとされる。 Preferably, the metal spring manufacturing apparatus according to the present invention may further include gas discharge means for switching between discharge and stop of the gas in the atmospheric furnace, and a pressure sensor for detecting the pressure in the furnace.
In this case, the control device controls the operation of the gas discharge means so that the pressure in the furnace does not become negative based on the detection signal of the pressure sensor.

本発明に係る金属製ばねの製造方法及び製造装置によれば、所定時間以上に亘って継続すると金属製ばね本体に化合物層の生成を招く高濃度の窒化ポテンシャルで窒化処理を行っているので深い窒化層を金属製ばね本体の表面全体に可及的に均一に形成することができ、さらに、高濃度の窒化ポテンシャルでの窒化処理を化合物層の生成を招く前記所定時間より短く且つ前記所定時間の６０％以上の時間に制限しているので金属製ばね本体に化合物層が生成することを確実に防止することができる。 According to the method and apparatus for manufacturing a metal spring according to the present invention, since the metal spring body is nitrided at a high concentration of nitriding potential which causes the formation of a compound layer if it is continued for a predetermined time or more The nitrided layer can be formed as uniformly as possible on the entire surface of the metal spring main body, and further, the nitriding process at a high concentration of nitriding potential is shorter than the predetermined time which causes the formation of the compound layer and the predetermined time since more than 60% of the time is restricted it is possible to reliably prevent the compound layer is produced on a metallic spring body.

図１は、本発明の一実施の形態に係る金属製ばね製造方法を実施する製造装置の一例の模式図である。FIG. 1 is a schematic view of an example of a manufacturing apparatus that performs a metal spring manufacturing method according to an embodiment of the present invention. 図２は、炉内ガスの水素濃度、アンモニア濃度及び窒素濃度と炉内の窒化ポテンシャルとの関係を示す表であり、水素濃度が０％〜３９％の場合の関係を示している。FIG. 2 is a table showing the relationship between the hydrogen concentration, ammonia concentration, and nitrogen concentration of the furnace gas and the nitriding potential in the furnace, and shows the relationship when the hydrogen concentration is 0% to 39%. 図３は、図２と同じ表であり、水素濃度が４０％〜７５％の場合の関係を示している。FIG. 3 is the same table as FIG. 2 and shows the relationship when the hydrogen concentration is 40% to 75%. 図４は、本発明の一実施の形態に係る金属製ばね製造方法における炉内雰囲気制御のタイムチャートである。FIG. 4 is a time chart of the furnace atmosphere control in the metal spring manufacturing method according to one embodiment of the present invention. 図５は、窒化生成相に及ぼす窒化ポテンシャルと窒化処理温度との関係を示すレーラー状態図の一例である。FIG. 5 is an example of a Railer state diagram showing the relationship between the nitriding potential and the nitriding temperature affecting the nitriding product phase.

以下、本発明に係る金属製ばねの製造方法の一実施の形態について、添付図面を参照しつつ説明する。   Hereinafter, an embodiment of a metal spring manufacturing method according to the present invention will be described with reference to the accompanying drawings.

まず、本実施の形態に係る金属製ばねの製造方法を実施する際に用いられる製造装置の一例１００について説明する。
図１に、前記製造装置１００の模式図を示す。 First, an example 100 of a manufacturing apparatus used when implementing the method for manufacturing a metal spring according to the present embodiment will be described.
A schematic view of the manufacturing apparatus 100 is shown in FIG.

図１に示すように、前記製造装置１００は、気密性雰囲気炉１０と、前記炉１０内を加熱するヒーター等の加熱手段２０と、前記炉１０へのアンモニアガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能なアンモニアガス供給手段３０と、前記炉１０への水素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な水素ガス供給手段４０と、前記炉１０への窒素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な窒素ガス供給手段５０と、前記炉１０内の窒化ポテンシャルＫｎを検出する窒化ポテンシャルセンサ６０と、前記炉１０内の温度を検出する温度センサ６１と、制御装置９０とを備えている。   As shown in FIG. 1, the manufacturing apparatus 100 switches between an airtight atmosphere furnace 10, heating means 20 such as a heater for heating the inside of the furnace 10, and supply and stop of supply of ammonia gas to the furnace 10. Further, the ammonia gas supply means 30 capable of adjusting the supply amount at the time of supply and the hydrogen gas supply means capable of switching supply and stop of supply of hydrogen gas to the furnace 10 and further capable of adjusting the supply amount at the time of supply. 40, the nitrogen gas supply means 50 capable of switching the supply and stop of the supply of nitrogen gas to the furnace 10, and adjusting the supply amount at the time of supply, and the nitriding potential for detecting the nitriding potential Kn in the furnace 10. The sensor 60, the temperature sensor 61 which detects the temperature in the said furnace 10, and the control apparatus 90 are provided.

図１に示すように、本実施の形態においては、前記アンモニアガス供給手段３０は、前記炉１０にアンモニアガスを供給するアンモニアガス供給ライン３１と、前記アンモニアガス供給ライン３１に介挿されたアンモニアガス制御手段３５とを有している。   As shown in FIG. 1, in the present embodiment, the ammonia gas supply means 30 includes an ammonia gas supply line 31 for supplying ammonia gas to the furnace 10, and ammonia interposed in the ammonia gas supply line 31. And gas control means 35.

本実施の形態においては、図１に示すように、前記アンモニアガス供給ライン３１は、大流量のアンモニアガスが供給される第１アンモニアガス供給ライン３１ａ及び小流量のアンモニアガスが供給される第２アンモニアガス供給ライン３１ｂを含んでおり、前記アンモニアガス制御手段３５は、前記第１及び第２アンモニアガス供給ライン３１ａ、３１ｂをそれぞれＯＮ／ＯＦＦする第１及び第２アンモニアガス電磁弁３５ａ、３５ｂを含んでいる。
当然ながら、前記アンモニアガス供給ライン３１が流量の異なる３本以上のアンモニアガス供給ラインを有するように構成することも可能である。 In the present embodiment, as shown in FIG. 1, the ammonia gas supply line 31 includes a first ammonia gas supply line 31a to which a large amount of ammonia gas is supplied and a second ammonia gas to which a small amount of ammonia gas is supplied. The ammonia gas control means 35 includes first and second ammonia gas solenoid valves 35a, 35b for turning ON / OFF the first and second ammonia gas supply lines 31a, 31b, respectively. Contains.
Naturally, the ammonia gas supply line 31 can be configured to have three or more ammonia gas supply lines having different flow rates.

また、前記アンモニアガス制御手段３５として、前記電磁弁３５ａ、３５ｂに代えて、弁開度を連続的に且つ自由に調整可能な電動弁（図示せず）を採用することも可能である。
この場合には、前記アンモニアガス供給手段３０は、大流量のアンモニアガスが供給される単一のアンモニアガス供給ラインと、前記アンモニアガス供給ラインに介挿されるアンモニアガス電動弁とを有するものとなる。 Further, as the ammonia gas control means 35, an electric valve (not shown) capable of continuously and freely adjusting the valve opening degree may be employed instead of the electromagnetic valves 35a and 35b.
In this case, the ammonia gas supply means 30 has a single ammonia gas supply line to which a large flow rate of ammonia gas is supplied, and an ammonia gas motor operated valve inserted in the ammonia gas supply line. .

図１に示すように、本実施の形態においては、前記水素ガス供給手段４０は、前記炉１０に水素ガスを供給する水素ガス供給ライン４１と、前記水素ガス供給ライン４１に介挿された電磁弁又は電動弁等の水素ガス制御手段４５とを有している。   As shown in FIG. 1, in the present embodiment, the hydrogen gas supply means 40 includes a hydrogen gas supply line 41 that supplies hydrogen gas to the furnace 10, and an electromagnetic that is interposed in the hydrogen gas supply line 41. And hydrogen gas control means 45 such as a valve or a motorized valve.

図１に示すように、本実施の形態においては、前記窒素ガス供給手段５０は、前記炉１０に窒素ガスを供給する窒素ガス供給ライン５１と、前記窒素ガス供給ライン５１に介挿された電磁弁又は電動弁等の窒素ガス制御手段５５とを有している。   As shown in FIG. 1, in the present embodiment, the nitrogen gas supply means 50 includes a nitrogen gas supply line 51 that supplies nitrogen gas to the furnace 10, and an electromagnetic that is interposed in the nitrogen gas supply line 51. And nitrogen gas control means 55 such as a valve or a motor operated valve.

前記制御装置９０は、前記各種センサ等から入力される信号に基づいて演算処理を実行する制御演算手段を含む演算部と、制御プログラム及び制御条件を記憶すると共に、前記演算部による演算中に生成されるデータを一時的に保持する記憶部とを備えている。   The control device 90 stores a calculation unit including a control calculation unit that executes calculation processing based on signals input from the various sensors and the like, a control program and control conditions, and is generated during calculation by the calculation unit. And a storage unit that temporarily holds the data to be stored.

本実施の形態においては、前記制御装置９０は、前記各種センサからの入力信号及び前記制御プログラムに基づき、前記アンモニアガス供給手段（前記アンモニアガス制御手段３５）、前記水素ガス供給手段（前記水素ガス制御手段４５）、前記窒素ガス供給手段（前記窒素ガス制御手段５５）及び前記加熱手段２０の作動制御を司る。   In the present embodiment, the control device 90 is configured such that the ammonia gas supply means (the ammonia gas control means 35), the hydrogen gas supply means (the hydrogen gas) based on input signals from the various sensors and the control program. It controls the operation of the control means 45), the nitrogen gas supply means (the nitrogen gas control means 55) and the heating means 20.

ここで、窒化ポテンシャルＫｎについて説明する。
窒化ポテンシャルＫｎとは、炉内雰囲気の窒化力を示す指標であって、次式によって表される。
Ｋｎ＝ＰＮＨ３／ＰＨ２ ３／２
（式中のＰＮＨ３ はアンモニア（ＮＨ３）の分圧、ＰＨ２は水素（Ｈ２）の分圧を示す） Here, the nitriding potential Kn will be described.
The nitriding potential Kn is an index indicating the nitriding power of the atmosphere in the furnace, and is expressed by the following equation.
Kn = P NH3 / P H2 3/2
( PNH 3 in the formula represents partial pressure of ammonia (NH 3 ), and PH 2 represents partial pressure of hydrogen (H 2 ))

この窒化ポテンシャルＫｎは水素濃度を検出することによって算出され得る。
即ち、炉内に供給されたアンモニアガス（ＮＨ３）は次式に基づいて、窒素（Ｎ２）と水素（Ｈ２）とに熱分解する。
ＮＨ３ → （１／２）Ｎ２ ＋ （３／２）Ｈ２ The nitriding potential Kn can be calculated by detecting the hydrogen concentration.
That is, the ammonia gas (NH 3 ) supplied into the furnace is thermally decomposed into nitrogen (N 2 ) and hydrogen (H 2 ) based on the following formula.
NH 3 → (1/2) N 2 + (3/2) H 2

ここで、アンモニアガスの単位量が炉内に導入された際の当該アンモニアガスの分解率をαとすれば、未分解アンモニア量は１−α、発生窒素量はα／２、発生水素量は３α／２となり、これらガスの総量は１＋αとなる。   Here, assuming that the decomposition rate of ammonia gas when a unit amount of ammonia gas is introduced into the furnace is α, the amount of undecomposed ammonia is 1−α, the amount of generated nitrogen is α / 2, and the amount of generated hydrogen is The total amount of these gases is 1 + α.

従って、アンモニア分圧ＰＮＨ３、窒素分圧ＰＮ２、水素分圧ＰＨ２は、次式によって表される。
ＰＮＨ３＝（１−α）／（１＋α） ・・・ （１）
ＰＮ２ ＝（α／２）／（１＋α） ・・・ （２）
ＰＨ２ ＝（３α／２）／（１＋α） ・・・ （３） Therefore, the ammonia partial pressure P NH3 , the nitrogen partial pressure P N2 , and the hydrogen partial pressure P H2 are represented by the following equations.
P NH3 = (1−α) / (1 + α) (1)
P N2 = (α / 2) / (1 + α) (2)
P H2 = (3α / 2) / (1 + α) (3)

前記式（１）〜（３）から、ＰＮＨ３及びＰＮ２は、それぞれ、
ＰＮＨ３＝（３−４ＰＨ２）／３
ＰＮ２ ＝ＰＨ２／３
となり、前述の窒化ポテンシャルＫｎは、
Ｋｎ＝ＰＮＨ３／ＰＨ２ ３／２
＝（３−４ＰＨ２）／３ＰＨ２ ３／２
＝（１−４ＰＨ２／３）／ＰＨ２ ３／２
となる。 From the above formulas (1) to (3), P NH3 and P N2 are respectively
P NH3 = (3-4P H2) / 3
P N2 = P H2 / 3
And the aforementioned nitriding potential Kn is
Kn = P NH3 / P H2 3/2
= (3-4P H2) / 3P H2 3/2
= (1-4P H2 / 3) / P H2 3/2
It becomes.

従って、前記雰囲気炉内の水素分圧ＰＨ２を検出すれば、炉内雰囲気の窒化ポテンシャルＫｎを求めることができる。 Therefore, by detecting the hydrogen partial pressure P H2 of the atmosphere furnace, it is possible to obtain the nitride potential Kn in the furnace atmosphere.

この点から、前記窒化ポテンシャルセンサ６０として、水素センサを好適に用いることができる。
前記水素センサとしては、例えば、水素分子透過性を備えた測定管によるもの（例えば、独Ｉｐｓｏｎ社製：ＨｙｄｒｏＮｉｔ−ｓｏｎｄｅ）を用いることができるが、炉体に直接装着することができ、炉内の水素濃度を連続的に測定できる点から、熱伝導式センサー（例えば、独Ｓｔａｎｇｅ社製：ＳＥ−Ｈ２）が好適に利用され得る。 From this point of view, a hydrogen sensor can be suitably used as the nitriding potential sensor 60.
As the hydrogen sensor, for example, one using a measuring tube having hydrogen molecule permeability (for example, HydroNit-sonde manufactured by Ipson of Germany) can be used, but it can be directly attached to the furnace body, and can be installed in the furnace. From the point that the hydrogen concentration of can be continuously measured, a heat conduction sensor (for example, manufactured by Stange, Germany: SE-H2) can be suitably used.

参考として、図２及び図３に、前記関係式に基づき得られる、窒化ポテンシャルＫｎと水素濃度、アンモニア濃度及び窒素濃度との関係を示す。
所望の窒化層を形成するために必要な窒化ポテンシャルＫｎが定まれば、前記関係式又は図２及び図３に示す表から、前記雰囲気炉内において制御目標値とすべき水素分圧ＰＨ２を求めることができる。 For reference, FIGS. 2 and 3 show the relationship between the nitriding potential Kn, the hydrogen concentration, the ammonia concentration, and the nitrogen concentration obtained based on the relational expression.
If the nitriding potential Kn necessary to form a desired nitrided layer is determined, the hydrogen partial pressure PH2 to be the control target value in the atmosphere furnace is determined from the above-mentioned relational expression or the table shown in FIG. 2 and FIG. Can be sought.

なお、本発明において、前記アンモニアガス供給ライン３１を介して前記炉１０内にアンモニアガスを供給する構成には、アンモニアガスだけを供給する態様に加えて、所謂、ガス軟窒化処理の態様も含まれる。前記ガス軟窒化処理には、アンモニアガスに炭酸ガスを加えたアンモニア・炭酸混合ガスを供給する態様や、アンモニアガスにアセチレンガスを加えたアンモニア・アセチレン混合ガスを供給する態様が含まれる。   In the present invention, the configuration in which ammonia gas is supplied into the furnace 10 through the ammonia gas supply line 31 includes a so-called gas soft nitriding treatment mode in addition to a mode in which only ammonia gas is supplied. Be The gas soft nitriding treatment includes an aspect of supplying an ammonia / carbonic acid mixed gas obtained by adding carbon dioxide gas to ammonia gas, and an aspect of supplying an ammonia / acetylene mixed gas obtained by adding acetylene gas to ammonia gas.

アンモニア・炭酸混合ガスを供給する態様においても、炭酸ガスの量はアンモニアガスに比して３〜５％程度であるため、前記炭酸ガスの存在を無視して、前記関係式（図２及び図３の関係表）を利用することができる。同様に、アンモニア・アセチレン混合ガスを供給する態様においても、前記関係式（図２及び図３の関係表）を利用することができる。   Even in the aspect of supplying the ammonia / carbonic acid mixed gas, the amount of carbonic acid gas is about 3 to 5% as compared with the ammonia gas. 3 relationship table) can be used. Similarly, in the aspect of supplying the ammonia / acetylene mixed gas, the relational expression (the relational tables in FIGS. 2 and 3) can be used.

好ましくは、図１に示すように、前記製造装置１００には、前記炉１０内のガスの排出及び排出停止を切り換えるガス排出手段７０と、前記炉１０内の圧力を検出する圧力センサ６２とが備えられる。   Preferably, as shown in FIG. 1, in the manufacturing apparatus 100, a gas discharge means 70 for switching between discharge and stop of gas discharge in the furnace 10 and a pressure sensor 62 for detecting the pressure in the furnace 10 are provided. Be equipped.

この場合、前記制御装置９０は、前記圧力センサ６２の検出信号に基づき前記炉１０内の圧力が負圧とならないように前記ガス排出手段７０の作動制御を行う。   In this case, the control device 90 controls the operation of the gas discharging means 70 based on the detection signal of the pressure sensor 62 so that the pressure in the furnace 10 does not become a negative pressure.

本実施の形態においては、図１に示すように、前記ガス排出手段７０は、前記炉１０内のガスを排出させる排出ライン７１と、前記排出ライン７１に介挿された排出電磁弁７５とを有しており、前記排出電磁弁７５が前記制御装置９０によって作動制御される。   In the present embodiment, as shown in FIG. 1, the gas discharge means 70 includes a discharge line 71 for discharging the gas in the furnace 10, and a discharge electromagnetic valve 75 interposed in the discharge line 71. The discharge solenoid valve 75 is operated and controlled by the controller 90.

本実施の形態においては、図１に示すように、前記製造装置１００は、さらに、前記排出ライン７１の下流端に接続された分解炉８０を有しており、前記炉１０内での窒化処理での残余のアンモニアが前記分解炉８０によって分解され、排出ガス中の可燃性ガス成分と共に燃焼炉８５で燃焼された上で、大気に放出される。   In the present embodiment, as shown in FIG. 1, the manufacturing apparatus 100 further includes a cracking furnace 80 connected to the downstream end of the discharge line 71, and nitriding treatment in the furnace 10 is performed. The remaining ammonia is decomposed by the cracking furnace 80, burned in the combustion furnace 85 together with the combustible gas component in the exhaust gas, and then released to the atmosphere.

ここで、本実施の形態に係る金属製ばね製造方法について説明する。
図４に、本実施の形態に係る金属製ばね製造方法における炉内雰囲気制御のタイムチャートを示す。 Here, the metal spring manufacturing method concerning this embodiment is explained.
FIG. 4 shows a time chart of furnace atmosphere control in the metal spring manufacturing method according to the present embodiment.

図１に示すように、本実施の形態に係る金属製ばね製造方法は、昇温工程と、第１窒化工程と、窒化ポテンシャル低下工程と、第２窒化工程とを含んでいる。   As shown in FIG. 1, the metal spring manufacturing method according to the present embodiment includes a temperature raising step, a first nitriding step, a nitriding potential lowering step, and a second nitriding step.

前記昇温工程は、小量のアンモニアガス及び窒素ガスを供給しつつ、炉内温度を所定の窒化処理温度（例えば４５０℃）まで上昇させるものであり、これにより、炉内及び被処理体である金属製ばね本体の酸化を防止する。
なお、後続する前記第１窒化工程、前記窒化ポテンシャル低下工程及び前記第２窒化工程では炉内温度は前記所定窒化処理温度に維持される。 In the temperature raising step, the furnace temperature is raised to a predetermined nitriding temperature (for example, 450 ° C.) while supplying small amounts of ammonia gas and nitrogen gas. Prevent oxidation of certain metal spring bodies.
In the subsequent first nitriding step, nitriding potential lowering step, and second nitriding step, the furnace temperature is maintained at the predetermined nitriding temperature.

前記第１窒化工程は、前記炉１０内の窒化ポテンシャルＫｎが前記金属製ばね本体の表面に化合物層の生成を招く高レベル値となるように、アンモニアガスを供給する。 Wherein the first nitriding step, as nitriding potential Kn in the furnace 10 becomes the high level value to cause the formation of a compound layer on the surface of the metallic spring body, for supplying ammonia gas.

ここで、所定窒化処理温度及び窒化ポテンシャルの高レベル値は、図５に示すレーラー状態図を利用して予め設定され、前記制御装置９０に制御条件として記憶される。   Here, the predetermined nitriding treatment temperature and the high level value of the nitriding potential are set in advance using the Lealer state diagram shown in FIG. 5 and stored in the control device 90 as control conditions.

即ち、図５に示すレーラー状態図は、窒化生成相に及ぼす窒化ポテンシャルＫｎと処理温度の関係を示しており、鋼部品にガス窒化処理（あるいは軟窒化処理）を施す際に、目的とする相組成の窒化層を形成するために必要な窒化ポテンシャルＫｎを求めるのに利用することができる。   That is, the Railer phase diagram shown in FIG. 5 shows the relationship between the nitriding potential Kn and the treatment temperature on the nitriding phase, and the target phase when the gas nitriding treatment (or soft nitriding treatment) is performed on the steel part. It can be used to determine the nitriding potential Kn necessary to form a nitride layer of composition.

なお、図５に示すレーラー状態図は、純鉄から成るワーク表面の窒化ポテンシャルＫｎと炉内雰囲気の窒化ポテンシャルＫｎとが一致する平衡状態をベースに作成されているので、現実の処理状況の非平衡状態、及び／又は、被処理体である金属製ばね本体の材質（鋼種）によっては、多少の誤差が生じることが考えられる。   Note that the Lealer phase diagram shown in FIG. 5 is created based on an equilibrium state in which the nitriding potential Kn of the work surface made of pure iron and the nitriding potential Kn of the atmosphere in the furnace coincide with each other. Depending on the material (steel grade) of the metal spring main body which is an equilibrium state and / or a to-be-processed object, it is considered that some errors occur.

したがって、現実の処理状態、金属製ばね本体の材質、及び／又は、軟窒化処理時における炭酸ガス又はアセチレンガスの添加量が比較的多い場合などには、必要に応じて、事前試験によって補正し、予め必要な窒化ポテンシャルＫｎ及び窒化処理温度を求めておくことが望ましい。   Therefore, if there is a relatively large amount of carbon dioxide gas or acetylene gas at the time of actual processing condition, material of metal spring body and / or soft nitriding, etc., correction is made by preliminary test if necessary. It is desirable to previously obtain the necessary nitriding potential Kn and the nitriding treatment temperature.

前記第１窒化工程の処理時間は、事前試験によって得られるデータに基づいて予め以下のように設定され、前記制御装置９０に制御条件として記憶される。
即ち、前記第１窒化工程における窒化条件、つまり、窒化ポテンシャルＫｎが前記高レベル値で且つ炉内温度が前記窒化処理温度とされた窒化条件での窒化処理において、前記金属製ばね本体の表面に化合物層が生じ始める所定時間を、予め、事前試験によって確認する。 The processing time of the first nitriding step is set in advance as follows based on data obtained by a preliminary test, and is stored in the control device 90 as a control condition.
That is, in the nitriding process in the first nitriding step, that is, in the nitriding process under the nitriding condition in which the nitriding potential Kn is the high level value and the furnace temperature is the nitriding process temperature, The predetermined time at which the compound layer starts to occur is confirmed in advance by a preliminary test.

その上で、前記第１窒化工程の処理時間を前記所定時間より短い時間に設定し、前記制御装置９０に記憶する。
好ましくは、前記第１窒化工程の処理時間は、前記所定時間の６０％以上、より好ましくは前記所定時間の８０％以上とされる。 Then, the processing time of the first nitriding step is set to a time shorter than the predetermined time, and stored in the control device 90.
Preferably, the processing time of the first nitriding step is 60% or more of the predetermined time, more preferably 80% or more of the predetermined time.

前記窒化ポテンシャル低下工程は、炉内温度を前記所定窒化処理温度に維持しつつ、前記炉１０内へのアンモニアガスの供給を停止し且つ前記炉１０内に水素ガス及び窒素ガスを３：１の割合で供給して、前記炉１０内の窒化ポテンシャルＫｎを前記金属製ばね本体に化合物層が生成しない低レベル値まで低下させる。   In the nitriding potential lowering step, the supply of the ammonia gas into the furnace 10 is stopped while maintaining the temperature in the furnace at the predetermined nitriding treatment temperature, and the hydrogen gas and the nitrogen gas in the furnace 10 are 3: 1. By supplying a proportion, the nitriding potential Kn in the furnace 10 is lowered to a low level value at which no compound layer is formed on the metal spring body.

詳しくは、前記窒化ポテンシャルＫｎの前記低レベル値は、前記レーラー状態図、及び／又は、事前試験に基づいて、予め設定され、前記制御装置９０に制御条件として記憶される。   Specifically, the low level value of the nitriding potential Kn is set in advance based on the Railer state diagram and / or a preliminary test, and is stored in the control device 90 as a control condition.

前記制御装置９０は、前記温度センサ６１に基づいて得られる炉内温度が前記所定窒化処理温度に維持されるように前記加熱手段２０を作動させつつ、前記窒化ポテンシャルセンサ６０からの信号に基づいて得られる前記炉１０内の窒化ポテンシャルＫｎが前記低レベル値まで低下するように前記水素ガス電磁弁４５及び前記窒素ガス電磁弁５５の作動制御を行う。   The controller 90 operates the heating means 20 so that the furnace temperature obtained based on the temperature sensor 61 is maintained at the predetermined nitriding temperature, and based on a signal from the nitriding potential sensor 60. The operation control of the hydrogen gas solenoid valve 45 and the nitrogen gas solenoid valve 55 is performed so that the nitriding potential Kn in the furnace 10 obtained is lowered to the low level value.

前記第２窒化工程は、炉内温度を前記所定窒化処理温度に保持し且つ前記炉１０内の窒化ポテンシャルＫｎを前記低レベル値に保持した状態を所定時間維持する。   In the second nitriding step, the furnace temperature is maintained at the predetermined nitriding temperature and the nitriding potential Kn in the furnace 10 is maintained at the low level for a predetermined time.

即ち、前記制御装置９０は、前記温度センサ６１に基づいて得られる炉内温度が前記所定窒化処理温度に維持されるように前記加熱手段２０を作動させつつ、前記窒化ポテンシャルセンサ６０からの信号に基づいて得られる前記炉１０内の窒化ポテンシャルＫｎが前記低レベル値に維持されるように前記アンモニアガス制御手段３５、前記水素ガス制御手段４５及び前記窒素ガス制御手段５５の作動制御を行う。   That is, while the control device 90 operates the heating unit 20 so that the temperature in the furnace obtained based on the temperature sensor 61 is maintained at the predetermined nitriding processing temperature, a signal from the nitriding potential sensor 60 is used. The operation control of the ammonia gas control means 35, the hydrogen gas control means 45 and the nitrogen gas control means 55 is performed so that the nitriding potential Kn in the furnace 10 obtained on the basis is maintained at the low level value.

なお、前記炉１０内の窒化ポテンシャルＫｎの前記低レベル値の維持は、前記アンモニアガス制御手段３５のＯＮ／ＯＦＦ制御によって行うこともできるし、アンモニアガスの供給による窒化ポテンシャルの上昇制御と窒素ガス及び水素ガスの供給（水素ガス及び窒素ガスの３：１の割合での供給）による窒化ポテンシャルの下降制御との組み合わせによって行うことも可能である。   The low level value of the nitriding potential Kn in the furnace 10 can be maintained by ON / OFF control of the ammonia gas control means 35, or the control of increasing the nitriding potential by supplying ammonia gas and the nitrogen gas. It is also possible to carry out by the combination with the lowering control of the nitriding potential by the supply of hydrogen gas (supply of hydrogen gas and nitrogen gas at a ratio of 3: 1).

前記第２窒化工程の処理時間も予め設定されており、前記制御装置９０は、制御条件として記憶されている処理時間に亘って前記第２窒化工程を実行する。   The processing time of the second nitriding step is also set in advance, and the control device 90 executes the second nitriding step over the processing time stored as the control condition.

かかる構成の金属製ばね製造方法によれば、以下の効果を得ることができる。
即ち、窒化処理前の金属製ばね本体の表面は、汚れ状態や酸化状態に関し均一とは言えない。
従って、このような状態の処理対象物（金属製ばね本体）に対して低濃度の窒化ポテンシャルで窒化処理を行うと、金属製ばね本体の表面に窒化のばらつきが生じ、結果として、金属製ばねの耐久性を十分には向上できない。 According to the metal spring manufacturing method of such a configuration, the following effects can be obtained.
That is, the surface of the metal spring main body before the nitriding treatment can not be said to be uniform with respect to the dirty state and the oxidized state.
Therefore, when nitriding treatment is carried out with a low concentration nitriding potential on the processing object (metal spring main body) in such a state, the surface of the metal spring main body becomes uneven in nitriding, and as a result, the metal spring Can not sufficiently improve the durability of the

これに対し、本実施の形態に係る前記製造方法によれば、金属製ばね本体に対する最初の窒化処理（前記第１窒化工程）は、前記金属製ばね本体の表面に化合物層の生成を招くような高レベル値の窒化ポテンシャルで行われている。   On the other hand, according to the manufacturing method according to the present embodiment, the first nitriding treatment (the first nitriding step) on the metal spring body causes the formation of a compound layer on the surface of the metal spring body. This is done with a high level of nitriding potential.

従って、窒化処理前の状態において金属製ばね本体の表面が汚れ状態や酸化状態に関し均一では無かったとしても、金属製ばね本体への窒化を可及的に均一且つ深く行うことができる。   Therefore, even if the surface of the metal spring main body is not uniform with respect to the dirty state and the oxidation state in the state before the nitriding treatment, the metal spring main body can be nitrided as uniformly and deeply as possible.

さらに、前記第１窒化工程においては、処理時間を制御することによって、処理対象物である金属製ばね本体の表面に化合物層が生成することを防止している。
従って、高レベル値の窒化ポテンシャルで窒化処理を行うことによって金属製ばね本体に深い窒化層を有効に形成しつつ、金属製ばね本体に化合物層が生成することを、簡単な制御で且つ確実に防止することができる。 Further, in the first nitriding step, the formation of the compound layer on the surface of the metal spring body that is the object to be processed is prevented by controlling the treatment time.
Therefore, while performing a nitriding process at a high level value of nitriding potential, a deep nitrided layer is effectively formed on the metal spring body, while the compound layer is formed on the metal spring body with simple control and reliably. Can be prevented.

即ち、理論上においては、窒化ポテンシャルＫｎの濃度の増減制御を繰り返し行うことによっても、金属製ばね本体の表面に深い窒化層を得ることが可能である。   That is, in theory, it is possible to obtain a deep nitrided layer on the surface of the metal spring body also by repeatedly controlling the concentration of the nitriding potential Kn.

しかしながら、窒化ポテンシャルＫｎの濃度の増減制御を応答性良く且つ正確に行うことは、現実的には非常に困難である。   However, it is actually very difficult to control the increase / decrease in the concentration of the nitriding potential Kn with good responsiveness.

これに対し、本実施の形態においては、前記第１窒化工程における窒化ポテンシャルＫｎ及び炉内温度は一定とされており、窒化処理処理時間を制御することによって、高濃度の窒化ポテンシャルで窒化処理を行いつつ化合物層の生成を防止している。
従って、高レベル値の窒化ポテンシャルで窒化処理を行うことによって深い窒化層を形成しつつ、化合物層の生成を簡単な制御で確実に防止することができる。 On the other hand, in the present embodiment, the nitriding potential Kn and the temperature in the furnace in the first nitriding step are constant, and the nitriding treatment is performed at a high concentration nitriding potential by controlling the nitriding treatment time. While preventing the formation of a compound layer.
Therefore, the formation of the compound layer can be surely prevented by simple control while forming a deep nitride layer by performing nitriding with a high level nitriding potential.

好ましくは、前記昇温工程においても、前記高レベル値を目標値として前記炉１０内に対するアンモニアガスの供給制御を行うことができる。
斯かる構成によれば、第１窒化工程の処理時間を可及的に短縮化させることができる。 Preferably, also in the temperature raising step, supply control of the ammonia gas to the inside of the furnace 10 can be performed with the high level value as a target value.
According to such a configuration, the processing time of the first nitriding step can be shortened as much as possible.

本実施の形態に係る製造方法は、図４に示すように、前記昇温工程の前に、アイドリング工程（待機工程）を有している。
アイドリング工程は、前記金属製ばね本体を炉内の雰囲気に慣らす為の処理である。 As shown in FIG. 4, the manufacturing method according to the present embodiment includes an idling process (standby process) before the temperature raising process.
The idling step is a process for adjusting the metal spring body to the atmosphere in the furnace.

前記金属製ばね製造方法は、好ましくは、前記昇温工程の前に、前記金属製ばね本体に対してショットブラストを行う前処理工程を含むことができる。
前記前処理工程を備えることにより、後続する前記第１及び第２窒化工程での窒化処理の安定化を図ることができる。 The metal spring manufacturing method may preferably include a pretreatment step of performing shot blasting on the metal spring main body before the temperature raising step.
By providing the pre-treatment step, stabilization of the nitriding treatment in the subsequent first and second nitriding steps can be achieved.

また、前記金属製ばね製造方法は、好ましくは、前記第２窒化工程の後に、前記金属製ばね本体に対してショットブラスト又はショットピーニングを行う後処理工程を含むことができる。
前記後処理工程を備えることにより、金属製ばねの耐久性を向上させることができる。 The metal spring manufacturing method may preferably include a post-processing step of performing shot blasting or shot peening on the metal spring body after the second nitriding step.
By including the post-treatment step, the durability of the metal spring can be improved.

１０ 気密性雰囲気炉
２０ 加熱手段
３０ アンモニアガス供給手段
４０ 水素ガス供給手段
５０ 窒素ガス供給手段
６０ 窒化ポテンシャルセンサ
６１ 温度センサ
６２ 圧力センサ
７０ ガス排出手段
９０ 制御装置
１００ 金属製ばね製造装置 DESCRIPTION OF SYMBOLS 10 Airtight atmosphere furnace 20 Heating means 30 Ammonia gas supply means 40 Hydrogen gas supply means 50 Nitrogen gas supply means 60 Nitriding potential sensor 61 Temperature sensor 62 Pressure sensor 70 Gas discharge means 90 Control apparatus 100 Metal spring manufacturing apparatus

Claims (7)

表面に窒化層が形成された金属製ばねの製造方法であって、
所定のばね形状に形成された金属製ばね本体を気密性雰囲気炉内に配置させた状態で炉内温度を所定窒化処理温度まで上昇させる昇温工程と、
炉内温度を前記所定窒化処理温度に保持しつつ、前記炉内の窒化ポテンシャルが所定の高レベル値となるようにアンモニアガスを供給する第１窒化工程と、
炉内温度を前記所定窒化処理温度に保持しつつ、前記炉内へのアンモニアガスの供給を停止し且つ前記炉内に水素ガス及び窒素ガスを３：１の割合で供給して、前記炉内の窒化ポテンシャルを前記金属製ばね本体に化合物層が生成しない低レベル値まで低下させる窒化ポテンシャル低下工程と、
炉内温度を前記所定窒化処理温度に保持し且つ前記炉内の窒化ポテンシャルを前記低レベル値に保持する第２窒化工程とを含み、
前記第１窒化工程における窒化ポテンシャルの前記高レベル値は、当該第１窒化工程を所定時間以上に亘って継続すると前記金属製ばね本体に化合物層の生成を招く濃度とされており、前記第１窒化工程の処理時間は化合物層の生成を招く前記所定時間より短く且つ前記所定時間の６０％以上の時間とされていることを特徴とする金属製ばねの製造方法。 A method of manufacturing a metal spring having a nitrided layer formed on its surface, comprising:
A temperature raising step for raising the furnace temperature to a predetermined nitriding temperature in a state where the metal spring body formed in a predetermined spring shape is arranged in an airtight atmosphere furnace,
A first nitriding step of supplying ammonia gas so that the nitriding potential in the furnace becomes a predetermined high level value while maintaining the furnace temperature at the predetermined nitriding temperature;
While maintaining the furnace temperature at the predetermined nitriding temperature, the supply of ammonia gas into the furnace is stopped and hydrogen gas and nitrogen gas are supplied into the furnace at a ratio of 3: 1, A nitriding potential lowering step of lowering the nitriding potential of the metal spring main body to a low level value at which no compound layer is formed in the metal spring body;
A second nitriding step of maintaining the furnace temperature at the predetermined nitriding temperature and maintaining the nitriding potential in the furnace at the low level value,
The high level value of the nitriding potential in the first nitriding step, the has a first nitriding process is concentration lead to formation of compound layer on the metal spring body to continue for more than a predetermined time, the first method for producing a metal spring, wherein the processing time of the nitriding step, which is 60% more time than the tank and the predetermined time than the predetermined time lead to formation of compound layer. 前記第１窒化工程の処理時間は、化合物層の生成を招く前記所定時間より短く且つ前記所定時間の８０％以上の時間とされていることを特徴とする請求項１に記載の金属製ばねの製造方法。 2. The metal spring according to claim 1, wherein a processing time of the first nitriding step is shorter than the predetermined time leading to generation of a compound layer and 80% or more of the predetermined time . Production method. 前記昇温工程は、前記炉内にアンモニアガスを供給しつつ行われることを特徴とする請求項１又は２に記載の金属製ばねの製造方法。   The method according to claim 1, wherein the temperature raising step is performed while supplying ammonia gas into the furnace. 前記昇温工程の前に、前記金属製ばね本体に対してショットブラストを行う前処理工程を含むことを特徴とする請求項１から３の何れかに記載の金属製ばねの製造方法。   The method for manufacturing a metal spring according to any one of claims 1 to 3, further comprising a pretreatment step of performing shot blasting on the metal spring main body before the temperature raising step. 前記第２窒化工程の後に、前記金属製ばね本体に対してショットブラスト又はショットピーニングを行う後処理工程を含むことを特徴とする請求項１から４の何れかに記載の金属製ばねの製造方法。   The method for manufacturing a metal spring according to any one of claims 1 to 4, further comprising a post-treatment step of performing shot blasting or shot peening on the metal spring body after the second nitriding step. . 気密性雰囲気炉と、前記雰囲気炉内を加熱する加熱手段と、前記雰囲気炉へのアンモニアガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能なアンモニアガス供給手段と、前記雰囲気炉への水素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な水素ガス供給手段と、前記雰囲気炉への窒素ガスの供給及び供給停止を切り換えることができ、さらに供給時には供給量を調整可能な窒素ガス供給手段と、前記雰囲気炉内の窒化ポテンシャルを検出する窒化ポテンシャルセンサと、前記雰囲気炉内の温度を検出する温度センサと、制御装置とを備え、
前記制御装置には、事前試験に基づき予め設定された制御モードが記憶されており、
前記制御モードは、被処理体である金属製ばね本体が前記炉内に配置された状態で前記温度センサによって検出される炉内温度が事前試験に応じて予め設定された所定窒化処理温度まで上昇するように前記加熱手段を制御する昇温工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが事前試験に応じて予め設定された所定の高レベル値となるように前記アンモニアガス供給手段を制御する第１窒化工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが事前試験に応じて予め設定された所定の低レベル値まで低下するように、前記アンモニアガス供給手段を停止制御させて前記炉内へのアンモニアガスの供給を停止させ且つ前記水素ガス供給手段及び前記窒素ガス供給手段を供給制御させて前記炉内に水素ガス及び窒素ガスを３：１の割合で供給させる窒化ポテンシャル低下工程と、前記温度センサによって検出される炉内温度が前記所定窒化処理温度に保持されるように前記加熱手段を制御しつつ、前記窒化ポテンシャルセンサに基づく前記炉内の窒化ポテンシャルが前記低レベル値に保持されるように、前記アンモニアガス供給手段、前記水素ガス供給手段及び前記窒素ガス供給手段の作動制御を行う第２窒化工程とを含み、
窒化ポテンシャルの前記高レベル値は、前記所定窒化処理温度での窒化処理を所定時間以上に亘って継続すると前記金属製ばね本体に化合物層の生成を招くものとされており、
前記第１窒化工程の処理時間は化合物層の生成を招く前記所定時間より短く且つ前記所定時間の６０％以上の時間とされ、
窒化ポテンシャルの前記低レベル値は、前記所定窒化処理温度での窒化処理を行っても前記金属製ばね本体に化合物層を生成させないものとされていることを特徴とする金属製ばねの製造装置。 An airtight atmosphere furnace, a heating means for heating the inside of the atmosphere furnace, an ammonia gas supply means capable of switching the supply and the supply stop of the ammonia gas to the atmosphere furnace, and capable of adjusting the supply amount at the time of supply; It is possible to switch the supply and stop of the supply of hydrogen gas to the atmosphere furnace, and switch the supply and stop of the supply of nitrogen gas to the atmosphere furnace and the hydrogen gas supply means capable of adjusting the supply amount at the time of supply. Furthermore, it comprises nitrogen gas supply means capable of adjusting the supply amount at the time of supply, a nitriding potential sensor for detecting the nitriding potential in the atmosphere furnace, a temperature sensor for detecting the temperature in the atmosphere furnace, and a control device.
The control device stores a control mode set in advance based on the pre-test,
In the control mode, the furnace temperature detected by the temperature sensor rises to a predetermined nitriding temperature set in advance according to a preliminary test in a state where the metal spring body as the object to be processed is arranged in the furnace. Based on the nitriding potential sensor while controlling the heating means so that the temperature inside the furnace detected by the temperature sensor is maintained at the predetermined nitriding temperature The first nitriding step of controlling the ammonia gas supply means so that the nitriding potential in the furnace becomes a predetermined high level value preset according to the preliminary test, and the temperature in the furnace detected by the temperature sensor While controlling the heating means to be maintained at the predetermined nitriding temperature, the nitriding potential in the furnace based on the nitriding potential sensor is preliminarily tested. The ammonia gas supply means is controlled to stop so as to decrease to a predetermined low level value set in advance according to the condition to stop the supply of ammonia gas into the furnace, and the hydrogen gas supply means and the nitrogen gas The nitriding potential lowering step of supplying the hydrogen gas and the nitrogen gas at a ratio of 3: 1 by controlling the supply means to supply the hydrogen gas and the nitrogen gas in the furnace, and the temperature in the furnace detected by the temperature sensor are maintained at the predetermined nitriding processing temperature The ammonia gas supply means, the hydrogen gas supply means, and the nitrogen gas so that the nitriding potential in the furnace based on the nitriding potential sensor is maintained at the low level value while controlling the heating means to And d) a second nitriding step for controlling the operation of the supply means,
The high level value of the nitriding potential is assumed to lead to formation of the compound layer to nitriding treatment at the predetermined nitriding temperature in said metal spring body to continue for more than a predetermined time,
The processing time of the first nitriding step is less than 60% of the time tank and the predetermined time than the predetermined time lead to formation of the compound layer,
The apparatus for manufacturing a metal spring, wherein the low level value of the nitriding potential is such that the metal spring body does not form a compound layer even if the nitriding process is performed at the predetermined nitriding treatment temperature. 前記雰囲気炉のガスの排出及び排出停止を切り換えるガス排出手段と、
前記炉内の圧力を検出する圧力センサとを備え、
前記制御装置は、前記圧力センサの検出信号に基づき前記炉内の圧力が負圧とならないように前記ガス排出手段の作動制御を行うことを特徴とする請求項６に記載の金属製ばねの製造装置。 Gas discharge means for switching between discharge and stop of gas in the atmosphere furnace;
A pressure sensor for detecting the pressure in the furnace;
The said control apparatus performs operation control of the said gas discharge means so that the pressure in the said furnace does not become negative pressure based on the detection signal of the said pressure sensor, The manufacture of the metal spring of Claim 6 characterized by the above-mentioned. apparatus.
JP2015024398A 2015-02-10 2015-02-10 Method and apparatus for manufacturing metal spring Active JP6552209B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2015024398A JP6552209B2 (en) 2015-02-10 2015-02-10 Method and apparatus for manufacturing metal spring
PCT/JP2016/051374 WO2016129333A1 (en) 2015-02-10 2016-01-19 Method and device for producing metal springs

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2015024398A JP6552209B2 (en) 2015-02-10 2015-02-10 Method and apparatus for manufacturing metal spring

Related Child Applications (1)

Application Number Title Priority Date Filing Date
JP2019091076A Division JP6812494B2 (en) 2019-05-14 2019-05-14 Metal spring manufacturing method and manufacturing equipment

Publications (2)

Publication Number Publication Date
JP2016148068A JP2016148068A (en) 2016-08-18
JP6552209B2 true JP6552209B2 (en) 2019-07-31

Family

ID=56614536

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2015024398A Active JP6552209B2 (en) 2015-02-10 2015-02-10 Method and apparatus for manufacturing metal spring

Country Status (2)

Country Link
JP (1) JP6552209B2 (en)
WO (1) WO2016129333A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019039049A (en) * 2017-08-28 2019-03-14 エア・ウォーターＮｖ株式会社 Spring excellent in fatigue resistance, and production method thereof
JP2019157163A (en) * 2018-03-08 2019-09-19 Ntn株式会社 Heat treatment method and heat treatment apparatus for workpiece
JP6503122B1 (en) 2018-08-17 2019-04-17 パーカー熱処理工業株式会社 Surface hardening treatment apparatus and surface hardening treatment method
JPWO2020090999A1 (en) * 2018-11-02 2021-12-02 パーカー熱処理工業株式会社 Nitride steel member and manufacturing method and manufacturing equipment for nitrided steel member
TW202124731A (en) * 2019-10-11 2021-07-01 日商帕卡熱處理工業股份有限公司 Surface hardening apparatus and surface hardening method

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006028588A (en) * 2004-07-16 2006-02-02 Toyota Motor Corp Nitriding treatment method
JP4711403B2 (en) * 2005-07-26 2011-06-29 本田技研工業株式会社 Steel spring member and manufacturing method thereof
JP5883727B2 (en) * 2012-06-01 2016-03-15 株式会社日本テクノ Gas nitriding and gas soft nitriding methods
JP5671588B2 (en) * 2013-08-27 2015-02-18 オリエンタルエンヂニアリング株式会社 Surface hardening processing apparatus and surface hardening processing method

Also Published As

Publication number Publication date
JP2016148068A (en) 2016-08-18
WO2016129333A1 (en) 2016-08-18

Similar Documents

Publication Publication Date Title
JP6552209B2 (en) Method and apparatus for manufacturing metal spring
JP5883727B2 (en) Gas nitriding and gas soft nitriding methods
JP3839615B2 (en) Vacuum carburizing method
JP2000178710A (en) Method of carburizing and carbonitriding treatment
JP6812494B2 (en) Metal spring manufacturing method and manufacturing equipment
JP6576209B2 (en) Nitriding processing apparatus and nitriding processing method
JP6543213B2 (en) Surface hardening method and surface hardening apparatus
JP5233258B2 (en) Method and apparatus for producing steel material having steel surface with controlled carbon concentration
JP2005179714A (en) Carburizing method
KR102255936B1 (en) Nitriding Treatment Method
KR102243284B1 (en) Nitriding Apparatus and Nitriding Treatment Method
US20140366993A1 (en) Method of carburizing
JP5683416B2 (en) Method for improving insulation resistance of vacuum heating furnace
JP2008260994A (en) Method for producing carburized product
EP3168314A1 (en) Method for heat treating metallic work pieces
JP2009299122A (en) Nitriding-quenching method, heater for nitriding-quenching and nitriding-quenching apparatus
JP6935326B2 (en) Gas carburizing method
JP6357042B2 (en) Gas soft nitriding method and gas soft nitriding apparatus
JP2000303160A (en) Carburizing treating method
JP6759842B2 (en) Steel manufacturing method
KR102495177B1 (en) Nitrocarburizing Treatment Method
JP2009270155A (en) Nitriding quenching method and nitrided quenched part
JP6724201B2 (en) Nitriding apparatus and nitriding method
JP2005350729A (en) Vacuum carburization method
JP2012126962A (en) Vacuum carburizing device, and temperature control method of carburizing gas

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20180202

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20190329

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20190514

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20190628

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20190702

R150 Certificate of patent or registration of utility model

Ref document number: 6552209

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250