JP2015025161A - Surface hardening method of iron or iron alloy and apparatus of the same, and surface hardening structure of iron or iron alloy - Google Patents

Surface hardening method of iron or iron alloy and apparatus of the same, and surface hardening structure of iron or iron alloy Download PDF

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JP2015025161A
JP2015025161A JP2013154704A JP2013154704A JP2015025161A JP 2015025161 A JP2015025161 A JP 2015025161A JP 2013154704 A JP2013154704 A JP 2013154704A JP 2013154704 A JP2013154704 A JP 2013154704A JP 2015025161 A JP2015025161 A JP 2015025161A
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均 椛澤
Hitoshi Kabasawa
均 椛澤
山本 博己
Hiromi Yamamoto
博己 山本
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Honda Motor Co Ltd
Nihon Techno KK
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Abstract

PROBLEM TO BE SOLVED: To provide a surface hardening method of iron or an iron alloy, which can provide a part from a cheap steel material such as carbon steel with a sufficient surface hardness and a small degree of thermal strain, and a small degree of dimensional change, a surface hardening apparatus of the iron or rion alloy, and a surface hardening structure of the iron or iron alloy obtained thereof.SOLUTION: A process of forming a two-layer structure of FeNand nitrogen martensite on an object to be treated includes the following steps: the object to be treated is transported to a heating room where ammonia gas is supplied; a temperature of the heating room is set to the temperature of a mixed phase region of austenite and iron nitride (FeN) in an iron-nitrogen phase equilibrium diagram so that the object to be treated is nitrided such that a surface nitrogen concentration of the object to be treated becomes a nitrogen concentration of FeN; and the object to be treated is rapidly cooled and heated again.

Description

本発明は、アンモニアガスで鉄または鉄合金の表面に窒素を供給して表面を硬化する表面硬化方法、当該方法に用いて好適な表面硬化装置、及び当該方法により得られる鉄または鉄合金の表面硬化構造に関するものである。   The present invention relates to a surface hardening method in which nitrogen is supplied to the surface of iron or iron alloy with ammonia gas to harden the surface, a surface hardening device suitable for use in the method, and the surface of iron or iron alloy obtained by the method It relates to a cured structure.

従来より、アンモニアガスにより鋼の表面を硬化する処理方法として、例えば、ガス窒化処理、ガス軟窒化処理及び浸窒焼入れ処理が知られている。   Conventionally, gas nitriding treatment, gas soft nitriding treatment, and nitriding quenching treatment are known as treatment methods for hardening the steel surface with ammonia gas.

ガス窒化処理は、合金鋼の表面にAl、Cr、V、Ti、Nb等の合金成分と窒素との硬い化合物(窒化物)を生成させることにより、強度、耐摩耗性、耐摩擦性、耐かじり性の向上を図る表面硬化処理であって、アンモニアガス単体、アンモニアガスと窒素ガスや水素ガス等の混合ガスを炉内に供給することによって処理がなされる。
このガス窒化処理は変態を伴わないので、熱処理ひずみや寸法変化が小さく、最終形状に仕上げられた部品に施されることが多い。この処理方法は、後述するガス軟窒化処理に比べ硬化層が深く硬度も高くなるが、高価な合金鋼が必要でしかも処理時間が長いという課題を有する。
In the gas nitriding treatment, a hard compound (nitride) of alloy components such as Al, Cr, V, Ti, and Nb and nitrogen is formed on the surface of the alloy steel, so that strength, wear resistance, friction resistance, This is a surface hardening treatment for improving galling, and is performed by supplying ammonia gas alone or a mixed gas such as ammonia gas and nitrogen gas or hydrogen gas into the furnace.
Since this gas nitriding treatment is not accompanied by transformation, the heat treatment strain and dimensional change are small, and the gas nitriding treatment is often applied to a part finished in a final shape. This processing method has a problem that the hardened layer is deeper and the hardness is higher than the gas soft nitriding process described later, but expensive alloy steel is required and the processing time is long.

ガス軟窒化処理は、炭素鋼などの表面に鉄と窒素の化合物(窒化物)を生成することによって、耐摩耗性、耐摩擦性、耐かじり性の向上を図る処理であって、アンモニアガスとRXガスの混合ガス、アンモニアガスと窒素ガス及び炭酸ガスの混合ガス等を炉内に供給することによって処理がなされる。
このガス軟窒化処理も変態を伴わないので、熱処理ひずみや寸法変化が小さく、最終形状に仕上げられた部品に施されることが多い。この処理方法は、上述したガス窒化処理に比べ処理時間が短く炭素鋼等の安価な材料の処理に適しているが、硬化層が浅く(10μm前後)硬度も低いという課題を有する。
The gas soft nitriding treatment is a treatment for improving wear resistance, friction resistance, and galling resistance by generating a compound of iron and nitrogen (nitride) on the surface of carbon steel or the like. Processing is performed by supplying a mixed gas of RX gas, a mixed gas of ammonia gas, nitrogen gas, and carbon dioxide gas into the furnace.
Since this gas nitrocarburizing treatment is not accompanied by transformation, it is often applied to parts finished in a final shape with little heat treatment strain and dimensional change. This processing method is suitable for processing an inexpensive material such as carbon steel, which has a shorter processing time than the gas nitriding process described above, but has a problem that the hardened layer is shallow (around 10 μm) and the hardness is low.

浸窒焼入れ処理は、Fe−N系状態図のオーステナイト領域で鋼に窒素を侵入・固溶し、その後焼入れして固い窒素マルテンサイトを生成することによって、強度、耐摩耗性、耐摩擦性、耐かじり性の向上を図る表面硬化処理であって、アンモニアガスと窒素ガスの混合ガスを炉内に供給することによって処理がなされる。
この浸窒焼入れ処理は、ガス浸炭処理と、上述したガス窒化処理やガス軟窒化処理との中間に位置する処理で、処理時間が短く炭素鋼等の安価な材料の処理に適しているが、ガス浸炭処理程の硬化深さは得られず、ガス窒化処理やガス軟窒化処理程の熱処理ひずみや寸法変化も得ることができない。
Nitrogen quenching treatment involves intrusion and solid solution of nitrogen in the steel in the austenite region of the Fe-N phase diagram, followed by quenching to produce hard nitrogen martensite, thereby increasing strength, wear resistance, friction resistance, This is a surface hardening treatment for improving galling resistance, and is performed by supplying a mixed gas of ammonia gas and nitrogen gas into the furnace.
This nitriding quenching process is a process located between the gas carburizing process and the above-described gas nitriding process or gas soft nitriding process, and is suitable for processing inexpensive materials such as carbon steel with a short processing time. The hardening depth as in the gas carburizing process cannot be obtained, and the heat treatment strain and dimensional change as in the gas nitriding process and the gas soft nitriding process cannot be obtained.

なお、先行技術として、例えば、特許文献1には、アンモニアガスで鋼表面に窒化物を生成する窒化処理であって、窒化効率を上げるために、処理温度を580〜700℃と通常の窒化処理よりも約100℃高くするようにした表面硬化処理が開示されている。
また、特許文献2には、アンモニアガスにより鋼のA変態点(約723℃)〜850℃の温度域で浸窒し、その後650℃〜A変態点(約723℃)の温度域まで徐冷し、一定時間保持後急冷(油冷)して表面に窒素マルテンサイトを生成する表面硬化処理が開示されている。
また、特許文献3には、アンモニアガスにより鋼を600〜800℃で浸窒し、表面に0.05−1.50%の窒素を固溶させ、その後急冷(油冷)して表面に硬い窒素マルテンサイトを生成する表面硬化処理が開示されている。
As a prior art, for example, Patent Document 1 discloses a nitriding treatment in which a nitride is formed on a steel surface with ammonia gas, and the treatment temperature is set to 580 to 700 ° C. in order to increase the nitriding efficiency. A surface hardening treatment in which the temperature is higher by about 100 ° C. is disclosed.
In Patent Document 2, the ammonia gas and nitriding at a temperature range of A 1 transformation point of steel (approximately 723 ° C.) to 850 ° C., to a temperature range of subsequent 650 ° C. to A 1 transformation point (about 723 ° C.) A surface hardening treatment is disclosed in which it is gradually cooled, held for a certain period of time, and then rapidly cooled (oil cooled) to generate nitrogen martensite on the surface.
Further, in Patent Document 3, steel is nitrogenated with ammonia gas at 600 to 800 ° C., 0.05 to 1.50% nitrogen is solid-dissolved on the surface, and then rapidly cooled (oil-cooled) to be hard on the surface. A surface hardening treatment for generating nitrogen martensite is disclosed.

特開2003−286561号公報JP 2003-286561 A 特公昭59−17167号公報Japanese Patent Publication No.59-17167 特開2007−46088号公報JP 2007-46088 A

しかしながら、上記先行技術を始めとする、従来のガス窒化処理、ガス軟窒化処理及び浸窒焼入れ処理においては、上述したように、それぞれ一長一短があり、何れの処理方法も、炭素鋼のような安価な鋼材から、十分に高い表面硬度を有し且つ熱処理ひずみや寸法変化が少ない部品(すなわち、硬度とひずみの両条件を同時に満足するような部品)を得ることは困難であった。   However, in the conventional gas nitriding treatment, gas soft nitriding treatment, and nitrocarburizing treatment including the above-described prior art, as described above, there are advantages and disadvantages, and each treatment method is inexpensive such as carbon steel. It was difficult to obtain a part having a sufficiently high surface hardness and little heat treatment strain or dimensional change (that is, a part satisfying both the hardness and strain conditions) from such a steel material.

本発明は、かかる事情に鑑みてなされたもので、炭素鋼のような安価な鋼材を使用しても、高合金鋼の窒化表面と同程度の表面硬度を得ることができ、かつ熱処理ひずみや寸法変化をガス窒化処理やガス軟窒化処理と同程度に抑えることができる鉄または鉄合金の表面硬化方法、当該方法に用いて好適な表面硬化装置、及び当該方法により得られる鉄または鉄合金の表面硬化構造を提供することを目的とする。   The present invention has been made in view of such circumstances, and even if an inexpensive steel material such as carbon steel is used, a surface hardness comparable to that of the nitrided surface of high alloy steel can be obtained, and heat treatment strain or Surface hardening method of iron or iron alloy capable of suppressing dimensional change to the same extent as gas nitriding treatment or gas soft nitriding treatment, surface hardening apparatus suitable for use in the method, and iron or iron alloy obtained by the method It aims at providing a surface hardening structure.

本発明者等は、上記課題を解決すべく鋭意検討を重ねた結果、被処理品を鉄−窒素系平衡状態図のオーステナイト(γ)と鉄窒化物(FeN:γ’)の混相域温度で浸窒した後、被処理品を急冷及び再加熱して、被処理品表面にFe16(α”)と窒素マルテンサイトの2層構造を生成することによって、上記目的が達成できることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above-mentioned problems, the present inventors have determined that the product to be processed is a mixed phase region of austenite (γ) and iron nitride (Fe 4 N: γ ′) in an iron-nitrogen equilibrium diagram. After nitriding at a temperature, the object can be achieved by rapidly cooling and reheating the object to be processed to form a two-layer structure of Fe 16 N 2 (α ″) and nitrogen martensite on the surface of the object to be processed. As a result, the present invention has been completed.

すなわち、本発明は上記知見に基づくものであって、請求項1に記載の本発明に係る表面硬化方法は、鉄または鉄合金にて構成される被処理品に窒素を侵入・拡散・固溶させた後、急冷及び再加熱により被処理品表面を硬化させる処理方法において、アンモニアガスが供給される加熱室内に被処理品を送入し、前記加熱室の温度を被処理品の鉄−窒素系平衡状態図のオーステナイト(γ)と鉄窒化物(FeN:γ’)の混相領域の所定温度に昇温して前記被処理品の表面窒素濃度がFe16(α”)の窒素濃度となるように浸窒した後、前記被処理品を急冷し再加熱することにより、被処理品表面にFe16(α”)と窒素マルテンサイトの2層構造を生成することを特徴とするものである。 That is, the present invention is based on the above knowledge, and the surface hardening method according to the present invention described in claim 1 is a method for infiltrating / diffusing / dissolving nitrogen into an article to be treated composed of iron or an iron alloy. In the processing method of curing the surface of the article to be treated by rapid cooling and reheating, the article to be treated is sent into a heating chamber to which ammonia gas is supplied, and the temperature of the heating chamber is set to iron-nitrogen of the article to be treated. In the system equilibrium diagram, the surface nitrogen concentration of the article to be treated is Fe 16 N 2 (α ″) by raising the temperature to a predetermined temperature in the mixed phase region of austenite (γ) and iron nitride (Fe 4 N: γ ′). After nitriding to a nitrogen concentration, the treated product is rapidly cooled and reheated to produce a two-layer structure of Fe 16 N 2 (α ″) and nitrogen martensite on the treated product surface. It is a feature.

請求項2に記載の発明は、請求項1に記載の鉄または鉄合金の表面硬化方法において、前記加熱室内を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度620℃〜650℃に保持して、浸窒することを特徴とするものである。 The invention according to claim 2 is the iron or iron alloy surface hardening method according to claim 1, wherein the heating chamber is a mixed phase region of austenite and iron nitride (Fe 4 N) in an iron-nitrogen equilibrium diagram. The temperature is maintained at 620 ° C. to 650 ° C., and nitriding is performed.

請求項3に記載の発明は、請求項1または2に記載の鉄または鉄合金の表面硬化方法において、前記加熱室内を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度620℃〜650℃に保持し、処理ガスとして、アンモニアガスと窒素ガスの混合ガス、アンモニアガスと水素ガスの混合ガス、またはアンモニアガスと窒素ガスと水素ガスの混合ガスを用いて、浸窒することを特徴とするものである。 The invention according to claim 3 is the surface hardening method of iron or iron alloy according to claim 1 or 2, wherein the heating chamber is made of austenite and iron nitride (Fe 4 N) in an iron-nitrogen equilibrium diagram. Using a mixed gas of ammonia gas and nitrogen gas, a mixed gas of ammonia gas and hydrogen gas, or a mixed gas of ammonia gas, nitrogen gas and hydrogen gas as a processing gas, the mixed phase temperature is maintained at 620 ° C to 650 ° C. It is characterized by nitriding.

請求項4に記載の発明は、請求項1〜3の何れか一項に記載の鉄または鉄合金の表面硬化方法において、前記被処理品の表面窒素濃度が2.95±0.35質量%となるように浸窒することを特徴とするものである。   Invention of Claim 4 is the surface hardening method of the iron or iron alloy as described in any one of Claims 1-3, The surface nitrogen concentration of the said to-be-processed product is 2.95 +/- 0.35 mass%. It is characterized by nitriding so that

請求項5に記載の発明は、請求項1〜4の何れか一項に記載の鉄または鉄合金の表面硬化方法において、前記被処理品を急冷した後、前記被処理品を250℃〜350℃で再加熱することを特徴とするものである。   According to a fifth aspect of the present invention, in the surface hardening method of iron or iron alloy according to any one of the first to fourth aspects, the article to be treated is cooled to 250 ° C. to 350 ° C. after the article to be treated is rapidly cooled. It is characterized by reheating at a temperature of 0 ° C.

請求項6に記載の発明は、請求項5に記載の鉄または鉄合金の表面硬化方法において、前記被処理品の再加熱を250℃〜350℃で60分〜120分施すことを特徴とするものである。   The invention according to claim 6 is the surface hardening method for iron or iron alloy according to claim 5, wherein the re-treatment of the article to be treated is performed at 250 ° C. to 350 ° C. for 60 minutes to 120 minutes. Is.

請求項7に記載の発明は、請求項1〜6の何れか一項に記載の鉄または鉄合金の表面硬化方法において、被処理品を浸窒するために、真空気密構造で、且つ、加熱室に攪拌機を備えたホットウォール型真空熱処理炉を使用するとともに、加熱室の雰囲気を真空排気及び窒素復圧により窒素ガス100%の状態とした後に、加熱室に処理ガスを導入するようにしたことを特徴とするものである。   The invention according to claim 7 is the method of surface hardening of iron or iron alloy according to any one of claims 1 to 6, wherein the object to be treated is vacuum-tight and heated for nitriding the article to be treated. A hot wall type vacuum heat treatment furnace equipped with a stirrer was used in the chamber, and after the atmosphere of the heating chamber was brought to 100% nitrogen gas by evacuation and nitrogen return pressure, the processing gas was introduced into the heating chamber. It is characterized by this.

請求項8に記載の発明は、請求項1〜7の何れか一項に記載の鉄または鉄合金の表面硬化方法に用いる表面硬化装置であって、被処理品を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度に保持して被処理品の表面窒素濃度がFe16の窒素濃度となるように浸窒するための手段と、浸窒した被処理品を急冷するための手段と、急冷した被処理品を再加熱するための手段とを備えることを特徴とするものである。 Invention of Claim 8 is a surface hardening apparatus used for the surface hardening method of the iron or iron alloy as described in any one of Claims 1-7, Comprising: A to-be-processed object is an iron-nitrogen system equilibrium state figure Means for maintaining the mixed phase temperature of austenite and iron nitride (Fe 4 N) of the steel and performing nitriding so that the surface nitrogen concentration of the article to be treated becomes the nitrogen concentration of Fe 16 N 2 , It is characterized by comprising means for rapidly cooling the processed product and means for reheating the rapidly cooled processed product.

請求項9に記載の発明は、鉄または鉄合金の表面硬化構造において、Fe16と窒素マルテンサイトの2層構造を表面にもつことを特徴とするものである。 The invention according to claim 9 is characterized in that the surface hardening structure of iron or iron alloy has a two-layer structure of Fe 16 N 2 and nitrogen martensite on the surface.

本発明によれば、炭素鋼のような安価な鋼材の表面に高合金鋼の窒化表面と同程度のFe16と窒素マルテンサイトの高硬度の2層構造を生成することができる。 According to the present invention, it is possible to generate a high-hardness two-layer structure of Fe 16 N 2 and nitrogen martensite on the surface of an inexpensive steel material such as carbon steel, which is comparable to the nitrided surface of high alloy steel.

また、本発明によれば、処理温度が620〜650℃と低く、処理時間も2時間以内と短くなるため、省資源、省エネルギー、低コストの処理が可能になる。   Further, according to the present invention, the processing temperature is as low as 620 to 650 ° C., and the processing time is shortened to within 2 hours, so that resource-saving, energy-saving, and low-cost processing becomes possible.

さらに、本発明によれば、鉄−窒素系平衡状態図の620〜650℃から被処理品を急冷するようにしたので、被処理品表面には高硬度のFe16と窒素マルテンサイトの2層構造が生成されるが、内部はフェライトのままなので焼きが入らず硬化しない。そのため、ガス窒化処理やガス軟窒化処理と同程度の極めて変形、変寸の少ない処理が可能である。 Furthermore, according to the present invention, since the article to be treated is rapidly cooled from 620 to 650 ° C. in the iron-nitrogen equilibrium diagram, the surface of the article to be treated is made of high-hardness Fe 16 N 2 and nitrogen martensite. A two-layer structure is produced, but since the inside remains ferrite, it does not burn and does not harden. For this reason, processing with very little deformation and change in size is possible, similar to gas nitriding or gas soft nitriding.

また、本発明によれば、被処理品の最表面が、マルテンサイトに比べて加熱に対する軟化抵抗性に優れたFe16の生成により硬化されることとなるため、被処理品を、高面圧、高荷重、高回転など、過酷な用途に適用することができる。 In addition, according to the present invention, the outermost surface of the article to be treated is cured by the production of Fe 16 N 2 which has superior softening resistance to heating compared to martensite. It can be applied to severe applications such as surface pressure, high load, and high rotation.

なお、前述した従来のガス窒化処理、ガス軟窒化処理及び浸窒焼入れ処理においては、雰囲気及び鋼表面の窒素濃度を精度よく、且つ、再現性よく制御することが難しいという問題点があり、そのため、従来のガス窒化処理及びガス軟窒化処理では、積極的に窒化物を生成させるために、窒素濃度を高目にして処理する必要があり、一方、従来の浸窒焼入れ処理では、窒化物を生成させずに窒素マルテンサイトを生成させるために、窒素濃度を低目にして処理する必要があった。その結果、従来のガス窒化処理及びガス軟窒化処理にあっては、高目の、浸窒焼入れ処理にあっては、低目のいずれも広い窒素濃度域で処理せざるを得なかった。
これに対して、本発明によれば、真空気密構造で、且つ、加熱室に攪拌機を備えたホットウォール型真空熱処理炉を用い、真空パージ(真空排気・窒素ガス復圧)により、加熱室を窒素ガス100%にしてから処理ガス(アンモニアガス及び窒素ガス)を導入することにより、従来のガス窒化処理、ガス軟窒化処理及び浸窒焼入れ処理では困難とされていた雰囲気及び鋼表面の窒素濃度の制御を、精度よく、且つ、再現性をよく行うことができる。
In the conventional gas nitriding treatment, gas soft nitriding treatment, and nitriding quenching treatment described above, there is a problem that it is difficult to control the atmosphere and the nitrogen concentration on the steel surface with good accuracy and reproducibility. In the conventional gas nitriding treatment and gas soft nitriding treatment, in order to positively generate nitride, it is necessary to treat the nitrogen concentration at a high level, while in the conventional nitriding quenching treatment, the nitride is not treated. In order to produce nitrogen martensite without producing it, it was necessary to treat with a low nitrogen concentration. As a result, in the conventional gas nitriding treatment and gas soft nitriding treatment, both the high and nitriding quenching treatments had to be treated in a wide nitrogen concentration range.
On the other hand, according to the present invention, a heating wall is formed by vacuum purging (vacuum exhaustion / nitrogen gas return pressure) using a hot wall type vacuum heat treatment furnace having a vacuum-tight structure and equipped with a stirrer in the heating chamber. By introducing treatment gas (ammonia gas and nitrogen gas) after making nitrogen gas 100%, the atmosphere and the nitrogen concentration on the steel surface, which were considered difficult in conventional gas nitriding treatment, gas soft nitriding treatment and nitriding quenching treatment This control can be performed with high accuracy and good reproducibility.

図1は、Fe−N系平衡状態図であり、縦軸が温度、横軸が窒素濃度をそれぞれ示している。FIG. 1 is an Fe—N system equilibrium diagram, in which the vertical axis represents temperature and the horizontal axis represents nitrogen concentration. 図2は、本発明の実施例に用いたホットウォール型真空熱処理炉の構造を示す概略図である。FIG. 2 is a schematic view showing the structure of the hot wall type vacuum heat treatment furnace used in the embodiment of the present invention. 図3は、本発明の実施例におけるヒートサイクルを示す図である。FIG. 3 is a diagram showing a heat cycle in the embodiment of the present invention. 図4は、本発明の表面硬化方法によって処理した試験片の断面金属組織を示す光学顕微鏡写真である。FIG. 4 is an optical micrograph showing a cross-sectional metallographic structure of a test piece treated by the surface hardening method of the present invention. 図5は、本発明の表面硬化方法によって処理した試験片の表面からの距離と硬度との関係を示す図である。FIG. 5 is a diagram showing the relationship between the distance from the surface of the test piece treated by the surface hardening method of the present invention and the hardness. 図6は、本発明の表面硬化方法によって処理した試験片の表面からの距離と窒素濃度との関係を示す図である。FIG. 6 is a diagram showing the relationship between the distance from the surface of the test piece treated by the surface hardening method of the present invention and the nitrogen concentration.

本発明の鉄または鉄合金の表面硬化方法においては、例えば、後述するホットウォール型真空熱処理炉を用いて加熱室の被処理品を、窒素雰囲気下または真空下で620〜650℃の温度域(図1に示す鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度)に加熱し、一定時間均熱後、加熱室内を真空排気・窒素ガス復圧する。 In the surface hardening method for iron or iron alloy of the present invention, for example, the article to be processed in the heating chamber is heated to a temperature range of 620 to 650 ° C. in a nitrogen atmosphere or under vacuum using a hot wall type vacuum heat treatment furnace described later. The mixture is heated to austenite and iron nitride (Fe 4 N) mixed phase temperature in the iron-nitrogen system equilibrium diagram shown in FIG.

ここで、被処理品を620〜650℃の温度域に加熱するのは、オーステナイト(γ)にFeN(γ’)が固溶した組織を得るためである。650℃以上ではオーステナイト(γ)にFe2〜3N(ε)が固溶した組織になり、620℃以下ではフェライト(α)にFeN(γ’)が固溶した組織になるので、浸窒後急冷・再加熱してもFe16(α’’)を析出させることはできない。 Here, the reason why the article to be treated is heated to a temperature range of 620 to 650 ° C. is to obtain a structure in which Fe 4 N (γ ′) is dissolved in austenite (γ). At 650 ° C. or higher, Fe 2-3 N (ε) is dissolved in austenite (γ), and at 620 ° C. or lower, Fe 4 N (γ ′) is dissolved in ferrite (α). Fe 16 N 2 (α ″) cannot be deposited even after rapid cooling and reheating after nitriding.

その後、加熱室に一定量の処理ガスを流して、被処理品(ワーク)表面がFe16の窒素濃度2.95質量%になるように浸窒する。その際に、加熱室のアンモニアガス濃度または水素ガス濃度を測定し、雰囲気を自動制御することが望ましいが、ホットウォール型真空熱処理炉の場合、処理条件さえ決まれば、アンモニアガスと窒素ガスの流量管理でも十分処理できる。
なお、被処理品表面の窒素濃度は、2.95質量%よりも高くなると次第に窒化物が生成し、2.95質量%よりも低くなると次第に窒素マルテンサイトが生成し、いずれも表面硬度が低くなるため、経済性を考慮し実操業では2.95±0.35質量%になるように雰囲気を制御する。被処理品表面の窒素濃度を2.60%〜3.30%にすることによって、被処理品の表面を実用上有効なHV950以上に硬化することができる。
具体的に、処理ガスとしては、例えば、アンモニアガスと窒素ガスの混合ガス、アンモニアガスと水素ガスの混合ガス、またはアンモニアガスと窒素ガスと水素ガスの混合ガスの何れかを用いることができる。
Thereafter, a certain amount of processing gas is allowed to flow into the heating chamber, and the surface of the object to be processed (workpiece) is subjected to nitrogen so that the nitrogen concentration of Fe 16 N 2 is 2.95% by mass. At that time, it is desirable to automatically control the atmosphere by measuring the ammonia gas concentration or hydrogen gas concentration in the heating chamber. However, in the case of a hot wall type vacuum heat treatment furnace, the flow rate of ammonia gas and nitrogen gas is only required if the processing conditions are determined. Even management can handle enough.
In addition, when the nitrogen concentration on the surface of the article to be processed is higher than 2.95% by mass, nitrides are gradually formed, and when it is lower than 2.95% by mass, nitrogen martensite is gradually formed, both of which have low surface hardness. Therefore, the atmosphere is controlled so as to be 2.95 ± 0.35 mass% in actual operation in consideration of economy. By setting the nitrogen concentration on the surface of the article to be treated to 2.60% to 3.30%, the surface of the article to be treated can be cured to a practically effective HV950 or higher.
Specifically, as the processing gas, for example, any of a mixed gas of ammonia gas and nitrogen gas, a mixed gas of ammonia gas and hydrogen gas, or a mixed gas of ammonia gas, nitrogen gas and hydrogen gas can be used.

その後、処理温度620〜650℃温度域、表面窒素濃度2.95±0.35%の条件で浸窒された被処理品を、冷却油槽にて速やかに急冷(油冷)した後、250〜350℃の温度域で60分〜120分間再加熱して、被処理品表面に硬いFe16と窒素マルテンサイトの2層構造を生成する。
ここで、被処理品を250〜350℃の温度域で再加熱するのは、250℃未満ではFe16が十分析出せず、350℃以上では、Fe16が[αFe+FeN(γ’)]に変化していずれも硬度が下がるからである。そのため再加熱の温度域は、被処理品表面に十分な硬度を付与できる250〜350℃にするのが望ましい。
Thereafter, the article to be treated, which has been subjected to nitriding under conditions of a treatment temperature of 620 to 650 ° C. and a surface nitrogen concentration of 2.95 ± 0.35%, is rapidly quenched (oil-cooled) in a cooling oil tank, and then 250 to Reheating in a temperature range of 350 ° C. for 60 to 120 minutes generates a two-layer structure of hard Fe 16 N 2 and nitrogen martensite on the surface of the object to be processed.
Here, when the article to be treated is reheated in a temperature range of 250 to 350 ° C., Fe 16 N 2 does not sufficiently precipitate at a temperature lower than 250 ° C., and Fe 16 N 2 becomes [αFe + Fe 4 N ( This is because the hardness is lowered in any case. Therefore, it is desirable that the reheating temperature range is 250 to 350 ° C., which can impart sufficient hardness to the surface of the article to be processed.

このような本発明の表面硬化方法には、例えば、ホットウォール型真空熱処理炉からなる表面硬化装置を好適に用いることができる。ホットウォール型真空熱処理炉は、被処理品を浸窒する加熱室と、被処理品を急冷(油冷)する真空パージ室兼油槽とを備える。
加熱室は、当該加熱室を真空にする真空排気手段と、加熱室の圧力を大気圧以上に保持する圧力制御手段と、加熱室を加熱する加熱手段と、加熱室を所定の温度に保持する温度制御手段と、加熱室を断熱する断熱手段と、加熱室の出入り口を断熱する断熱扉手段と、加熱室の雰囲気を攪拌する攪拌手段と、加熱室にアンモニアガスと窒素ガスを供給するガス供給手段と、加熱室雰囲気のアンモニアガス濃度を測定する測定手段または加熱室雰囲気の水素ガス濃度を測定する測定手段とを備えることができる。
一方、真空パージ室兼油槽(以下、前室と称する。)は、前室の出入口を密閉にするための密閉手段と、前室を真空排気するための真空排気手段と、前室の圧力を大気圧以上に保持する圧力制御手段と、被処理品を急冷(油冷)するための急冷手段と、前室油槽の油を加熱する加熱手段と、前室油槽の油を冷却する冷却手段と、前室油槽の油を攪拌する攪拌手段と、被処理品を炉内搬送する搬送手段とを備えることができる。
In such a surface curing method of the present invention, for example, a surface curing apparatus comprising a hot wall type vacuum heat treatment furnace can be suitably used. The hot wall type vacuum heat treatment furnace includes a heating chamber for nitriding the article to be treated, and a vacuum purge chamber / oil tank for rapidly cooling (oil cooling) the article to be treated.
The heating chamber is a vacuum evacuation unit that evacuates the heating chamber, a pressure control unit that holds the pressure of the heating chamber at atmospheric pressure or higher, a heating unit that heats the heating chamber, and holds the heating chamber at a predetermined temperature. Temperature control means, heat insulation means for insulating the heating chamber, heat insulating door means for insulating the entrance of the heating chamber, stirring means for stirring the atmosphere of the heating chamber, and gas supply for supplying ammonia gas and nitrogen gas to the heating chamber Means and measuring means for measuring the ammonia gas concentration in the heating chamber atmosphere or measuring means for measuring the hydrogen gas concentration in the heating chamber atmosphere.
On the other hand, the vacuum purge chamber / oil tank (hereinafter referred to as the front chamber) includes a sealing means for sealing the entrance / exit of the front chamber, a vacuum exhaust means for evacuating the front chamber, and a pressure in the front chamber. Pressure control means for maintaining the pressure above atmospheric pressure, rapid cooling means for rapidly cooling (oil cooling) the article to be treated, heating means for heating the oil in the front chamber oil tank, and cooling means for cooling the oil in the front chamber oil tank The agitation means for agitating the oil in the front chamber oil tank and the conveyance means for conveying the article to be processed in the furnace can be provided.

以下、本発明を実施例に基づいて具体的に説明するが、本発明は、このような実施例のみに限定されるものではない。   EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, this invention is not limited only to such an Example.

[ホットウォール型真空熱処理炉]
図2は、本発明の実施例に用いたホットウォール型真空熱処理炉1の構造を示すもので、このホットウォール型真空熱処理炉1は、炉本体となる加熱室2と、急冷用の油槽4を備えた前室3とから主に構成されており、前室3にはトレーに載置した被処理品を前室3と加熱室2の間で移動させるための炉内搬送装置5と、被処理品を油槽4中の冷却油に浸漬するための昇降装置(エレベータ)6とを備えている。さらに、前室3には、油槽4中の冷却油を加熱するためのパイプヒータ7と、冷却油を循環させるための油撹拌装置(アジタ)8が設けてあると共に、図外には冷却油を冷却するための水冷装置と、冷却油の温度を検出する熱電対などを備えている。
[Hot wall type vacuum heat treatment furnace]
FIG. 2 shows the structure of the hot wall type vacuum heat treatment furnace 1 used in the embodiment of the present invention. The hot wall type vacuum heat treatment furnace 1 includes a heating chamber 2 as a furnace body and an oil bath 4 for rapid cooling. An in-furnace transfer device 5 for moving an article to be processed placed on a tray between the front chamber 3 and the heating chamber 2; An elevating device (elevator) 6 for immersing the article to be processed in the cooling oil in the oil tank 4 is provided. Further, the front chamber 3 is provided with a pipe heater 7 for heating the cooling oil in the oil tank 4 and an oil agitator (agitator) 8 for circulating the cooling oil. A water-cooling device for cooling the water and a thermocouple for detecting the temperature of the cooling oil.

一方、加熱室2は、断熱材9によって内張された加熱室2の内部に加熱源としてのラジアントチューブヒータ10と、炉内温度を検出するための熱電対11と、炉内の雰囲気(窒素)を強制撹拌するための雰囲気攪拌装置12とを備えており、炉内の温度を均一にして被処理品の昇温を速やかなものとすることができるようになっている。また、加熱室2には、当該加熱室2の内部にアンモニアガス及び窒素ガスを供給する処理ガス供給手段が連結されていている。この処理ガス供給手段は、アンモニアガスを供給する第1供給管と、窒素ガスを供給する第2供給管と、それら供給管からのガスを受け入れて加熱室2に導く接続管と、それら管の各々に設けられたバルブとにより構成されている。   On the other hand, the heating chamber 2 includes a radiant tube heater 10 as a heating source in the heating chamber 2 lined with a heat insulating material 9, a thermocouple 11 for detecting the temperature in the furnace, and the atmosphere (nitrogen in the furnace). ) Is forcibly stirred, and the temperature inside the furnace can be made uniform by increasing the temperature in the furnace. The heating chamber 2 is connected to processing gas supply means for supplying ammonia gas and nitrogen gas into the heating chamber 2. The processing gas supply means includes a first supply pipe that supplies ammonia gas, a second supply pipe that supplies nitrogen gas, a connection pipe that receives gas from the supply pipe and leads it to the heating chamber 2, It is comprised by the valve | bulb provided in each.

さらに、加熱室2及び前室3は、図外にそれぞれ真空排気装置を備え、それぞれ独立して気圧制御ができるようになっていると共に、図示しないガス制御装置を介して図外の窒素源(窒素ボンベ)に連結されている。   Further, the heating chamber 2 and the front chamber 3 are each provided with an evacuation device outside the figure, and can control the atmospheric pressure independently, and a nitrogen source (not shown) via a gas control device (not shown). Nitrogen cylinder).

[実施例]
先ず、処理に先立ち、JIS G 3445に規程される機械構造炭素鋼鋼管STKM−13Cからなる試験片(20mm×20mm×5mm)を用意した。
そして、この試験片の表面に硬化層深さが30μm、表面硬さがマイクロビッカース硬さで930以上のFe16と窒素マルテンサイトの2層構造を生成することを目的として、600mm幅×900mm奥行×600mm高さの炉内有効寸法を有する上述した構造のホットウォール型真空熱処理炉により、図3に示すヒートサイクルの処理を施した。
[Example]
First, prior to the treatment, a test piece (20 mm × 20 mm × 5 mm) made of a mechanical structure carbon steel pipe STKM-13C regulated by JIS G 3445 was prepared.
Then, for the purpose of generating a two-layer structure of Fe 16 N 2 and nitrogen martensite having a hardened layer depth of 30 μm and a surface hardness of 930 or more on the surface of this test piece and having a micro Vickers hardness of 600 mm width × The heat cycle treatment shown in FIG. 3 was performed by a hot wall type vacuum heat treatment furnace having the above-described structure having an effective dimension in the furnace of 900 mm depth × 600 mm height.

図3に示すように、浸窒温度を640℃に設定し、処理ガス供給手段により窒素ガスの供給量とアンモニアガスの供給量を次のように調整した。
窒素ガス(N):1Nm/Hr
アンモニアガス(NH):0.48Nm/Hr(=8Nl/min)
ここで、窒素ガスとアンモニアガスの各流量は、事前の条件出しで決定した。すなわち、条件出しでは、窒素ガスの流量を1Nm/Hrで固定し、炉内の残留アンモニアガス濃度が1.4〜1.6%(例えば、1.5%)になるようにアンモニアガスの流量を調整し、最終的に0.48Nm/Hr(=8Nl/min)に決定した。
As shown in FIG. 3, the nitriding temperature was set to 640 ° C., and the supply amount of nitrogen gas and the supply amount of ammonia gas were adjusted as follows by the processing gas supply means.
Nitrogen gas (N 2 ): 1 Nm 3 / Hr
Ammonia gas (NH 3 ): 0.48 Nm 3 / Hr (= 8 Nl / min)
Here, the flow rates of nitrogen gas and ammonia gas were determined in advance. That is, in determining the conditions, the flow rate of nitrogen gas is fixed at 1 Nm 3 / Hr, and the ammonia gas concentration is adjusted so that the residual ammonia gas concentration in the furnace becomes 1.4 to 1.6% (for example, 1.5%). The flow rate was adjusted and finally determined to be 0.48 Nm 3 / Hr (= 8 Nl / min).

試験片の処理に際しては、先ず、ホットウォール型真空熱処理炉1の前室3の前室入口真空扉3aを開放し、試験片をトレーに載置した状態で前室3内に入れ、前室入口真空扉3aを閉じ、真空窒素パージ(真空排気・窒素復圧)を行った。すなわち、真空排気装置を作動させて前室3及び加熱室2内の空気をパージしたのち、図外のガス制御装置を介して窒素ガスを導入して大気圧に復圧し、前室3及び加熱室2内を窒素ガスに置換した。   When processing the test piece, first, the front chamber entrance vacuum door 3a of the front chamber 3 of the hot wall type vacuum heat treatment furnace 1 is opened, and the test piece is placed in the front chamber 3 with the tray placed thereon. The inlet vacuum door 3a was closed, and a vacuum nitrogen purge (vacuum exhaustion / nitrogen return pressure) was performed. That is, after operating the evacuation device to purge the air in the front chamber 3 and the heating chamber 2, nitrogen gas is introduced through a gas control device (not shown) to restore the atmospheric pressure, and the front chamber 3 and the heating chamber are heated. The inside of the chamber 2 was replaced with nitrogen gas.

次に、前室入口真空扉3aを閉じた状態で、前室3の前室出口真空扉3b及び加熱室2の断熱扉2aを開放すると共に、炉内搬送装置5を作動させて試験片をトレーと共に押し出し、加熱室2内に装入したのち、真空扉3b及び断熱扉2aを閉じ、加熱室2に窒素ガスを1Nm/Hr流しながら、加熱室2のラジアントチューブヒータ10に通電して昇温を開始した。なお、窒素ガスの供給は、真空窒素パージ工程を除き処理が終了するまで継続した。 Next, with the front chamber inlet vacuum door 3a closed, the front chamber outlet vacuum door 3b of the front chamber 3 and the heat insulating door 2a of the heating chamber 2 are opened, and the in-furnace transfer device 5 is operated to remove the test piece. After extruding with the tray and inserting into the heating chamber 2, the vacuum door 3 b and the heat insulating door 2 a are closed, and the radiant tube heater 10 in the heating chamber 2 is energized while flowing 1 Nm 3 / Hr of nitrogen gas into the heating chamber 2. Heating started. The supply of nitrogen gas was continued until the process was completed except for the vacuum nitrogen purge process.

その後、加熱室2を浸窒温度の640℃まで昇温させた後、この温度を30分間保持して、試験片の温度を640℃に均一化した。この30分間の均熱後、加熱室を30Paまで真空排気・窒素復圧して浸窒工程に備えた。   Then, after heating the heating chamber 2 to 640 degreeC of nitriding temperature, this temperature was hold | maintained for 30 minutes and the temperature of the test piece was equalized to 640 degreeC. After the soaking for 30 minutes, the heating chamber was evacuated to 30 Pa and the pressure was returned to nitrogen to prepare for the nitriding step.

真空排気・窒素復圧後、加熱室2に1Nm/Hrの窒素ガスと、0.48Nm/Hr(=8Nl/min)のアンモニアガスを供給し、試験片を浸窒した。アンモニアガスは、浸窒工程の90分間連続供給した。 Evacuation-nitrogen condensate depressurizing, a nitrogen gas 1 Nm 3 / Hr into the heating chamber 2, supplying ammonia gas 0.48Nm 3 / Hr (= 8Nl / min), and nitriding the specimen. Ammonia gas was continuously supplied for 90 minutes in the nitriding step.

なお、浸窒の雰囲気管理は、窒素ガスとアンモニアガスの流量による条件管理で行ったが、確認のため赤外線アンモニア分析計により炉内のアンモニアガス濃度を測定した。測定の結果、浸窒工程における加熱室2のアンモニアガス濃度は、アンモニアガス供給15分後に1.4%、30分後に1.45%、40分後に1.5%であった。   Nitrogen atmosphere was controlled by conditions based on the flow rates of nitrogen gas and ammonia gas. For confirmation, the ammonia gas concentration in the furnace was measured with an infrared ammonia analyzer. As a result of the measurement, the ammonia gas concentration in the heating chamber 2 in the nitriding step was 1.4% after 15 minutes of ammonia gas supply, 1.45% after 30 minutes, and 1.5% after 40 minutes.

浸窒工程終了後、真空扉3b及び断熱扉2aを開放して、試験片を炉内搬送装置5により加熱室2から前室3の昇降装置6上に搬出した後、昇降装置6の下降により65℃の油の中で急冷(油冷)した。   After completion of the nitriding step, the vacuum door 3b and the heat insulating door 2a are opened, and the test piece is carried out from the heating chamber 2 onto the lifting device 6 in the front chamber 3 by the in-furnace transport device 5, and then the lifting device 6 is lowered. It was quenched in oil at 65 ° C (oil cooling).

次いで、急冷した試験片を、600mm幅×900mm奥行×600mm高さの炉内有効寸法を有する流気式焼戻炉(図示省略)において280℃で90分間再加熱した。   Next, the rapidly cooled test piece was reheated at 280 ° C. for 90 minutes in an air-flow tempering furnace (not shown) having an effective dimension in the furnace of 600 mm width × 900 mm depth × 600 mm height.

このような処理が施された試験片を光学顕微鏡で撮影したところ、図4(b)に示すように、その表面に2つの層が形成されていることが確認された。そして、それぞれの層の組成を解析したところ、上側が主にFe16を含む層であり、下側が主にマルテンサイトを含む層であることが判明した。なお、浸窒後(再加熱を行う前)は図4(a)に示すように、その表面にはFe16と窒素マルテンサイトの2層構造は生成されていなかった。 When the test piece subjected to such treatment was photographed with an optical microscope, it was confirmed that two layers were formed on the surface thereof as shown in FIG. And when the composition of each layer was analyzed, it turned out that the upper side is a layer mainly containing Fe 16 N 2 and the lower side is a layer mainly containing martensite. In addition, after nitriding (before reheating), as shown in FIG. 4A, a two-layer structure of Fe 16 N 2 and nitrogen martensite was not generated on the surface.

また、マイクロビッカース硬度計で硬さ分布を測定したところ、図5に示すように、その表面硬さがマイクロビッカース硬さで930以上であることが確認された。また、試験片のひずみ量を測定したところ、±15μm以内であり、ガス窒化処理やガス軟窒化処理と同程度であることが確認された。
さらに、上記試験片について、表面からの断面の窒素濃度分布を測定したところ、図6に示すような結果が得られた。この図6によれば、窒素濃度分布は2段になっており、図4(b)の2層構造の組織に対応している。
Further, when the hardness distribution was measured with a micro Vickers hardness meter, as shown in FIG. 5, it was confirmed that the surface hardness was 930 or more in terms of micro Vickers hardness. Further, when the strain amount of the test piece was measured, it was within ± 15 μm, and it was confirmed that it was the same level as the gas nitriding treatment or gas soft nitriding treatment.
Furthermore, when the nitrogen concentration distribution of the cross section from the surface was measured about the said test piece, the result as shown in FIG. 6 was obtained. According to FIG. 6, the nitrogen concentration distribution has two stages, which corresponds to the two-layer structure of FIG.

各種条件で処理を行った結果を表1及び表2に示す。   The results of processing under various conditions are shown in Tables 1 and 2.

Figure 2015025161
Figure 2015025161

この表1は、浸窒温度を変化させたときの処理結果を示すもので、何れもアンモニア濃度を1.5%、再加熱温度を280℃、再加熱時間を90分としている。この表1に示すように、浸窒温度を640℃とした場合(試験No.4)に、被処理品表面に硬度1023(HV)のFe16と窒素マルテンサイトの2層構造を形成することができた。また、浸窒温度を620℃とした場合(試験No.3)には、試験No.4よりも硬度が落ちるが、822(HV)の表面硬度を得ることができた。 Table 1 shows the treatment results when the nitriding temperature is changed. In each case, the ammonia concentration is 1.5%, the reheating temperature is 280 ° C., and the reheating time is 90 minutes. As shown in Table 1, when the nitriding temperature is 640 ° C. (Test No. 4), a two-layer structure of Fe 16 N 2 having hardness 1023 (HV) and nitrogen martensite is formed on the surface of the object to be processed. We were able to. When the nitriding temperature was 620 ° C. (test No. 3), test no. Although the hardness was lower than 4, a surface hardness of 822 (HV) could be obtained.

Figure 2015025161
Figure 2015025161

この表2は、浸窒時間を変化させたときの処理結果を示すもので、何れもアンモニア濃度を1.5%、再加熱温度を280℃、再加熱時間を90分としている。この表2に示すように、浸窒時間を90分とした場合(試験No.3)に、被処理品表面に硬度1023(HV)のFe16と窒素マルテンサイトの2層構造を形成することができた。また、浸窒時間を70分とした場合(試験No.2)には、試験No.3よりも硬度が落ちるが、910(HV)の表面硬度を得ることができた。 Table 2 shows the treatment results when the nitriding time is changed. In each case, the ammonia concentration is 1.5%, the reheating temperature is 280 ° C., and the reheating time is 90 minutes. As shown in Table 2, when the nitriding time is 90 minutes (Test No. 3), a two-layer structure of Fe 16 N 2 having a hardness of 1023 (HV) and nitrogen martensite is formed on the surface of the object to be processed. We were able to. When the nitriding time was 70 minutes (Test No. 2), Test No. Although the hardness was lower than 3, a surface hardness of 910 (HV) could be obtained.

1 ホットウォール型真空熱処理炉
2 加熱室
2a 加熱室断熱扉
3 前室
3a 前室入口真空扉
3b 前室出口真空扉
4 油槽
5 搬送装置
6 昇降装置
7 パイプヒータ
8 油攪拌装置
9 断熱材
10 ラジアントチューブヒータ
11 熱電対
12 雰囲気攪拌装置
DESCRIPTION OF SYMBOLS 1 Hot wall type vacuum heat treatment furnace 2 Heating chamber 2a Heating chamber heat insulation door 3 Front chamber 3a Front chamber entrance vacuum door 3b Front chamber exit vacuum door 4 Oil tank 5 Conveyance device 6 Lifting device 7 Pipe heater 8 Oil stirring device 9 Heat insulation material 10 Radiant Tube heater 11 Thermocouple 12 Atmosphere stirrer

Claims (9)

鉄または鉄合金にて構成される被処理品に窒素を侵入・拡散・固溶させた後、急冷及び再加熱により被処理品表面を硬化させる処理方法であって、
アンモニアガスが供給される加熱室内に被処理品を送入し、前記加熱室の温度を被処理品の鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相領域の所定温度に昇温して前記被処理品の表面窒素濃度がFe16の窒素濃度となるように浸窒した後、前記被処理品を急冷し再加熱することにより、被処理品表面にFe16と窒素マルテンサイトの2層構造を生成することを特徴とする鉄または鉄合金の表面硬化方法。
A treatment method in which nitrogen is infiltrated, diffused, and solid-dissolved in an article to be treated composed of iron or iron alloy, and then the surface of the article to be treated is cured by rapid cooling and reheating,
An article to be treated is fed into a heating chamber to which ammonia gas is supplied, and the temperature of the heating chamber is set to a predetermined phase in the mixed phase region of austenite and iron nitride (Fe 4 N) in the iron-nitrogen equilibrium diagram of the article to be treated. After the temperature is raised to nitrogen and the surface nitrogen concentration of the article to be treated is equal to the nitrogen concentration of Fe 16 N 2 , the article to be treated is rapidly cooled and reheated, whereby Fe A surface hardening method for iron or an iron alloy, characterized in that a two-layer structure of 16 N 2 and nitrogen martensite is generated.
前記加熱室内を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度620℃〜650℃に保持して、浸窒することを特徴とする請求項1に記載の鉄または鉄合金の表面硬化方法。 2. The nitriding is performed while the heating chamber is maintained at a mixed phase temperature of 620 ° C. to 650 ° C. of austenite and iron nitride (Fe 4 N) in an iron-nitrogen equilibrium diagram. A method for surface hardening of iron or iron alloys. 前記加熱室内を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度620℃〜650℃に保持し、処理ガスとして、アンモニアガスと窒素ガスの混合ガス、アンモニアガスと水素ガスの混合ガス、またはアンモニアガスと窒素ガスと水素ガスの混合ガスを用いて、浸窒することを特徴とする請求項1または2に記載の鉄または鉄合金の表面硬化方法。 The heating chamber is maintained at a mixed phase temperature of 620 ° C. to 650 ° C. of austenite and iron nitride (Fe 4 N) in an iron-nitrogen equilibrium diagram, and a mixed gas of ammonia gas and nitrogen gas, ammonia gas as a processing gas The surface hardening method of iron or an iron alloy according to claim 1 or 2, wherein the nitriding is performed by using a mixed gas of hydrogen and hydrogen gas, or a mixed gas of ammonia gas, nitrogen gas and hydrogen gas. 前記被処理品の表面窒素濃度が2.95±0.35質量%となるように浸窒することを特徴とする1〜3の何れか一項に記載の鉄または鉄合金の表面硬化方法。   4. The surface hardening method for iron or iron alloy according to any one of claims 1 to 3, wherein the nitrogen treatment is performed so that the surface nitrogen concentration of the article to be treated is 2.95 ± 0.35 mass%. 前記被処理品を急冷した後、前記被処理品を250℃〜350℃で再加熱することを特徴とする1〜4の何れか一項に記載の鉄または鉄合金の表面硬化方法。   The method for surface hardening of iron or iron alloy according to any one of claims 1 to 4, wherein after the article to be treated is rapidly cooled, the article to be treated is reheated at 250 ° C to 350 ° C. 前記被処理品の再加熱を250℃〜350℃で60分〜120分施すことを特徴とする請求項5に記載の鉄または鉄合金の表面硬化方法。   6. The method for hardening a surface of iron or an iron alloy according to claim 5, wherein the article to be treated is reheated at 250 to 350 [deg.] C. for 60 to 120 minutes. 被処理品を浸窒するために、真空気密構造で、且つ、加熱室に攪拌機を備えたホットウォール型真空熱処理炉を使用するとともに、加熱室の雰囲気を真空排気及び窒素復圧により窒素ガス100%の状態とした後に、加熱室に処理ガスを導入するようにしたことを特徴とする請求項1〜6の何れか一項に記載の鉄または鉄合金の表面硬化方法。   In order to nitrify the object to be treated, a hot wall type vacuum heat treatment furnace having a vacuum-tight structure and equipped with a stirrer in the heating chamber is used. The method of hardening a surface of iron or an iron alloy according to any one of claims 1 to 6, wherein a processing gas is introduced into the heating chamber after being in the state of%. 請求項1〜7の何れか一項に記載の鉄または鉄合金の表面硬化方法に用いる表面硬化装置であって、
被処理品を鉄−窒素系平衡状態図のオーステナイトと鉄窒化物(FeN)の混相域温度に保持して被処理品の表面窒素濃度がFe16の窒素濃度となるように浸窒するための手段と、
浸窒した被処理品を急冷するための手段と、
急冷した被処理品を再加熱するための手段とを備えることを特徴とする鉄または鉄合金の表面硬化装置。
It is a surface hardening apparatus used for the surface hardening method of the iron or iron alloy as described in any one of Claims 1-7,
Immersion is performed so that the surface nitrogen concentration of the processed product becomes the nitrogen concentration of Fe 16 N 2 while maintaining the processed product at the mixed phase temperature of austenite and iron nitride (Fe 4 N) in the iron-nitrogen system equilibrium diagram. Means for nitriding,
Means for rapidly cooling the nitriding object,
A surface hardening apparatus for iron or an iron alloy, comprising: means for reheating a rapidly cooled workpiece.
Fe16と窒素マルテンサイトの2層構造を表面にもつことを特徴とする鉄または鉄合金の表面硬化構造。 A surface hardened structure of iron or an iron alloy having a two-layer structure of Fe 16 N 2 and nitrogen martensite on the surface.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106057392A (en) * 2016-06-26 2016-10-26 彭晓领 Low-temperature in-situ preparation method for [alpha]-Fe/[gamma]'-Fe4N soft magnetic composite material
JP2017197822A (en) * 2016-04-28 2017-11-02 株式会社日本テクノ Surface hardening method and surface hardening apparatus
CN110029303A (en) * 2019-05-21 2019-07-19 南京林业大学 A kind of Nitrizing Treatment device of automobile metal material
JP2019218576A (en) * 2018-06-15 2019-12-26 住友電気工業株式会社 Method for producing iron nitride material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07118702A (en) * 1993-10-21 1995-05-09 Mitsubishi Materials Corp Production of fe-n soft magnetic powder having high saturation magnetic flux density
JPH11269631A (en) * 1998-03-23 1999-10-05 Tokico Ltd Surface treating method for parts made of steel
JP2011241470A (en) * 2010-05-21 2011-12-01 Jfe Steel Corp Ferrous material and method of manufacturing the same
JP2013044036A (en) * 2011-08-25 2013-03-04 Jfe Steel Corp Method for producing ferrous material
JP2013108145A (en) * 2011-11-22 2013-06-06 Jtekt Corp Sliding member, clutch plate and methods for manufacturing the same
US20160130692A1 (en) * 2014-11-07 2016-05-12 Caterpillar Inc. Rapid Nitriding Through Nitriding Potential Control

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07118702A (en) * 1993-10-21 1995-05-09 Mitsubishi Materials Corp Production of fe-n soft magnetic powder having high saturation magnetic flux density
JPH11269631A (en) * 1998-03-23 1999-10-05 Tokico Ltd Surface treating method for parts made of steel
JP2011241470A (en) * 2010-05-21 2011-12-01 Jfe Steel Corp Ferrous material and method of manufacturing the same
JP2013044036A (en) * 2011-08-25 2013-03-04 Jfe Steel Corp Method for producing ferrous material
JP2013108145A (en) * 2011-11-22 2013-06-06 Jtekt Corp Sliding member, clutch plate and methods for manufacturing the same
US20160130692A1 (en) * 2014-11-07 2016-05-12 Caterpillar Inc. Rapid Nitriding Through Nitriding Potential Control

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017197822A (en) * 2016-04-28 2017-11-02 株式会社日本テクノ Surface hardening method and surface hardening apparatus
CN106057392A (en) * 2016-06-26 2016-10-26 彭晓领 Low-temperature in-situ preparation method for [alpha]-Fe/[gamma]'-Fe4N soft magnetic composite material
JP2019218576A (en) * 2018-06-15 2019-12-26 住友電気工業株式会社 Method for producing iron nitride material
JP7062529B2 (en) 2018-06-15 2022-05-06 住友電気工業株式会社 Manufacturing method of iron nitride material
CN110029303A (en) * 2019-05-21 2019-07-19 南京林业大学 A kind of Nitrizing Treatment device of automobile metal material

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