JPH11229113A - Oxide film removing method, gas nitro-carburizing method, and method for using organic chloride - Google Patents

Oxide film removing method, gas nitro-carburizing method, and method for using organic chloride

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Publication number
JPH11229113A
JPH11229113A JP4891498A JP4891498A JPH11229113A JP H11229113 A JPH11229113 A JP H11229113A JP 4891498 A JP4891498 A JP 4891498A JP 4891498 A JP4891498 A JP 4891498A JP H11229113 A JPH11229113 A JP H11229113A
Authority
JP
Japan
Prior art keywords
oxide film
gas
furnace
organic chloride
alloy steel
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.)
Granted
Application number
JP4891498A
Other languages
Japanese (ja)
Other versions
JP3643882B2 (en
Inventor
Masahiro Suzuki
雅浩 鈴木
Masashige Kiine
正成 木稲
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.)
Dowa Holdings Co Ltd
Original Assignee
Dowa Mining Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dowa Mining Co Ltd filed Critical Dowa Mining Co Ltd
Priority to JP04891498A priority Critical patent/JP3643882B2/en
Publication of JPH11229113A publication Critical patent/JPH11229113A/en
Application granted granted Critical
Publication of JP3643882B2 publication Critical patent/JP3643882B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To safely and easily realize the gas-nitrocarburizing treatment free from variance in a nitrided layer which unnecessitates handling harmful matters and low in labor in a short time by completely removing an oxide film on a surface of an alloy steel using an organic chloride. SOLUTION: An ammonium gas or a mixed gas of ammonium and nitrogen is introduced in a nitriding furnace which is a heat treatment furnace. In addition, an organic chloride such as vinylidene chloride or methylene chloride as an oxide film removing agent is poured therein by approximately 10-250 ml/m<3> , an alloy steel is charged in the furnace, and heated to approximately >=250 deg.C. A fine and adhesive oxide film containing chromium oxide on a surface of the alloy steel is completely removed by the effect of the organic chloride. Then, the furnace temperature is raised to approximately 500-600 deg.C. A nitrided layer free from variance is formed on the surface of the alloy steel without any oxide film to prevent penetration of the nitriding gas.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、合金鋼材の表面の
酸化皮膜を除去する方法、該方法を含むガス軟窒化処理
方法、および、有機系塩化物の使用方法に関する。
The present invention relates to a method for removing an oxide film on the surface of an alloy steel material, a gas nitrocarburizing method including the method, and a method for using an organic chloride.

【0002】[0002]

【従来の技術】合金鋼のうち、ステンレス鋼,耐熱鋼等
の、クロムやニッケルを多く含有するものにおいては、
その表面の、緻密で密着性のある酸化皮膜(酸化クロ
ム)が窒素ガスの浸透を妨げるため、一般に、ガス軟窒
化処理が困難である。
2. Description of the Related Art Among alloy steels, those containing a large amount of chromium and nickel, such as stainless steel and heat-resistant steel,
In general, a gas nitrocarburizing treatment is difficult because a dense and adherent oxide film (chromium oxide) on the surface prevents the penetration of nitrogen gas.

【0003】そこで、従来、塩酸やリン酸を用いて酸化
皮膜を除去し、その後でガス軟窒化処理を行うようにし
たり、ガス軟窒化処理に代えて、塩浴軟窒化処理を行っ
たりしていた。
Therefore, conventionally, an oxide film is removed by using hydrochloric acid or phosphoric acid, and then a gas nitrocarburizing treatment is performed, or a salt bath nitrocarburizing treatment is performed instead of the gas nitrocarburizing treatment. Was.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、塩酸や
リン酸を用いて酸化皮膜を除去する方法では、酸化皮膜
を完全には除去することができないので、ガス軟窒化処
理において窒化層にバラツキが生ずるという問題があっ
た。
However, in the method of removing an oxide film using hydrochloric acid or phosphoric acid, the oxide film cannot be completely removed, so that a variation occurs in the nitrided layer in the gas nitrocarburizing treatment. There was a problem.

【0005】また、塩浴軟窒化処理を実施するには、塩
の主剤として、有害物質であるシアン塩やシアン酸塩を
用いざるを得なかったので、これら有害物質の取り扱い
が難しいほか、その管理が煩雑であった。さらに、表面
に付着した有害物質を除去するため、塩浴処理後に、処
理済品の洗浄を行う手数がかかるほか、処理済品の表面
から流れ落ちる洗浄水には有害物質が混入してしまうの
で、それを除去しなければ排水できない、等の欠点があ
った。
Further, in order to carry out the salt bath nitrocarburizing treatment, a harmful substance such as cyanide or cyanate had to be used as a main component of the salt. Management was complicated. Furthermore, in order to remove harmful substances attached to the surface, it takes time and effort to wash the treated product after the salt bath treatment, and harmful substances are mixed in the washing water flowing down from the surface of the treated product, There are drawbacks such that the water cannot be drained unless it is removed.

【0006】本発明は、こうした事情に鑑みてなされた
もので、その第一の解決課題は、合金鋼材の表面の酸化
皮膜を完全に除去し得る、酸化皮膜の除去方法を提供す
ることである。
The present invention has been made in view of such circumstances, and a first problem to be solved is to provide a method of removing an oxide film which can completely remove an oxide film on the surface of an alloy steel material. .

【0007】第二の解決課題は、窒化層にバラツキを生
ずることのないガス軟窒化処理方法を提供することであ
る。
A second object of the present invention is to provide a gas nitrocarburizing method which does not cause a variation in a nitride layer.

【0008】第三の解決課題は、有害物質の取り扱いを
要せず、したがって、少ない手数で安全かつ簡単に窒化
処理済品を得ることができるガス軟窒化処理方法を提供
することである。
A third object of the present invention is to provide a gas nitrocarburizing method which does not require handling of harmful substances and can safely and easily obtain a nitrided product with a small number of steps.

【0009】第四の解決課題は、一般に長時間を要する
ガス軟窒化処理の時間短縮を達成し得る、ガス軟窒化処
理方法を提供することである。
A fourth object of the present invention is to provide a gas nitrocarburizing method capable of shortening the time required for a gas nitrocarburizing process which generally takes a long time.

【0010】第五の解決課題は、前記各課題を解決する
上で有効な、有機系塩化物の使用方法を提供することで
ある。
A fifth object of the present invention is to provide a method of using an organic chloride which is effective in solving the above-mentioned problems.

【0011】[0011]

【課題を解決するための手段】前記第一の課題を解決す
るため、本発明に係る酸化皮膜の除去方法は、合金鋼材
の表面の酸化皮膜を有機系塩化物を用いて除去するもの
である(請求項1)。
Means for Solving the Problems In order to solve the first problem, a method for removing an oxide film according to the present invention is to remove an oxide film on the surface of an alloy steel material using an organic chloride. (Claim 1).

【0012】前記第二ないし第四の課題を解決するた
め、本発明に係るガス軟窒化処理方法は、合金鋼材の酸
化皮膜除去剤として有機系塩化物を用いるものである
(請求項2)。具体的には、合金鋼材の表面の酸化皮膜
を有機系塩化物を用いて除去するとともにガス軟窒化処
理を行う(請求項3)。この場合、合金鋼材の表面の酸
化皮膜を有機系塩化物を用いて除去した後にガス軟窒化
処理を行うようにしてもよいし(請求項4)、また、熱
処理炉に合金鋼材と有機系塩化物とを一緒に入れてガス
軟窒化処理を行うようにしてもよい(請求項5)。
In order to solve the above-mentioned second to fourth problems, a gas nitrocarburizing method according to the present invention uses an organic chloride as an oxide film removing agent for an alloy steel material. Specifically, the oxide film on the surface of the alloy steel material is removed using an organic chloride and gas nitrocarburizing is performed (claim 3). In this case, the gas nitrocarburizing treatment may be performed after removing the oxide film on the surface of the alloy steel using an organic chloride (Claim 4), or the alloy steel and the organic chloride may be placed in a heat treatment furnace. The gas nitrocarburizing treatment may be performed by putting the material together.

【0013】より具体的には、例えば、窒化雰囲気中に
処理対象物を入れて加熱し、有機系塩化物を用いて前記
処理対象物の表面の酸化皮膜を除去し、その後さらに加
熱して軟窒化処理を行う(請求項6)。
More specifically, for example, the object to be treated is placed in a nitriding atmosphere and heated, an oxide film on the surface of the object to be treated is removed using an organic chloride, and then further heated to soften. A nitriding treatment is performed (claim 6).

【0014】前記第五の課題を解決するため、本発明に
係る有機系塩化物の使用方法は、有機系塩化物を合金鋼
材の酸化皮膜除去剤として用いるものである(請求項
7)。
In order to solve the fifth problem, the method of using an organic chloride according to the present invention uses an organic chloride as an oxide film remover for an alloy steel material.

【0015】[0015]

【発明の実施の形態】熱処理炉である窒化炉中に、アン
モニアガスまたはアンモニアと窒素の混合ガスを流入さ
せて、窒化雰囲気をつくる。この窒化雰囲気中に、処理
対象物である合金鋼材を入れて、250℃以上に加熱す
る。その後、有機系塩化物である塩化ビニリデンまたは
塩化メチレンを10ないし250ml/m 注入す
る。すると、注入された前記有機系塩化物の作用で、前
記合金鋼材の表面の酸化皮膜が除去される。続いて、5
00ないし600℃まで昇温させ、0.5ないし8時間
のガス軟窒化処理を行う。
DESCRIPTION OF THE PREFERRED EMBODIMENTS A nitriding atmosphere is created by flowing ammonia gas or a mixed gas of ammonia and nitrogen into a nitriding furnace which is a heat treatment furnace. An alloy steel material to be treated is put in the nitriding atmosphere and heated to 250 ° C. or higher. Thereafter, 10 to 250 ml / m 3 of vinylidene chloride or methylene chloride as an organic chloride is injected. Then, the oxide film on the surface of the alloy steel material is removed by the action of the injected organic chloride. Then, 5
The temperature is raised to 00 to 600 ° C., and a gas nitrocarburizing treatment is performed for 0.5 to 8 hours.

【0016】なお、前記有機系塩化物は、前記合金鋼材
と一緒に前記軟窒化雰囲気中に入れて(、酸化膜除去工
程に引き続きガス軟窒化を行って)もよい。
The organic chloride may be put in the nitrocarburizing atmosphere together with the alloy steel material (by performing gas nitrocarburization following the oxide film removing step).

【0017】[0017]

【実施例】第一実施例を説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS A first embodiment will be described.

【0018】窒化処理対象物として、耐熱鋼(SUH3
5)棒材を準備し、これを、窒化炉に入れた。該窒化炉
内の窒化雰囲気を、アンモニアガス50炉内%,窒素ガ
ス50炉内%とし、500℃まで加熱した。その後、前
記窒化炉内に、塩化ビニリデンを125ml/m
入した。そして、窒化炉内の温度を500℃に保持した
ままで、8時間ガス軟窒化処理を行い、前記耐熱鋼棒材
を前記窒化炉から取り出した。前記耐熱鋼棒材の表面に
は、35μmの均一な窒化層が形成されていた。
Heat-resistant steel (SUH3
5) A bar was prepared and placed in a nitriding furnace. The nitriding atmosphere in the nitriding furnace was set to 50% in an ammonia gas furnace and 50% in a nitrogen gas furnace, and heated to 500 ° C. Thereafter, 125 ml / m 3 of vinylidene chloride was injected into the nitriding furnace. Then, while keeping the temperature in the nitriding furnace at 500 ° C., a gas soft nitriding treatment was performed for 8 hours, and the heat-resistant steel bar was taken out of the nitriding furnace. A uniform nitrided layer of 35 μm was formed on the surface of the heat-resistant steel bar.

【0019】第二実施例を説明する。A second embodiment will be described.

【0020】窒化処理対象物として、ステンレス鋼(S
US304)材を準備し、これを、窒化炉に入れた。該
窒化炉内の窒化雰囲気を、アンモニアガス40炉内%,
窒素ガス60炉内%とし、570℃まで加熱した。その
後、前記窒化炉内に、塩化ビニリデンを250ml/m
注入した。そして、窒化炉内の温度を570℃に保
持したままで、1時間ガス軟窒化処理を行い、前記ステ
ンレス鋼材を前記窒化炉から取り出した。前記ステンレ
ス鋼材の表面には、40μmの均一な窒化層が形成され
ていた。
As an object to be nitrided, stainless steel (S
US304) A material was prepared and placed in a nitriding furnace. The nitriding atmosphere in the nitriding furnace was set to 40%
The furnace was heated to 570 ° C. with nitrogen gas at 60% in furnace. Thereafter, 250 ml / m of vinylidene chloride was introduced into the nitriding furnace.
Three injections were made. Then, while the temperature in the nitriding furnace was maintained at 570 ° C., a gas soft nitriding treatment was performed for one hour, and the stainless steel material was taken out of the nitriding furnace. A uniform nitride layer of 40 μm was formed on the surface of the stainless steel material.

【0021】第三実施例を説明する。A third embodiment will be described.

【0022】窒化処理対象物として、ステンレス鋼(S
US316)材を準備した。窒化炉内を、アンモニアガ
ス50炉内%,窒素ガス50炉内%の窒化雰囲気とし、
300℃に保持した。この状態の窒化炉内に、前記ステ
ンレス鋼材を塩化ビニリデン12.5ml/m とと
もに入れ、570℃まで昇温させた。そのまま2時間ガ
ス軟窒化処理を行い、前記ステンレス鋼材を前記窒化炉
から取り出した。前記ステンレス鋼材の表面には、45
μmの均一な窒化層が形成されていた。
As an object to be nitrided, stainless steel (S
US316) materials were prepared. The inside of the nitriding furnace is a nitriding atmosphere of 50% of furnace gas in ammonia gas and 50% of furnace gas in nitrogen gas.
It was kept at 300 ° C. The stainless steel material was put into the nitriding furnace in this state together with 12.5 ml / m 3 of vinylidene chloride, and the temperature was raised to 570 ° C. The gas soft nitriding treatment was performed for 2 hours, and the stainless steel material was taken out of the nitriding furnace. On the surface of the stainless steel material, 45
A uniform nitride layer of μm was formed.

【0023】第四実施例を説明する。A fourth embodiment will be described.

【0024】窒化処理対象物として、ステンレス鋼(S
US304)材を準備し、これを窒化炉に入れた。該窒
化炉内の窒化雰囲気を、アンモニアガス40炉内%,窒
素ガス60炉内%とし、570℃まで加熱した。その
後、前記窒化炉内に、塩化メチレンを90ml/m
注入した。そして、窒化炉内の温度を570℃に保持し
たままで、1時間ガス軟窒化処理を行い、前記ステンレ
ス鋼材を前記窒化炉から取り出した。前記ステンレス鋼
材の表面には、45μmの均一な窒化層が形成されてい
た。
As an object to be nitrided, stainless steel (S
US304) A material was prepared and placed in a nitriding furnace. The nitriding atmosphere in the nitriding furnace was set to 40% in an ammonia gas furnace and 60% in a nitrogen gas furnace, and heated to 570 ° C. Thereafter, 90 ml / m 3 of methylene chloride was introduced into the nitriding furnace.
Injected. Then, while the temperature in the nitriding furnace was maintained at 570 ° C., a gas soft nitriding treatment was performed for one hour, and the stainless steel material was taken out of the nitriding furnace. A uniform nitride layer of 45 μm was formed on the surface of the stainless steel material.

【0025】第五実施例を説明する。A fifth embodiment will be described.

【0026】窒化処理対象物として、耐熱鋼(SUH3
5)棒材を準備し、これを、窒化炉に入れた。該窒化炉
内の窒化雰囲気を、アンモニアガス50炉内%,窒素ガ
ス50炉内%とし、570℃まで加熱した。その後、前
記窒化炉内に、塩化メチレンを45ml/m 注入し
た。そして、窒化炉内の温度を570℃に保持したまま
で、1時間ガス軟窒化処理を行い、前記耐熱鋼棒材を前
記窒化炉から取り出した。前記耐熱鋼棒材の表面には、
40μmの均一な窒化層が形成されていた。
Heat-resistant steel (SUH3
5) A bar was prepared and placed in a nitriding furnace. The nitriding atmosphere in the nitriding furnace was set to 50% in an ammonia gas furnace and 50% in a nitrogen gas furnace, and heated to 570 ° C. Thereafter, 45 ml / m 3 of methylene chloride was injected into the nitriding furnace. Then, while keeping the temperature in the nitriding furnace at 570 ° C., gas nitrocarburizing treatment was performed for one hour, and the heat-resistant steel bar was taken out of the nitriding furnace. On the surface of the heat-resistant steel bar,
A uniform nitride layer of 40 μm was formed.

【0027】第六実施例を説明する。A sixth embodiment will be described.

【0028】窒化処理対象物として、工具鋼(SKD6
1)棒材を準備し、これを窒化炉に入れた。該窒化炉内
の窒化雰囲気を、アンモニアガス45炉内%,窒素ガス
55炉内%とし、570℃まで加熱した。その後、前記
窒化炉内に、塩化メチレンを90ml/m 注入し
た。そして、窒化炉内の温度を570℃に保持したまま
で、1時間ガス軟窒化処理を行い、前記工具鋼棒材を前
記窒化炉から取り出した。前記工具鋼棒材の表面には、
100μmの均一な窒化層が形成されていた。
As the nitriding object, tool steel (SKD6)
1) A bar was prepared and placed in a nitriding furnace. The nitriding atmosphere in the nitriding furnace was set to 45% in an ammonia gas furnace and 55% in a nitrogen gas furnace, and heated to 570 ° C. Thereafter, 90 ml / m 3 of methylene chloride was injected into the nitriding furnace. Then, while the temperature in the nitriding furnace was maintained at 570 ° C., gas soft nitriding was performed for 1 hour, and the tool steel bar was taken out of the nitriding furnace. On the surface of the tool steel bar,
A uniform nitride layer having a thickness of 100 μm was formed.

【0029】[0029]

【発明の効果】請求項1に記載の本発明によれば、有機
系塩化物の作用により、合金鋼材の表面の酸化皮膜を完
全に除去できる。
According to the present invention, the oxide film on the surface of the alloy steel material can be completely removed by the action of the organic chloride.

【0030】請求項2ないし6に記載の本発明によれ
ば、合金鋼材の表面に、均一な窒化層が得られる。ま
た、ガス軟窒化処理が困難との理由で従来採用されてい
た塩浴処理とは異なり、有害物質の取り扱いを要しない
ので、少ない手数で安全かつ簡単に窒化処理済品を得る
ことができる。さらに、一般に長時間を要するガス軟窒
化処理の時間が短縮される。
According to the present invention, a uniform nitrided layer can be obtained on the surface of the alloy steel material. Further, unlike the salt bath treatment which has been conventionally employed because gas nitrocarburizing treatment is difficult, it is not necessary to handle harmful substances, so that a nitrided product can be obtained safely and easily with a small number of steps. Furthermore, the time of the gas nitrocarburizing process, which generally takes a long time, is reduced.

Claims (7)

【特許請求の範囲】[Claims] 【請求項1】 合金鋼材の表面の酸化皮膜を有機系塩化
物を用いて除去することを特徴とする酸化皮膜の除去方
法。
1. A method for removing an oxide film, comprising removing an oxide film on the surface of an alloy steel material using an organic chloride.
【請求項2】 合金鋼材の酸化皮膜除去剤として有機系
塩化物を用いることを特徴とするガス軟窒化処理方法。
2. A gas nitrocarburizing method comprising using an organic chloride as an oxide film remover for an alloy steel material.
【請求項3】 合金鋼材の表面の酸化皮膜を有機系塩化
物を用いて除去するとともにガス軟窒化処理を行うこと
を特徴とする、ガス軟窒化処理方法。
3. A gas nitrocarburizing method comprising removing an oxide film on the surface of an alloy steel material using an organic chloride and performing a gas nitrocarburizing process.
【請求項4】 合金鋼材の表面の酸化皮膜を有機系塩化
物を用いて除去した後にガス軟窒化処理を行うことを特
徴とする、ガス軟窒化処理方法。
4. A gas nitrocarburizing method comprising removing an oxide film on the surface of an alloy steel material using an organic chloride and then performing a gas nitrocarburizing process.
【請求項5】 熱処理炉に合金鋼材と有機系塩化物とを
入れてガス軟窒化処理を行うことを特徴とする、ガス軟
窒化処理方法。
5. A gas nitrocarburizing method comprising the steps of: introducing an alloy steel material and an organic chloride into a heat treatment furnace and performing a gas nitrocarburizing process.
【請求項6】 窒化雰囲気中に処理対象物を入れて加熱
し、有機系塩化物を用いて前記処理対象物の表面の酸化
皮膜を除去し、その後さらに加熱して窒化処理を行うこ
とを特徴とする、ガス軟窒化処理方法。
6. An object to be treated is placed in a nitriding atmosphere and heated, an oxide film on the surface of the object to be treated is removed using an organic chloride, and thereafter, a nitriding treatment is performed by further heating. Gas nitrocarburizing treatment method.
【請求項7】 有機系塩化物を合金鋼材の酸化皮膜除去
剤として用いることを特徴とする、有機系塩化物の使用
方法。
7. A method for using an organic chloride, wherein the organic chloride is used as an oxide film remover for an alloy steel material.
JP04891498A 1998-02-13 1998-02-13 Removal method of oxide film, gas soft nitriding method, usage of organic chloride Expired - Fee Related JP3643882B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1176224A1 (en) * 2000-07-24 2002-01-30 Nissan Motor Co., Ltd. Nitrided maraging steel and method of manufacturing thereof
KR20030081993A (en) * 2002-04-15 2003-10-22 대한민국(전북대학교 총장) High pressure nitrocarburizing treatment method of cold press die for automobile parts

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1176224A1 (en) * 2000-07-24 2002-01-30 Nissan Motor Co., Ltd. Nitrided maraging steel and method of manufacturing thereof
US6733600B2 (en) 2000-07-24 2004-05-11 Nissan Motor Co., Ltd. Nitrided maraging steel and method of manufacture thereof
KR20030081993A (en) * 2002-04-15 2003-10-22 대한민국(전북대학교 총장) High pressure nitrocarburizing treatment method of cold press die for automobile parts

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