JPH02111900A - Production of stainless steel spring material - Google Patents
Production of stainless steel spring materialInfo
- Publication number
- JPH02111900A JPH02111900A JP26293588A JP26293588A JPH02111900A JP H02111900 A JPH02111900 A JP H02111900A JP 26293588 A JP26293588 A JP 26293588A JP 26293588 A JP26293588 A JP 26293588A JP H02111900 A JPH02111900 A JP H02111900A
- Authority
- JP
- Japan
- Prior art keywords
- stainless steel
- steel
- oxide film
- spring
- heat treatment
- 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
Links
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 24
- 239000010935 stainless steel Substances 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 230000005611 electricity Effects 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 9
- 239000010959 steel Substances 0.000 abstract description 9
- 239000002932 luster Substances 0.000 abstract 2
- 238000007743 anodising Methods 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 15
- 230000000694 effects Effects 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 5
- 229910000679 solder Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005097 cold rolling Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Landscapes
- Heat Treatment Of Steel (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高いぼね特性の必要な電子機器、精密機械等
多方面の分野に用いられるステンレスばね材の製造方法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing stainless steel spring materials used in various fields such as electronic equipment and precision machinery that require high spring characteristics.
近年、キーボードスイッチばね、ジンバルばね、ドーム
ばね等各種分野に使用されるばね材は、ミクロ化、極薄
化の発展に伴い、部品として高いぼね特性が要求される
とともに、表面光沢や耐錆性も要求されている。このた
めばね特性の優れたステンレスばね材の需要が増大して
いる。In recent years, spring materials used in various fields such as keyboard switch springs, gimbal springs, and dome springs have become micronized and ultra-thin, requiring high spring characteristics as parts, as well as surface gloss and rust resistance. Sex is also required. For this reason, demand for stainless steel spring materials with excellent spring properties is increasing.
従来よりステンレス鋼のばね特性の向上には強度増大の
観点から、鋼の成分を改良する方法(例えば特開昭6O
−89553)や最終冷間圧延の圧下率を高くとる方法
(例えば特開昭63−125614)が用いられている
。しかし、前者の方法では鋼の強度以外の性質も著しく
変化し、特に加工性や表面性状が劣化する傾向があり、
また後者の方法では伸びが著しく低下し加工性を損なう
。そこでばね特性を効果的に向上させる方法として冷間
圧延後に降伏点以下の引張力を与えながら熱処理する方
法(特公昭46−26219)が現在広く用いられてい
る。Conventionally, the spring characteristics of stainless steel have been improved by improving the composition of the steel from the perspective of increasing strength (for example, Japanese Patent Application Laid-open No. 6
-89553) and a method of increasing the reduction ratio in the final cold rolling (for example, Japanese Patent Application Laid-Open No. 63-125614). However, with the former method, properties other than the steel's strength change significantly, and in particular, workability and surface texture tend to deteriorate.
Furthermore, the latter method significantly reduces elongation and impairs workability. Therefore, as a method for effectively improving the spring properties, a method of heat-treating after cold rolling while applying a tensile force below the yield point (Japanese Patent Publication No. 46-26219) is currently widely used.
[発明が解決しようとする課題〕
しかしこの方法で製造されたステンレスばね材は、熱処
理により表面の光沢、はんだ性、耐錆性が著しく劣化す
ると言う問題があった。ステンレス鋼のはんだ性を改善
する手法として、光輝焼鈍したステンレス鋼帯を硝酸電
解することにより酸化皮膜を除去する方法(特開昭55
〜141596)が知られている。しかし、ばね性向上
のための光輝熱処理を行ったステンレス鋼に対しては、
この電解処理条件でははんだ性、耐錆性を改善するには
到らず充分な方法とは言えない。[Problems to be Solved by the Invention] However, the stainless steel spring material manufactured by this method has a problem in that the surface gloss, solderability, and rust resistance are significantly deteriorated by heat treatment. As a method to improve the solderability of stainless steel, a method is proposed in which the oxide film is removed by electrolyzing brightly annealed stainless steel strip with nitric acid (Japanese Patent Laid-Open No. 55
~141596) are known. However, for stainless steel that has undergone bright heat treatment to improve spring properties,
These electrolytic treatment conditions cannot be said to be a sufficient method as they do not improve solderability or rust resistance.
本発明は、ばね特性、表面光沢に優れかつはんだ性、耐
錆性の良好なステンレスばね材の製造方法の提供を目的
とする。An object of the present invention is to provide a method for manufacturing a stainless steel spring material that has excellent spring properties and surface gloss, as well as good solderability and rust resistance.
〔課題を解決するための手段及び作用〕本発明は、冷間
圧延したステンレス鋼帯に0.2%耐力以下の張力を付
与しつつ、露点−35℃以下の非酸化性雰囲気ガス中に
於いて350〜700℃で熱処理を施した後に、硝酸、
燐酸の1種あるいは2種を含みその総濃度が7.0〜3
0.0wt%となる水溶液中で、0.05〜5.OA/
dイの電流密度の範囲で全電解電気量が10〜500C
/dn−rの陽極電解処理を行うことを特徴とする。[Means and effects for solving the problems] The present invention provides a cold-rolled stainless steel strip with a tension of 0.2% proof stress or less while placing it in a non-oxidizing atmospheric gas with a dew point of -35°C or less. After heat treatment at 350-700℃, nitric acid,
Contains one or two types of phosphoric acid and has a total concentration of 7.0 to 3
In an aqueous solution of 0.0 wt%, 0.05 to 5. OA/
The total amount of electrolytic electricity is 10 to 500 C within the current density range of d
It is characterized by performing anodic electrolysis treatment of /dn-r.
以下に本発明方法の詳細を説明する。The details of the method of the present invention will be explained below.
まず、冷間圧延したステンレス鋼帯に0.2%耐力以下
の張力を付加しつつ350℃〜700 ℃で熱処理する
ことにより、ばね限界値が向上する。First, the spring limit value is improved by heat-treating a cold-rolled stainless steel strip at 350°C to 700°C while applying a tension of 0.2% proof stress or less.
熱処理温度が350℃未満の場合は、ばね限界値の向上
効果が得られず、また7 00 ℃を越えると鋼中に炭
化クロムが析出して耐錆性が劣化すると同時に鋼の強度
も軟化し始めるためばね性が低下する。熱処理は露点−
35℃以下の非酸化性雰囲気ガス中で行う。これは露点
が一35°Cよりも高いと酸化度膜厚が増大し変色及び
光沢の劣化が生じる上、下記に述べる電解処理で酸化皮
膜の除去が充分に行われないためである。If the heat treatment temperature is less than 350°C, the effect of improving the spring limit value will not be obtained, and if it exceeds 700°C, chromium carbide will precipitate in the steel, which will deteriorate the rust resistance and at the same time weaken the strength of the steel. The springiness decreases due to the start of the process. Heat treatment is dew point -
It is carried out in a non-oxidizing atmosphere gas at 35°C or lower. This is because when the dew point is higher than 135°C, the oxidation degree film thickness increases, causing discoloration and deterioration of gloss, and the oxide film is not removed sufficiently by the electrolytic treatment described below.
次に、ステンレス鋼を電解処理することにより、熱処理
で生じた酸化度Jiffを除去すると同時に薄い均一な
酸化皮膜を形成させる必要がある。このための電解液と
して非還元性水溶液である硝酸、燐酸の1種あるいは2
種を含む水溶液を用いる。同様の効果が期待されるもの
としてクロム酸、過塩素酸、過酸化水素等の水溶液があ
るが、価格及び取り扱い性の面より硝酸あるいは燐酸の
水溶液が最も好ましい。酸の濃度については7.0wt
%未満では酸としての効果が小さく、酸化皮膜の電解除
去が不充分となり、30.0wt%を越える高濃度では
硝酸の場合は酸化性が強過ぎるため酸化皮膜の電解除去
が充分に行われなくなり、また燐酸の場合は電解の効果
が飽和してしまう。このような水溶液中でステンレス鋼
を陽極として電解処理を行う。電流密度は0.05A/
dn?未満の場合、必要な電解除去を行う為の時間が長
くなり、生産性が悪く、また5 A / d rdを超
えると酸化皮膜の均一な溶解が行われず表面光沢を劣化
させる上ばね特性の劣化も起こるため不適当である。全
電解電気量は単位面積当たりIOC/dn(未満では酸
化皮膜の充分な溶解が行われずはんだ性の改善に到らな
い。また5 00 C/ d rdを超える電解ではは
んだ性、耐錆性の改善効果が飽和するのみならず、溶解
量が大きすぎるために表面光沢を劣化させることになる
。従って全電解電気量は10〜500C/drrrの範
囲とした。また電解液温度は低いと電解除去反応が低下
するため、15℃以上が好ましい。Next, by electrolytically treating the stainless steel, it is necessary to remove the oxidation degree Jiff generated by the heat treatment and at the same time form a thin and uniform oxide film. The electrolyte for this purpose is one or two types of non-reducing aqueous solutions such as nitric acid and phosphoric acid.
An aqueous solution containing seeds is used. Although aqueous solutions of chromic acid, perchloric acid, hydrogen peroxide, etc. are expected to have similar effects, aqueous solutions of nitric acid or phosphoric acid are most preferred from the viewpoint of cost and ease of handling. Regarding acid concentration: 7.0wt
If the concentration is less than 30.0 wt%, the effect as an acid will be small and the electrolytic removal of the oxide film will not be sufficient, and if the concentration exceeds 30.0 wt%, the oxidizing property of nitric acid will be too strong and the electrolytic removal of the oxide film will not be sufficient. In addition, in the case of phosphoric acid, the electrolytic effect becomes saturated. Electrolytic treatment is performed in such an aqueous solution using stainless steel as an anode. Current density is 0.05A/
dn? If it is less than 5 A/d rd, it will take a long time to carry out the necessary electrolytic removal, resulting in poor productivity, and if it exceeds 5 A/d rd, the oxide film will not be uniformly dissolved, leading to deterioration of the surface gloss and deterioration of the spring characteristics. This is inappropriate because it also occurs. If the total electrolysis amount is less than IOC/dn per unit area, the oxide film will not be sufficiently dissolved and solderability will not be improved.If the amount of electricity exceeds 500 C/dn, the solderability and rust resistance will deteriorate. Not only will the improvement effect be saturated, but the surface gloss will deteriorate because the amount of dissolution is too large. Therefore, the total amount of electrolytic electricity was set in the range of 10 to 500 C/drrr. Also, if the electrolytic solution temperature is low, electrolytic removal will occur. The temperature is preferably 15° C. or higher because the reaction decreases.
本発明法における熱処理は、前記特開昭5514159
6における光輝焼鈍条件に比べてはるかに低い温度で行
われるので、雰囲気中にH2が存在してもステンレス網
の酸化皮膜が還元され難い。従って、熱処理後に公知の
電解処理を行ったのでは、はんだ性および耐錆性を向上
させることが困難である。本発明法における電解条件に
よれば、はんだ性も耐錆性も容易に向上させることがで
き、しかも表面光沢を劣化させることがない。The heat treatment in the method of the present invention is carried out in
Since the bright annealing is performed at a much lower temperature than the bright annealing conditions in No. 6, the oxide film on the stainless steel mesh is hardly reduced even if H2 is present in the atmosphere. Therefore, if known electrolytic treatment is performed after heat treatment, it is difficult to improve solderability and rust resistance. According to the electrolytic conditions in the method of the present invention, both solderability and rust resistance can be easily improved without deteriorating the surface gloss.
尚、熱処理後のステンレス鋼のはんだ性、耐錆性を改善
する方法としては、硝ぶつ酸、塩酸、硫酸等の還元性の
酸による酸洗や機械的研削も同様の効果を示すが、表面
性状の劣化によって商品的イメージを損なうため、本発
明において対象外とした。Pickling with reducing acids such as nitric acid, hydrochloric acid, and sulfuric acid and mechanical grinding have similar effects as methods for improving the solderability and rust resistance of stainless steel after heat treatment, but It is excluded from the scope of the present invention because it damages the product image due to deterioration of properties.
以上のような本発明法を用いれば、ばね特性、表面光沢
に優れかつはんだ性、耐錆性の良好な電子機器用ステン
レスばね材を得ることができる。By using the method of the present invention as described above, it is possible to obtain a stainless steel spring material for electronic devices that has excellent spring properties and surface gloss, as well as good solderability and rust resistance.
供試材としては5US304,5US430を使用し、
第1表に示す圧下率で最終冷間圧延を行った後、各々の
条件において熱処理及び陽極電解処理を行った。特性の
評価として、ばね特性はばね限界値(JIS H313
0)を用い、はんだ性ははんだと供試材間の表面張力に
よるはんだ濡れ性をレスカ製5AT2000ソルダーチ
エッカ−を用いて評価し、濡れ性の良い順にA、B、C
の三段階で示した。ただし、A、B、Cの基準は次の通
りである。5US304 and 5US430 were used as test materials.
After final cold rolling was performed at the rolling reduction ratio shown in Table 1, heat treatment and anodic electrolytic treatment were performed under each condition. As an evaluation of the characteristics, the spring characteristics are determined based on the spring limit value (JIS H313
0), and the solderability was evaluated by evaluating the solder wettability due to the surface tension between the solder and the test material using Resca's 5AT2000 solder checker, and ranked A, B, and C in descending order of wettability.
It was shown in three stages. However, the criteria for A, B, and C are as follows.
A:はんだが良く付く
B:はんだ付けは可能だが、Aより劣るC:はんだ付け
が不可能
尚、フラックスは塩化亜鉛系を使用した。A: Solder adheres well B: Soldering is possible, but inferior to A. C: Soldering is not possible. Zinc chloride-based flux was used.
さらに耐錆性は塩水噴霧試験をJIS Z 2371に
準じて行いその結果を目視により評価した。表面光沢は
JIS Z 8741の鏡面光沢度測定方法に準じて測
定を行った。Furthermore, the rust resistance was evaluated by performing a salt spray test according to JIS Z 2371 and visually observing the results. Surface gloss was measured according to JIS Z 8741 specular gloss measurement method.
第1表に示す如く本発明例は熱処理のみを行った従来例
(m13,14.15)に比べはんだ性、耐錆性、表面
光沢にすぐれており、かつばね性の劣化も少ない。また
、熱処理も行わない従来例(Ih16)に対しては、ば
ね性が著しく優れている。比較例魚10は電解電気量が
過少であるため、熱処理で生じた酸化皮膜が残存しはん
だ性および耐錆性が劣る。比較何階11は電解電気量が
過大であるため、また、比較何階12は電解の電流密度
が過大であるため、いずれも表面光沢が劣化している。As shown in Table 1, the examples of the present invention are superior in solderability, rust resistance, and surface gloss compared to the conventional examples (m13, 14.15) in which only heat treatment was performed, and there is less deterioration in spring properties. Further, the spring properties are significantly superior to the conventional example (Ih16) which is not subjected to heat treatment. In Comparative Example Fish 10, since the amount of electrolyzed electricity was too small, the oxide film produced by the heat treatment remained, resulting in poor solderability and rust resistance. Because the amount of electrolyzed electricity in Comparative Floor 11 is too high, and because the current density of electrolysis in Comparative Floor 12 is too high, the surface gloss has deteriorated in both cases.
以上のことから明らかな如く、本発明によれば、ばね性
、はんだ性、耐錆性、表面光沢に優れたステンレスばね
材が得られ、はんだ付は不良や発錆によって生じる回路
の断線や接点不良の少ない材料として電子機器や精密機
器の信頼性向上に大いに効果を発揮できる。さらに自動
車部品など各種分野におけるばね材に適用しても多大の
効果が期待できる。As is clear from the above, according to the present invention, a stainless steel spring material with excellent spring properties, solderability, rust resistance, and surface gloss can be obtained, and it is possible to obtain a stainless steel spring material with excellent spring properties, solderability, rust resistance, and surface gloss. As a material with few defects, it can be highly effective in improving the reliability of electronic equipment and precision equipment. Furthermore, great effects can be expected when applied to spring materials in various fields such as automobile parts.
特許出願人 新日本製鐵株式会社Patent applicant: Nippon Steel Corporation
Claims (1)
を付与しつつ、露点−35℃以下の非酸化性雰囲気ガス
中に於いて350〜700℃で熱処理を施した後に、硝
酸、燐酸の1種あるいは2種を含みその総濃度が7.0
〜30.0wt%となる水溶液中で、0.05〜5.0
A/dm^2の電流密度の範囲で全電解電気量が10〜
500C/dm^2の陽極電解処理を行うことを特徴と
するステンレスばね材の製造方法。A cold-rolled stainless steel strip is subjected to heat treatment at 350 to 700°C in a non-oxidizing atmosphere gas with a dew point of -35°C or less while applying a tension of 0.2% proof stress or less, and then treated with nitric acid and phosphoric acid. Contains one or two of the following, with a total concentration of 7.0
0.05 to 5.0 in an aqueous solution of ~30.0 wt%
The total amount of electrolytic electricity is 10~ within the current density range of A/dm^2.
A method for manufacturing a stainless steel spring material, characterized by performing anodic electrolysis treatment at 500C/dm^2.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63262935A JPH0663120B2 (en) | 1988-10-20 | 1988-10-20 | Manufacturing method of stainless spring material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63262935A JPH0663120B2 (en) | 1988-10-20 | 1988-10-20 | Manufacturing method of stainless spring material |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH02111900A true JPH02111900A (en) | 1990-04-24 |
JPH0663120B2 JPH0663120B2 (en) | 1994-08-17 |
Family
ID=17382623
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP63262935A Expired - Fee Related JPH0663120B2 (en) | 1988-10-20 | 1988-10-20 | Manufacturing method of stainless spring material |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0663120B2 (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5749640A (en) * | 1980-09-09 | 1982-03-23 | Fujikura Ltd | Flame retardant polyvinyl chloride composition |
JPS61170599A (en) * | 1985-01-23 | 1986-08-01 | Kawasaki Steel Corp | Manufacture of stainless steel sheet having fine surface luster and superior resistance to hydrogen brittleness |
-
1988
- 1988-10-20 JP JP63262935A patent/JPH0663120B2/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5749640A (en) * | 1980-09-09 | 1982-03-23 | Fujikura Ltd | Flame retardant polyvinyl chloride composition |
JPS61170599A (en) * | 1985-01-23 | 1986-08-01 | Kawasaki Steel Corp | Manufacture of stainless steel sheet having fine surface luster and superior resistance to hydrogen brittleness |
Also Published As
Publication number | Publication date |
---|---|
JPH0663120B2 (en) | 1994-08-17 |
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