JPH0368951B2 - - Google Patents
Info
- Publication number
- JPH0368951B2 JPH0368951B2 JP6552084A JP6552084A JPH0368951B2 JP H0368951 B2 JPH0368951 B2 JP H0368951B2 JP 6552084 A JP6552084 A JP 6552084A JP 6552084 A JP6552084 A JP 6552084A JP H0368951 B2 JPH0368951 B2 JP H0368951B2
- Authority
- JP
- Japan
- Prior art keywords
- phosphate
- steel sheet
- ultra
- low carbon
- 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.)
- Expired
Links
- 229910019142 PO4 Inorganic materials 0.000 claims description 27
- 239000010452 phosphate Substances 0.000 claims description 27
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 26
- 229910000831 Steel Inorganic materials 0.000 claims description 20
- 239000010959 steel Substances 0.000 claims description 20
- 238000000137 annealing Methods 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000010960 cold rolled steel Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000005238 degreasing Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- -1 hydrogen ions Chemical class 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000655 Killed steel Inorganic materials 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910001567 cementite Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- KSOKAHYVTMZFBJ-UHFFFAOYSA-N iron;methane Chemical compound C.[Fe].[Fe].[Fe] KSOKAHYVTMZFBJ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 150000004764 thiosulfuric acid derivatives Chemical class 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
Classifications
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
Description
本発明は、C0.005wt％以下、Si：0.05wt％以
下で、TiおよびまたはNbを含有する極低炭素冷
延鋼板のリン酸塩処理性を改善する方法に関する
ものである。
冷延鋼板は自動車車体・家電製品等様々な用途
に巾広く用いられているが、冷延鋼板が使用され
る際には裸のまま使用される例はほとんどなく、
大半が塗装前下地処理としてリン酸塩処理を施さ
れた後、塗装されている。このリン酸塩処理性は
塗装後の美観および耐食性等の塗装性能を決する
重要なフアクターになつている。
一方、最近では、深絞り性を要求される部分に
は、Ｃ量が0.005wt％以下で、かつ炭化物形成元
素としてNbおよびまたはTiを含有する極低炭素
鋼板が用いられることが多くなつている。ところ
が、この極低炭素鋼板にリン酸塩処理を施すとリ
ン酸塩皮膜結晶が粗大化し、また不被覆部が部分
的に生じる。すなわち、従来用いられてきたＣ量
0.02〜0.08％の低炭素鋼板と比較して、リン酸塩
処理性が著しく劣つていることが判明した。これ
は、鋼中Ｃ量の低減によるリン酸塩皮膜形成反応
におけるカソード部の減少によるものと考えられ
る。
本発明の目的は、かかる問題点を解決すべく、
リン酸塩皮膜形成反応において初期析出核の生成
サイトとなるカソード部を付与することにより、
リン酸塩処理性のすぐれた冷延鋼板の製造方法を
提供することにある。
本発明は、Ｃが0.005wt％以下、Siが0.05wt％
以下でTiおよびまたはNbを合計で0.005wt％以
上含有する極低炭素冷延鋼板を非酸化性雰囲気中
で連続焼鈍する前に、鋼板表面にＳ換算量として
0.1〜5.0mg／m2のＳ化合物を付着せしめることを
特徴とするリン酸塩処理性の優れた極低炭素冷延
鋼板の製造方法を提供するものである。
以下、本発明のリン酸塩処理性の優れた極低炭
素冷延鋼板の製造方法につき詳細に説明する。
リン酸塩皮膜形成反応は、
アノード部：
Fe＋2H3PO4→Fe（H2PO4）2＋H2↑ …(1)
カソード部：
2Zn（H2PO4）2＋Fe（H2PO4）2＋4H2O
→Zn2Fe（PO4）2・4H2O＋4H3PO4 …(2)
または
3Zn（H2PO4）2・4H2O
→Zn3（PO4）2・4H2O＋4H3PO4 …(3)
からなるPH3.0前後の酸中での腐食反応およびリ
ン酸塩析出反応である。
一方、Ｃは鋼中にあつてセメンタイトFe3Cと
して析出し、Fe3Cは鋼の水素過電圧を低下させ、
酸中いおける鉄の腐食反応において、水素イオン
の陰極還元に対しカソード部として働くことが知
られている。
すなわち、鋼中でのＣ量すなわちFe3C量の低
減は、リン酸塩皮膜形成反応でのカソード部の減
少を意味し、極低炭素鋼板にリン酸塩処理を行う
と反応はカソード律速となり、皮膜形成反応は抑
制される。従つて、皮膜形成反応を促進し、リン
酸塩処理性を向上するには、鋼板表面のミクロカ
ソード部を付与すればよい。
本発明者らはかかる見地に基づいて、極低炭素
鋼板表面にカソード部を付与する方法について
種々の実験および研究を重ねた結果、連続焼鈍前
に鋼板表面にＳ換算量として0.1〜5.0mg／m2のＳ
化合物を付着せしめた極低炭素鋼板が、リン酸塩
処理性に優れていることを知見した。
焼鈍前にＳ化合物を塗布する技術としては、特
開昭48−48317により方法や、リン酸塩処理性向
上を目的として、0.2wt％以上のSiを含有する鋼
板Ｓ化合物を塗布した後に非酸化性雰囲気中で焼
鈍する方法が特開昭57−161035に開示されてい
る。しかしながら、これらはいずれも、焼鈍前の
Ｓ塗布により焼鈍前の鋼中Ｃの濃化による鋼板表
面のグラフアイト析出を防止することを目的とし
たものである。しかるに、本発明では鋼中Ｃ量が
0.005wt％以下の極低炭素鋼連続焼鈍材が対象で
あり、かかる鋼板では鋼中Ｃ量および焼鈍時間の
短さから考えて、焼鈍前Ｓ化合物塗布如何に関わ
らず、グラフアイト析出は起り得ず、Ｓ化合物塗
布の目的が本発明と異なる。
本発明では、また、鋼中のSiを0.05wt％以下に
限定する。その理由は、Siが0.05wt％超では焼鈍
前Ｓ化合物の塗布を行つても、リン酸塩処理性の
改善が期待できないからである。
本発明によるリン酸塩処理性向上効果は、リン
酸塩処理性阻害元素の析出防止によるものではな
く、焼鈍前の電解脱脂工程中および／またはその
直後においてＳ化合物の形でＳを鋼板表面に付着
させ、しかる後に600℃以上の高温で焼鈍するこ
とにより、鋼中成分と化学結合させてカソード部
を提供することに依るものである。本発明者らの
研究のよると、リン酸塩処理性向上効果を与える
Ｓ付着量の下限値として0.1mg／m2という値を得
た。また、Ｓ付着量が5.0mg／m2を超えるとカソ
ード面積が増大し、リン酸塩処理性はかえつて阻
害される。
本発明で使用されるＳ化合物としてはいかなる
ものでもよいが、硫酸塩、亜硫酸塩、亜硫酸水
素、チオ硫酸塩などの酸化イオウ化塩、ハロゲン
化イオウ、硫化物、チオシアン化物およびチオ尿
素などの有機系化合物が有効である。また、鋼板
表面へのＳ付着方法としてはいかなるものでもよ
いが、連続焼鈍前工程において、Ｓ化合物を含有
した電解脱脂液中で鋼板を電解脱脂する方法、あ
るいは電解脱脂後の鋼板表面へスプレー、浸漬、
ロールなどにより塗布する方法が代表的に挙げら
れる。
次に、本発明を実施例につき具体的に説明す
る。
Ｃ：0.0028wt％、Si：0.014wt％、Mn：0.16wt
％、Nb：0.016wt％含有する極低炭連鋳アルミキ
ルド鋼の冷間圧延板（ｔ＝1.01mm）を５％NaOH
溶液中で電解脱脂後、第１表に示した各濃度の水
溶液中に鋼板を室温で浸漬し、リンガロールで水
切りした後、熱風乾燥し、N293％、H27％、露
点−47℃の雰囲気中で800℃×1minの焼鈍を施し
て試験片を作成し、リン酸塩処理性を評価した。
リン酸塩処理は日本ペイント(株)製、グラノジン
SD2000を用い、120秒浸漬処理により行なつた。
第１図に試料のリン酸塩処理性の結果を示し
た。横軸に鋼板表面Ｓ付着量、縦軸に析出リン酸
塩結晶数を示す。析出リン酸塩結晶数が多い程、
リン酸塩処理性は良好であることを意味する。
第１図より、表面Ｓ付着量が0.1〜5.0mg／m2の
範囲にあるとき、リン酸塩処理性が良好であるこ
とがわかる。
The present invention relates to a method for improving the phosphatability of an ultra-low carbon cold rolled steel sheet containing Ti and/or Nb with C0.005wt% or less and Si:0.05wt% or less. Cold-rolled steel sheets are widely used in various applications such as automobile bodies and home appliances, but when cold-rolled steel sheets are used, they are rarely used in their bare state.
Most of them are painted after being treated with phosphate as a base treatment before painting. This phosphate treatment property is an important factor that determines the appearance after painting and coating performance such as corrosion resistance. On the other hand, recently, ultra-low carbon steel sheets with a C content of 0.005wt% or less and containing Nb and/or Ti as carbide-forming elements have been increasingly used in parts that require deep drawability. . However, when this ultra-low carbon steel sheet is subjected to phosphate treatment, the phosphate coating crystals become coarse and some uncovered areas occur. In other words, the amount of C conventionally used
It was found that the phosphate treatability was significantly inferior compared to low carbon steel sheets containing 0.02 to 0.08%. This is considered to be due to a decrease in the cathode area in the phosphate film forming reaction due to the reduction in the amount of C in the steel. The purpose of the present invention is to solve such problems,
By providing a cathode part that becomes the initial precipitation nucleus generation site in the phosphate film formation reaction,
An object of the present invention is to provide a method for producing a cold rolled steel sheet with excellent phosphating properties. In the present invention, C is 0.005wt% or less and Si is 0.05wt%
Below, before continuous annealing of ultra-low carbon cold-rolled steel sheets containing 0.005wt% or more of Ti and/or Nb in total in a non-oxidizing atmosphere,
The present invention provides a method for producing an ultra-low carbon cold-rolled steel sheet with excellent phosphate treatment properties, which is characterized by depositing an S compound of 0.1 to 5.0 mg/m 2 . Hereinafter, the method for producing an ultra-low carbon cold-rolled steel sheet with excellent phosphate treatment properties according to the present invention will be described in detail. The phosphate film formation reaction is as follows: Anode: Fe+2H 3 PO 4 →Fe(H 2 PO 4 ) 2 +H 2 ↑ …(1) Cathode: 2Zn(H 2 PO 4 ) 2 +Fe(H 2 PO 4 ) 2 +4H 2 O →Zn 2 Fe (PO 4 ) 2・4H 2 O＋4H 3 PO 4 …(2) or 3Zn (H 2 PO 4 ) 2・4H 2 O →Zn 3 (PO 4 ) 2・4H 2 O＋4H 3 PO 4 ...(3) This is a corrosion reaction and a phosphate precipitation reaction in an acid around PH3.0. On the other hand, C is present in steel and precipitates as cementite Fe 3 C, and Fe 3 C reduces the hydrogen overvoltage of steel.
It is known that in the corrosion reaction of iron in acid, it acts as a cathode for the cathodic reduction of hydrogen ions. In other words, a reduction in the amount of C in the steel, that is, the amount of Fe 3 C, means a reduction in the cathode area in the phosphate film formation reaction, and when ultra-low carbon steel sheets are subjected to phosphate treatment, the reaction becomes rate-limited by the cathode. , the film-forming reaction is inhibited. Therefore, in order to promote the film-forming reaction and improve the phosphate treatment properties, it is sufficient to provide a microcathode portion on the surface of the steel sheet. Based on this point of view, the present inventors have conducted various experiments and research on methods for providing a cathode portion on the surface of an ultra-low carbon steel sheet. As a result, the inventors have conducted various experiments and research on methods for providing a cathode portion on the surface of an ultra-low carbon steel sheet. S of m2
It has been discovered that ultra-low carbon steel sheets coated with compounds have excellent phosphate treatment properties. As for the technique of applying an S compound before annealing, there is a method described in Japanese Patent Application Laid-Open No. 48-48317, and for the purpose of improving phosphating properties, a non-oxidizing method is proposed after applying an S compound to a steel sheet containing 0.2 wt% or more of Si. A method of annealing in a neutral atmosphere is disclosed in JP-A-57-161035. However, all of these methods are intended to prevent graphite precipitation on the steel plate surface due to concentration of C in the steel before annealing by applying S before annealing. However, in the present invention, the amount of C in the steel is
The target is continuously annealed ultra-low carbon steel materials with a carbon content of 0.005wt% or less, and considering the amount of C in the steel and the short annealing time, graphite precipitation may occur regardless of whether S compound is applied before annealing. First, the purpose of applying the S compound is different from that of the present invention. In the present invention, Si in the steel is also limited to 0.05wt% or less. The reason for this is that if Si exceeds 0.05 wt%, no improvement in phosphate treatability can be expected even if an S compound is applied before annealing. The effect of improving phosphating properties according to the present invention is not due to the prevention of precipitation of elements that inhibit phosphating properties, but rather S is added to the steel sheet surface in the form of S compounds during and/or immediately after the electrolytic degreasing process before annealing. This method relies on chemically bonding with the components in the steel by attaching it and then annealing it at a high temperature of 600°C or higher to provide a cathode part. According to the research conducted by the present inventors, a value of 0.1 mg/m 2 was obtained as the lower limit of the S adhesion amount that provides the effect of improving phosphate treatment properties. Furthermore, if the S adhesion amount exceeds 5.0 mg/m 2 , the cathode area increases, and the phosphate treatment property is rather inhibited. The S compound used in the present invention may be of any type, including oxidized sulfides such as sulfates, sulfites, hydrogen sulfites, and thiosulfates, and organic compounds such as sulfur halides, sulfides, thiocyanides, and thioureas. type compounds are effective. In addition, any method may be used to attach S to the surface of the steel sheet, such as a method of electrolytically degreasing the steel sheet in an electrolytic degreasing solution containing an S compound in the pre-continuous annealing process, or a method of spraying the surface of the steel sheet after electrolytic degreasing. immersion,
A typical example is a method of applying with a roll or the like. Next, the present invention will be specifically explained using examples. C: 0.0028wt%, Si: 0.014wt%, Mn: 0.16wt
%, Nb: A cold rolled plate (t = 1.01 mm) of ultra-low carbon continuously cast aluminum killed steel containing 0.016 wt% was coated with 5% NaOH.
After electrolytic degreasing in a solution, the steel plate was immersed in an aqueous solution of each concentration shown in Table 1 at room temperature, drained with a Ringer roll, and dried with hot air, with a concentration of 93% N 2 , 7% H 2 , and a dew point of -47. Test specimens were prepared by annealing at 800°C for 1 min in an atmosphere of 30°C, and the phosphate treatability was evaluated. Phosphate treatment is made by Nippon Paint Co., Ltd., Granozin
This was done using SD2000 by immersion treatment for 120 seconds. Figure 1 shows the results of the phosphate treatment of the samples. The horizontal axis shows the amount of S deposited on the steel plate surface, and the vertical axis shows the number of precipitated phosphate crystals. The greater the number of precipitated phosphate crystals, the more
Phosphate treatment property means good. From FIG. 1, it can be seen that when the surface S adhesion amount is in the range of 0.1 to 5.0 mg/m 2 , the phosphate treatment property is good.
【表】【table】
第１図は鋼板表面Ｓ付着量とリン酸塩処理性と
の関係を示すグラフである。
FIG. 1 is a graph showing the relationship between the amount of S deposited on the surface of a steel plate and the phosphate treatability.
Claims (1)
TiおよびまたはNbを合計で0.005wt％以上含有
する極低炭素冷延鋼板を非酸化性雰囲気中で連続
焼鈍する前に、鋼板表面にＳ換算量として0.1〜
5.0mg／m2のＳ化合物を付着せしめることを特徴
とするリン酸塩処理性の優れた極低炭素冷延鋼板
の製造方法。1 C is 0.005wt% or less, Si is 0.05wt% or less,
Before continuously annealing an ultra-low carbon cold rolled steel sheet containing Ti and/or Nb in total at least 0.005wt% in a non-oxidizing atmosphere, the amount of S equivalent on the surface of the steel sheet is 0.1~
A method for producing an ultra-low carbon cold-rolled steel sheet with excellent phosphate treatment properties, characterized by adhering 5.0 mg/m 2 of S compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6552084A JPS60208481A (en) | 1984-04-02 | 1984-04-02 | Production of dead soft cold rolled steel sheet having excellent phosphate treatability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6552084A JPS60208481A (en) | 1984-04-02 | 1984-04-02 | Production of dead soft cold rolled steel sheet having excellent phosphate treatability |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60208481A JPS60208481A (en) | 1985-10-21 |
| JPH0368951B2 true JPH0368951B2 (en) | 1991-10-30 |
Family
ID=13289380
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6552084A Granted JPS60208481A (en) | 1984-04-02 | 1984-04-02 | Production of dead soft cold rolled steel sheet having excellent phosphate treatability |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60208481A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2688517B1 (en) * | 1992-03-10 | 1994-06-03 | Stephanois Rech | PROCESS FOR THE PHOSPHATION OF STEEL PARTS, TO IMPROVE THEIR CORROSION AND WEAR RESISTANCES. |
| JP2007162057A (en) * | 2005-12-13 | 2007-06-28 | Jfe Steel Kk | High strength steel sheet having excellent phosphate treatability |
| JP5168793B2 (en) * | 2006-02-16 | 2013-03-27 | Ｊｆｅスチール株式会社 | Manufacturing method of high-strength cold-rolled steel sheet with excellent corrosion resistance after painting |
| JP4826297B2 (en) * | 2006-03-14 | 2011-11-30 | Ｊｆｅスチール株式会社 | Cold-rolled steel sheet with excellent phosphatability |
-
1984
- 1984-04-02 JP JP6552084A patent/JPS60208481A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60208481A (en) | 1985-10-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |