JP3303344B2 - Method for producing cold-rolled sheet of titanium or titanium alloy with few surface defects - Google Patents

Method for producing cold-rolled sheet of titanium or titanium alloy with few surface defects

Info

Publication number
JP3303344B2
JP3303344B2 JP21524392A JP21524392A JP3303344B2 JP 3303344 B2 JP3303344 B2 JP 3303344B2 JP 21524392 A JP21524392 A JP 21524392A JP 21524392 A JP21524392 A JP 21524392A JP 3303344 B2 JP3303344 B2 JP 3303344B2
Authority
JP
Japan
Prior art keywords
titanium
oxygen
rolled sheet
cold
rich layer
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 - Fee Related
Application number
JP21524392A
Other languages
Japanese (ja)
Other versions
JPH0657388A (en
Inventor
正人 福田
貴之 木田
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.)
Kobe Steel Ltd
Original Assignee
Kobe Steel 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 Kobe Steel Ltd filed Critical Kobe Steel Ltd
Priority to JP21524392A priority Critical patent/JP3303344B2/en
Publication of JPH0657388A publication Critical patent/JPH0657388A/en
Application granted granted Critical
Publication of JP3303344B2 publication Critical patent/JP3303344B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Description

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

【0001】[0001]

【産業上の利用分野】本発明は、表面疵の少ないチタン
およびチタン合金冷間圧延板の製造方法に関し、詳細に
は冷間圧延前に脱スケールと熱処理を行なって表面疵を
減少させたチタンおよびチタン合金冷間圧延板に関する
ものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a cold-rolled sheet of titanium and a titanium alloy having a small number of surface defects, and more particularly to a method of reducing the surface defects by performing descaling and heat treatment before cold rolling. And a cold rolled titanium alloy sheet.

【0002】[0002]

【従来の技術】チタンおよびチタン合金(以下チタン材
料と言うことがある)の薄板の製造は図1に示すように
熱間圧延,熱処理,脱スケールおよび冷間圧延工程を経
て行なわれるのが一般的である。この場合、薄板製品1
表面に図2に示すような表面疵2(以下ヘゲ疵と言う)
が生じ、製品不良の一因となっている。このヘゲ疵は熱
延板表面に存在する高濃度酸素固溶層(以下酸素リッチ
層と言う)が脱スケール時に充分除去されずに残留し、
次いで行なわれる冷間圧延時に母相金属との延性の差が
あるために疵になるものである。現状の技術では酸素リ
ッチ層の残留を非破壊的に検出できない(スケール残り
などの極端な場合を除く)ため、疵を完全に防止するこ
とが不可能である。
2. Description of the Related Art Thin sheets of titanium and titanium alloys (hereinafter sometimes referred to as titanium materials) are generally manufactured through hot rolling, heat treatment, descaling and cold rolling as shown in FIG. It is a target. In this case, the thin product 1
Surface flaw 2 on the surface as shown in FIG.
Occurs, which contributes to product failure. This scab is left without the high concentration oxygen solid solution layer (hereinafter referred to as oxygen rich layer) existing on the hot rolled sheet surface being sufficiently removed during descaling,
It is flawed due to the difference in ductility with the parent metal during the subsequent cold rolling. With the current technology, the residual oxygen-rich layer cannot be detected nondestructively (except for extreme cases such as residual scale), so that it is impossible to completely prevent flaws.

【0003】まずヘゲ疵の特徴は、図2に示したよう
に、微小割れを伴なうとともに母材金属(チタン材料)
よりも硬い部分が存在することである。この高硬度の部
分が高濃度の酸素を固溶している部分、すなわち酸素リ
ッチ層であり、その硬さレベルから酸素濃度は1%以上
と推測される。
First, as shown in FIG. 2, the characteristics of the scab flaws are accompanied by minute cracks and a base metal (titanium material).
Is that there are harder parts. The high-hardness portion is a portion in which high-concentration oxygen is dissolved, that is, an oxygen-rich layer. From the hardness level, the oxygen concentration is estimated to be 1% or more.

【0004】この酸素リッチ層は酸素を含んだ雰囲気下
でチタン材料を加熱することによって図3に示すように
層状に生成する。酸素リッチ層3の厚さは加熱温度が高
い程、また加熱時間が長い程厚くなる。酸素リッチ層は
熱間圧延工程で若干薄くなりながら分断され、熱延後の
板面には図4に示すように凹部に点々と残留することに
なる。この点状に残留している酸素リッチ層3は母材金
属のチタンよりも硬く延性挙動が異なるため、冷間圧延
工程で表面疵となる。従って冷間圧延工程の前の脱スケ
ール工程で酸素リッチ層をすべて取り除く必要性があ
る。
This oxygen-rich layer is formed in a layered form as shown in FIG. 3 by heating a titanium material in an atmosphere containing oxygen. The thickness of the oxygen-rich layer 3 increases as the heating temperature increases and as the heating time increases. The oxygen-rich layer is divided while being slightly thinned in the hot rolling step, and is left in the concave portions on the sheet surface after hot rolling as shown in FIG. Since the oxygen-rich layer 3 remaining in the form of dots is harder than titanium as the base metal and has a different ductile behavior, it becomes a surface flaw in the cold rolling step. Therefore, it is necessary to remove all the oxygen-rich layer in the descaling step before the cold rolling step.

【0005】酸素リッチ層の厚さは通常20〜50μm
であるが、生成する時の温度・時間等の加熱条件によっ
て層厚が増大していることも考えられるため、結局チタ
ン板の表面層を少なくとも両面で100μm以上は除去
しなければならない。この除去量は、冷間圧延板(コイ
ル)に供される熱間圧延板(コイル)の厚さが3〜4mm
であることから、全厚の5〜7%に当たり、非常に多い
歩留ロスである。さらに表面研削や硝弗酸による酸洗浄
で100μmもの板表面を除去するというのは非能率的
であり、工業的方法とはいえない。
The thickness of the oxygen-rich layer is usually 20 to 50 μm.
However, since it is conceivable that the layer thickness is increased by heating conditions such as temperature and time at the time of formation, it is necessary to remove the surface layer of the titanium plate by at least 100 μm on both surfaces. The thickness of the hot-rolled plate (coil) supplied to the cold-rolled plate (coil) is 3 to 4 mm.
Therefore, the yield loss is 5 to 7% of the total thickness, which is a very large yield loss. Further, removing a plate surface as large as 100 μm by surface grinding or acid cleaning with nitric hydrofluoric acid is inefficient and cannot be said to be an industrial method.

【0006】[0006]

【発明が解決しようとする課題】そこで本発明では、上
記残留酸素リッチ層を消滅もしくは軽減させ、ヘゲ疵の
発生のないチタンまたはチタン合金冷間圧延板を製造す
ることを目的とする。
SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to eliminate or reduce the residual oxygen-rich layer and to produce a titanium or titanium alloy cold-rolled plate free of bark defects.

【0007】[0007]

【課題を解決するための手段】上記目的を達成し得た本
発明は、チタンおよびチタン合金の熱間圧延板から冷間
圧延板を製造する工程において、熱間圧延板をショット
ブラスト処理した後に硝弗酸で脱スケールし、次いで6
00〜850℃で2時間以上非酸化性雰囲気焼鈍を行な
ったのちに冷間圧延するところに要旨を有する。
SUMMARY OF THE INVENTION The present invention, which has achieved the above-mentioned object, provides a process for producing a cold-rolled plate from a hot-rolled plate of titanium and a titanium alloy, after the hot-rolled plate is shot-blasted. Descaling with nitric hydrofluoric acid, then 6
The gist is that cold rolling is performed after annealing in a non-oxidizing atmosphere at 00 to 850 ° C. for 2 hours or more.

【0008】[0008]

【作用】熱間圧延後に図4のような状態で無数に点々と
存在する酸素リッチ層1個1個の厚さをすべて測定する
ことは不可能であり、非破壊的に検出する方法も確立さ
れていない。また従来法のように板表面を100μmも
除去することは無駄である。
After the hot rolling, it is impossible to measure the thickness of each of the oxygen-rich layers infinitely numerous in the state as shown in FIG. 4, and a non-destructive detection method has been established. It has not been. It is useless to remove the plate surface by 100 μm as in the conventional method.

【0009】そこで本発明者らは、検出困難な残留酸素
リッチ層中の酸素を熱処理によりチタン板内部に拡散さ
せて、酸素リッチ層を消滅あるいは軽減させた後に冷間
圧延することで、ヘゲ疵の無い(あるいは実用上無視し
得る発生率の)冷延板が得られることを見出し本発明に
至ったものである。
Therefore, the present inventors have made it difficult to diffuse the oxygen in the residual oxygen-rich layer, which is difficult to detect, into the inside of the titanium plate by heat treatment, to eliminate or reduce the oxygen-rich layer, and then to carry out cold rolling. The present inventors have found that a cold-rolled sheet having no flaws (or a practically negligible incidence) can be obtained, and the present invention has been accomplished.

【0010】まず本発明では熱間圧延板にショットブラ
スト処理を施して表面の酸化スケール皮膜を破壊したの
ち、硝弗酸で酸洗を行なう。酸洗によって除去すべき板
厚は両面の合計で5〜30μm、より好ましくは5〜1
0μmと少ない方が良い。冷間圧延板として供される熱
間圧延板は厚さ3〜4mmで、そのうち酸素リッチ層は2
0〜30μmであるが、本発明では酸洗工程後の熱処理
によって酸素リッチ層中の酸素を拡散させるため、従来
法のように100μmも除去する必要はない。
First, in the present invention, after the hot rolled sheet is subjected to shot blasting to break the oxide scale film on the surface, pickling is performed with nitric hydrofluoric acid. The thickness of the plate to be removed by pickling is 5 to 30 μm in total on both sides, more preferably 5 to 1 μm.
A smaller value of 0 μm is better. The hot-rolled plate serving as a cold-rolled plate has a thickness of 3 to 4 mm, of which the oxygen-rich layer is 2 mm.
In the present invention, since the oxygen in the oxygen-rich layer is diffused by the heat treatment after the pickling step, it is not necessary to remove 100 μm as in the conventional method.

【0011】酸洗後のチタン板は、冷間圧延工程の前に
非酸化性雰囲気下で焼鈍される。通常冷間圧延板(コイ
ル)は最終工程で真空またはアルゴンガス中で焼鈍が行
なわれるので、この工程用の設備を用いて冷間圧延前の
焼鈍を行なえば特殊な設備対応は不要である。
The pickled titanium sheet is annealed in a non-oxidizing atmosphere before the cold rolling step. Usually, the cold-rolled sheet (coil) is annealed in a vacuum or argon gas in the final step. Therefore, if annealing is performed before cold rolling using equipment for this step, no special equipment is required.

【0012】冷間圧延前の上記焼鈍は2時間以上行な
う。2時間より少ないと酸素リッチ層がチタン板表面に
残留する恐れがあり好ましくない。チタンまたはチタン
合金は、酸素との親和性が強い金属であり、ガス中の不
純物酸素を除去するために使用されるように有効な酸素
吸収媒体である。このため、外部からの酸素の供給を遮
断しながら焼鈍を行なうことにより、酸素リッチ層内の
酸素がチタン板の内部へと拡散するものと考えられる。
The above-mentioned annealing before cold rolling is performed for 2 hours or more. If it is less than 2 hours, the oxygen-rich layer may remain on the titanium plate surface, which is not preferable. Titanium or a titanium alloy is a metal having a strong affinity for oxygen, and is an effective oxygen absorbing medium to be used for removing impurity oxygen in a gas. For this reason, it is considered that by performing annealing while shutting off supply of oxygen from the outside, oxygen in the oxygen-rich layer diffuses into the titanium plate.

【0013】従ってショットブラスト、酸洗に続く、非
酸化性雰囲気での焼鈍という本発明法の処理により、酸
素リッチ層の酸素濃度低下および硬度の低下を達成させ
ることができ、その結果冷間圧延工程を行なってもヘゲ
疵は発生しない。
[0013] Therefore, the treatment of the method of the present invention of annealing in a non-oxidizing atmosphere following shot blasting and pickling can reduce the oxygen concentration and the hardness of the oxygen-rich layer. Even if the process is performed, no barbed flaw is generated.

【0014】[0014]

【実施例】以下に実施例を挙げ本発明をより具体的に説
明するが、下記実施例は本発明を制限するものではな
く、前・後記の趣旨を逸脱しない範囲で変更実施するこ
とはすべて本発明の技術的範囲に包含される。
EXAMPLES The present invention will be described in more detail with reference to the following examples. However, the following examples do not limit the present invention, and all changes and modifications may be made without departing from the spirit of the preceding and following aspects. It is included in the technical scope of the present invention.

【0015】実施例 厚さ3.5mm のチタン熱間圧延板を試料とした。酸素リッ
チ層の厚みは20〜30μmで表面に点々と存在していた。
まずショットブラスト処理を行なった後、2%HFと15
%HNO3 を含む硝弗酸で酸洗を行なった。酸洗によっ
て減少する板厚(両面合計量)を10,30,60,100 μm
と変化させた。酸洗後 650℃×2時間真空焼鈍を行なっ
た実施例1〜4と真空焼鈍を行なわなかった比較例1〜
4について冷間圧延を行なった。冷間圧延は圧下率49%
となるように行ない(板厚3.5mm→1.8mm )、冷間圧延
後の表面状態の観察を拡大写真により行なった。結果を
表1に示す。
[0015] and titanium hot-rolled plate of Example thickness 3.5mm and sample. The thickness of the oxygen-rich layer was 20 to 30 μm and existed on the surface in a dotted manner.
First, after shot blasting, 2% HF and 15%
Pickling was performed with nitric hydrofluoric acid containing% HNO 3 . Reduce the plate thickness (total amount on both sides) reduced by pickling to 10, 30, 60, 100 μm
Was changed. Examples 1-4, in which vacuum annealing was performed for 2 hours at 650 ° C. after pickling, and Comparative Examples 1, in which vacuum annealing was not performed.
4 was cold-rolled. 49% reduction in cold rolling
(From 3.5 mm to 1.8 mm in thickness), and observation of the surface state after cold rolling was carried out by an enlarged photograph. Table 1 shows the results.

【0016】[0016]

【表1】 [Table 1]

【0017】表1の結果から、真空焼鈍を行なわなかっ
た比較例は、酸洗で板表面を 100μm除去しなければ表
面疵の発生を防ぐことはできなかったのに対し、本発明
法による実施例では10μmの除去だけでも表面疵の発生
は全く認められず、真空焼鈍によって酸素リッチ層が拡
散あるいは消滅することが明らかである。
From the results in Table 1, it can be seen that in the comparative example in which vacuum annealing was not performed, the surface flaw could not be prevented unless the plate surface was removed by 100 μm by pickling. In the example, no surface flaws were generated at all even by removing 10 μm alone, and it is clear that the oxygen-rich layer diffuses or disappears by vacuum annealing.

【0018】[0018]

【発明の効果】本発明は以上のように構成されており、
真空焼鈍を行なうことによって酸洗による熱間圧延板表
面の除去量を非常に少なくすることができ、表面疵の全
くないチタンまたはチタン合金の冷間圧延板を製造でき
た。
The present invention is configured as described above.
By performing vacuum annealing, the removal amount of the hot-rolled sheet surface by pickling could be extremely reduced, and a cold-rolled sheet of titanium or a titanium alloy without any surface flaws could be produced.

【図面の簡単な説明】[Brief description of the drawings]

【図1】チタン薄板の一般的な製造工程図である。FIG. 1 is a general manufacturing process diagram of a titanium thin plate.

【図2】チタン板表面のヘゲ疵を上から見た状態の模式
図である。
FIG. 2 is a schematic diagram of a state in which a barb flaw on the surface of a titanium plate is viewed from above.

【図3】熱間圧延前の酸素リッチ層の存在を示すチタン
薄板の断面模式図である。
FIG. 3 is a schematic sectional view of a titanium sheet showing the presence of an oxygen-rich layer before hot rolling.

【図4】熱間圧延後の酸素リッチ層の存在を示すチタン
薄板の断面模式図である。
FIG. 4 is a schematic cross-sectional view of a titanium sheet showing the presence of an oxygen-rich layer after hot rolling.

【符号の説明】[Explanation of symbols]

1 チタン(またはチタン合金)薄板 2 ヘゲ疵 3 酸素リッチ層 1 Titanium (or titanium alloy) thin plate 2 Scratch flaw 3 Oxygen rich layer

───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭58−42761(JP,A) 特開 昭61−284559(JP,A) 特開 昭62−280353(JP,A) (58)調査した分野(Int.Cl.7,DB名) C22F 1/00 - 3/02 B21B 45/06 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-58-42761 (JP, A) JP-A-61-284559 (JP, A) JP-A-62-280353 (JP, A) (58) Field (Int.Cl. 7 , DB name) C22F 1/00-3/02 B21B 45/06

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 チタンおよびチタン合金の熱間圧延板か
ら冷間圧延板を製造する工程において、熱間圧延板をシ
ョットブラスト処理した後に硝弗酸で脱スケールし、次
いで 600〜 850℃で2時間以上非酸化性雰囲気焼鈍を行
なったのちに冷間圧延することを特徴とする表面疵の少
ないチタンまたはチタン合金の冷間圧延板の製造方法。
In a process of manufacturing a cold-rolled sheet from a hot-rolled sheet of titanium and a titanium alloy, the hot-rolled sheet is shot-blasted, descaled with nitric hydrofluoric acid, and then heated at 600 to 850 ° C. A method for producing a cold-rolled sheet of titanium or a titanium alloy having a small number of surface defects, wherein the sheet is subjected to annealing in a non-oxidizing atmosphere for at least one hour and then to cold rolling.
JP21524392A 1992-08-12 1992-08-12 Method for producing cold-rolled sheet of titanium or titanium alloy with few surface defects Expired - Fee Related JP3303344B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP21524392A JP3303344B2 (en) 1992-08-12 1992-08-12 Method for producing cold-rolled sheet of titanium or titanium alloy with few surface defects

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP21524392A JP3303344B2 (en) 1992-08-12 1992-08-12 Method for producing cold-rolled sheet of titanium or titanium alloy with few surface defects

Publications (2)

Publication Number Publication Date
JPH0657388A JPH0657388A (en) 1994-03-01
JP3303344B2 true JP3303344B2 (en) 2002-07-22

Family

ID=16669095

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JP3303344B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104070076A (en) * 2014-05-30 2014-10-01 云南钛业股份有限公司 Surface treatment process for hot rolled titanium coil for cold rolling

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102328278A (en) * 2011-07-01 2012-01-25 云南钛业股份有限公司 Method for removing scale through shot blasting on titanium and titanium alloy strip coils
CN102909236A (en) * 2012-11-14 2013-02-06 西部钛业有限责任公司 Preparing method of wide-width pure titanium roll
KR101522799B1 (en) * 2013-12-24 2015-05-26 주식회사 포스코 Method for manufacturing titanium sheet
WO2021152675A1 (en) * 2020-01-27 2021-08-05 オリンパス株式会社 Method for manufacturing ultrasonic treatment tool

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104070076A (en) * 2014-05-30 2014-10-01 云南钛业股份有限公司 Surface treatment process for hot rolled titanium coil for cold rolling

Also Published As

Publication number Publication date
JPH0657388A (en) 1994-03-01

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