JP4865425B2 - Method for producing aluminum alloy plate with excellent surface treatment - Google Patents
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この発明は、建材用内外装パネル、各種輸送機器のパネル、電気機器パネル、電気部品、光学機器、厨房機器、その他日用品など、表面品質が良好であることが要求される用途において、エッチングなどの化学的もしくは電気化学的表面処理を施して使用される表面処理用のアルミニウム合金板の製造方法に関するものである。 This invention can be used for interior and exterior panels for building materials, panels for various transportation equipment, electrical equipment panels, electrical components, optical equipment, kitchen equipment, other daily necessities, etc. The present invention relates to a method for producing an aluminum alloy plate for surface treatment that is used after being subjected to chemical or electrochemical surface treatment.
建材用内外装パネルや各種機器のパネルなどにおいては、商品価値の点から、表面品質が優れていて外観上の欠陥が少ないことが強く要求される。一方この種の用途では、素材アルミニウム板の表面に化学的もしくは電気化学的エッチングを施したり、またエッチング後にさらに陽極酸化処理(アルマイト処理)を施したりするなど、表面処理を施して使用することが多く、したがって素材板に対しては、エッチング性などの表面処理性が優れていて、表面処理後の表面にムラやストリークス(スジ)などの外観欠陥が生じることがないことが望まれている。 In the interior / exterior panels for building materials and the panels of various devices, from the viewpoint of commercial value, it is strongly required that the surface quality is excellent and there are few defects in appearance. On the other hand, in this type of application, the surface of the material aluminum plate may be subjected to a surface treatment such as chemical or electrochemical etching, or further anodizing (alumite treatment) after etching. Therefore, it is desired that the material plate has excellent surface treatment properties such as etching properties, and does not cause appearance defects such as unevenness and streaks on the surface after the surface treatment. .
ところで各種アルミニウム合金のうちでも、純アルミニウム系(JIS 1000番系)のアルミニウム合金は、強度はさほど高くないものの、表面品質が良好で、表面処理性も比較的良好であることから、この種の用途に従来から広く使用されている。但し、この種のパネル等の用途でも、ある程度は強度を有していることが要求されるのが通常である。このように表面処理性が良好でまたある程度の強度が要求されるパネル等の用途の純アルミニウム系のアルミニウム合金板の製造方法としては、従来は、鋳塊を熱間圧延後、中間焼鈍を施して冷間圧延を行なうか、または熱間圧延後の冷間圧延の中途で中間焼鈍を行ない、最終の冷間圧延によって調質度H18もしくはH24程度の硬質板とすること多い。このようにして、硬質板に仕上げられた板の組織は、冷間圧延による組織が残った繊維状の加工組織となる。 Among various aluminum alloys, pure aluminum (JIS 1000 series) aluminum alloys are not so high in strength, but have good surface quality and relatively good surface treatment properties. It has been widely used for applications. However, it is usually required to have a certain degree of strength even in applications such as this type of panel. As a method for producing a pure aluminum-based aluminum alloy plate for applications such as panels that require good surface treatment and a certain level of strength, conventionally, an ingot is subjected to intermediate annealing after hot rolling of the ingot. Cold rolling is performed, or intermediate annealing is performed in the middle of cold rolling after hot rolling, and a hard plate having a tempering degree of H18 or H24 is often obtained by final cold rolling. In this way, the structure of the plate finished into a hard plate becomes a fibrous processed structure in which the structure obtained by cold rolling remains.
一方、最近では、省エネルギ、工程数節減によるコストダウンを図るため、前述のような熱間圧延と冷間圧延との間、あるいは冷間圧延の中途における再結晶のための中間焼鈍を行なわず、熱間圧延からその巻取、冷却の過程で熱延板を自己再結晶させ、その後は冷間圧延のみを施して硬質板に仕上げることが多くなっている。 On the other hand, recently, in order to save energy and reduce costs by reducing the number of processes, intermediate annealing for recrystallization between hot rolling and cold rolling as described above or in the middle of cold rolling is not performed. In many cases, a hot rolled sheet is self-recrystallized in the process of hot rolling, winding and cooling, and thereafter only cold rolling is performed to finish a hard plate.
ところで一般にアルミニウム合金板の製造過程では、熱間圧延時に不均一に粗大な再結晶粒が生じてしまうことが多く、その粗大な再結晶粒に起因して、素材板に表面処理を行なった後の表面に、ストリークスやムラ等の外観欠陥が生じてしまうことがあり、特に前述のように中間焼鈍を行なわずに硬質板に仕上げた場合には、そのおそれが高い。 By the way, in general, in the process of manufacturing an aluminum alloy sheet, non-uniformly coarse recrystallized grains are often generated during hot rolling, and after the surface treatment is performed on the base plate due to the coarse recrystallized grains. In some cases, appearance defects such as streaks and unevenness may occur on the surface of the steel plate, and particularly when the hard plate is finished without performing the intermediate annealing as described above, the risk is high.
ここで、表面品質が優れていることが要求されるパネル等の用途の表面処理用アルミニウム合金板の製造方法としては、例えば特許文献1では、熱間圧延時の圧下量や圧延温度を最適化して粗大な再結晶の発生を防止し、製品板の粒径や同一結晶面を有する集合体のサイズを規制することによって、表面処理後の表面のストリークスやムラの発生を防止することが提案されている。 Here, as a method of manufacturing an aluminum alloy sheet for surface treatment for applications such as panels that require excellent surface quality, for example, in Patent Document 1, the reduction amount and rolling temperature during hot rolling are optimized. Proposal to prevent the occurrence of streak and unevenness of the surface after surface treatment by preventing the occurrence of coarse recrystallization and regulating the grain size of the product plate and the size of the aggregate having the same crystal plane Has been.
また特許文献2においては、熱間圧延条件を規制し、製品板の結晶方位を均一分散させる指標として、素材板表面の結晶粒の明暗のコントラストを分散(平均化)させることにより、表面処理後の表面性状を改善することが提案され、さらに特許文献3においては、アルミニウム合金板における種々の結晶方位のうち、S方位結晶粒の方位密度を12以上、Cu方位結晶粒の方位密度を10以上に規制することによって、表面性状の改善を図ることが提案されている。 In Patent Document 2, after the surface treatment, the hot rolling conditions are regulated, and the contrast of light and darkness of the crystal grains on the surface of the material plate is dispersed (averaged) as an index for uniformly dispersing the crystal orientation of the product plate. Further, in Patent Document 3, among various crystal orientations in an aluminum alloy plate, the orientation density of S orientation crystal grains is 12 or more, and the orientation density of Cu orientation crystal grains is 10 or more. It has been proposed to improve surface properties by restricting to the above.
前述のように建材内外装用パネルや電気機器パネルなどの用途においては、表面品質が優れていることが要求され、特にエッチング等の表面処理が施されるのが通常であることから、表面処理性が良好で、表面処理後の表面にムラやストリークス等の外観欠陥が生じないことが望まれるが、従来の方法では、未だ確実かつ安定してこのような要求を満たすことは困難であった。 As described above, in applications such as building interior / exterior panels and electrical equipment panels, surface quality is required to be excellent, and surface treatment such as etching is usually performed, so surface treatment properties It is desirable that appearance defects such as unevenness and streaks do not occur on the surface after the surface treatment, but it has been difficult to meet such requirements reliably and stably with the conventional method. .
例えば特許文献1の提案では、熱間圧延条件の最適化によって、ある程度は表面処理後の外観を良好にすることは可能ではあるが、実際には全てのプロセスで確実かつ安定して表面処理性の良好な板が得られるとは限らず、特に熱間圧延後に(あるいはその後の中間焼鈍の中途において)中間焼鈍を行なわずに、最終冷間圧延板で硬質板に仕上げるプロセスでは、表面処理性が劣ってしまう場合があることが本発明者等の実験によって確認されている。 For example, in the proposal of Patent Document 1, it is possible to improve the appearance after the surface treatment to some extent by optimizing the hot rolling conditions. It is not always possible to obtain a good quality plate, especially in the process of finishing to a hard plate with the final cold rolled plate without intermediate annealing after hot rolling (or in the middle of the subsequent intermediate annealing). Has been confirmed by experiments by the present inventors.
また特許文献2、特許文献3に示されるように結晶方位を制御する方法では、確かにある程度は表面処理後のムラ、ストリークスに対する改善効果は認めれるが、この場合も既に述べてような中間焼鈍を省略して硬質板に仕上げるプロセスに適用した場合には、確実かつ安定して表面処理性を向上させることは困難であった。 Further, as shown in Patent Document 2 and Patent Document 3, the method for controlling the crystal orientation certainly has an effect of improving the unevenness and streak after the surface treatment to some extent. When applied to the process of finishing to a hard plate by omitting annealing, it was difficult to improve the surface treatment property reliably and stably.
前述のように熱間圧延工程で自己再結晶させて、その後の中間焼鈍を省略した製造プロセスでは、中間焼鈍で再結晶させるプロセスと比較して、熱間圧延の各パスにおける温度や圧下量等の条件が、熱間圧延後の再結晶集合組織に大きな影響を与える。そしてこのような再結晶集合組織がその後の冷間圧延によって圧延集合組織に変化しても、当初の再結晶集合組織の影響が履歴として残り、表面処理性に大きな影響を与えてしまう。また一方、製品板に対する表面処理自体も、最近ではコスト低減のために工程や管理の省略が進んでおり、そのため表面処理後の表面性能も処理前の素板の影響を受けやすく、そこでエッチング等の表面処理の工程や条件が変わっても、安定してストリークスやムラが生じないことが望まれる。例えばエッチングにおいてコスト低減のために劣化液を使用してエッチング量が減少した場合でも、良好な表面品質が得られることが望まれる。 As described above, in the manufacturing process in which self-recrystallization is performed in the hot rolling process and subsequent intermediate annealing is omitted, the temperature and reduction amount in each pass of hot rolling are compared with the process of recrystallization by intermediate annealing. These conditions greatly affect the recrystallization texture after hot rolling. Even if such a recrystallized texture changes to a rolled texture by subsequent cold rolling, the influence of the initial recrystallized texture remains as a history, which greatly affects the surface processability. On the other hand, the surface treatment itself for the product plate has recently been omitted in order to reduce costs, so the surface performance after the surface treatment is also easily affected by the base plate before the treatment. Even if the surface treatment process and conditions are changed, it is desirable that streaks and unevenness do not occur stably. For example, it is desired that good surface quality can be obtained even when the etching amount is reduced by using a deteriorated liquid for cost reduction in etching.
しかしながら、従来の方法では、これらの点について充分な配慮がなされておらず、そのため常に確実かつ安定して表面処理性(特にエッチング性)に優れた表面処理用アルミニウム合金板が得られるとは限らないのが実情である。 However, the conventional method does not give sufficient consideration to these points, and therefore, it is not always possible to obtain an aluminum alloy plate for surface treatment that is reliable and stable and has excellent surface treatment properties (particularly etching properties). There is no actual situation.
この発明は以上の事情を背景としてなされたもので、JIS 1000番系のアルミニウム合金を素材とし、熱間圧延で自己再結晶させることによってその後の中間焼鈍を省略し、最終的に冷間圧延によって硬質板に仕上げる表面処理用アルミニウム合金板の製造において、常に確実かつ安定して表面処理性、特に化学的もしくは電気化学的エッチングによるエッチング性が優れており、表面処理後の外観にムラやストリーク(スジ)等の欠陥の少ない表面処理板を安定して得ることができるようにすることを課題としている。 This invention has been made against the background of the above circumstances. By using a JIS 1000 series aluminum alloy as a raw material, self-recrystallization by hot rolling eliminates subsequent intermediate annealing, and finally by cold rolling. In the manufacture of aluminum alloy plates for surface treatment that are finished into hard plates, the surface treatment properties, especially the etching properties by chemical or electrochemical etching, are always reliable and stable, and the appearance after surface treatment is uneven and streaks ( It is an object to be able to stably obtain a surface-treated plate with few defects such as stripes).
前述のような課題を解決するべく、本発明者等が種々実験・検討を重ねた結果、熱間圧延における最終パスからその数パス前までの各パスにおける歪の蓄積を適切に制御することによって、熱間圧延後の再結晶を安定して制御できることを見出し、特に熱間圧延における最終パスからその2パス前までの各パス(仕上げ3パス)において、熱間歪の蓄積の指標となるZ値(Zener−Hollomon Parameter)を、各パスの圧延開始温度との関係のもとに適切に規制することが、最終的に表面処理性に優れたアルミニウム合金板を確実かつ安定して得るために有効であることを新規に知見し、この発明をなすに至ったのである。 As a result of repeated experiments and studies by the present inventors in order to solve the problems as described above, by appropriately controlling the accumulation of strain in each pass from the final pass in hot rolling to several passes before , It is found that recrystallization after hot rolling can be controlled stably, and in particular, Z that is an index of accumulation of hot strain in each pass from the final pass to 2 passes before the hot pass (finishing 3 passes). Appropriately regulating the value (Zener-Holomon Parameter) based on the relationship with the rolling start temperature of each pass in order to reliably and stably obtain an aluminum alloy sheet excellent in surface treatment It was newly discovered that it was effective, and this invention was made.
具体的には、請求項1の表面処理用アルミニウム合金板の製造方法は、JIS 1000番系のアルミニウム合金鋳塊について、400〜610℃の範囲内の温度に加熱して熱間圧延を開始し、かつその熱間圧延の各パスのうち、上り3パスについては、各パスにおける圧延開始温度Tを280〜480℃の範囲内とするとともに、各パスにおけるLn(Z)値(注:ZはZener−Hollomon Parameterを示す)が、それぞれのパスの圧延開始温度T(℃)に応じて、次式
−0.0645×T+55.5≦Ln(Z)≦−0.0645×T+59.5
を満たすように圧延を行なって、270〜370℃の範囲内の温度で熱間圧延を終了させ、板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分の組織が、平均結晶粒径100μm以下の再結晶組織となっている熱間圧延上り板を得、その後冷間圧延を施すことを特徴とするものである。
Specifically, in the method for producing a surface-treated aluminum alloy sheet according to claim 1, hot rolling is started by heating a JIS 1000 series aluminum alloy ingot to a temperature within a range of 400 to 610 ° C. And, for each of the three passes of the hot rolling, for the up three passes, the rolling start temperature T in each pass is within the range of 280 to 480 ° C., and the Ln (Z) value in each pass (Note: Z is Zener-Holomon Parameter) represents the following formula −0.0645 × T + 55.5 ≦ Ln (Z) ≦ −0.0645 × T + 59.5 depending on the rolling start temperature T (° C.) of each pass.
The rolling is performed so as to satisfy the conditions, the hot rolling is finished at a temperature within the range of 270 to 370 ° C., and the structure of the portion from the surface of the plate to the position of at least 30% of the plate thickness in the thickness direction of the plate is A hot rolled up board having a recrystallized structure with an average crystal grain size of 100 μm or less is obtained, and then cold rolled.
この発明の表面処理用アルミニウム合金板の製造方法によれば、JIS 1000番系のアルミニウム合金を素材として、熱間圧延において自己焼鈍により再結晶させることにより、その後の中間焼鈍を省略し、最終的に冷間圧延により硬質板に仕上げるにあたり、熱間圧延における最終パスからその2パス前までの3パス(上がり3パス)における熱間歪の蓄積を、各パスでの熱間圧延開始温度との関係の下で適切に規制することによって、熱間圧延後の結晶サイズ、結晶方位密度分布を狭い範囲内に安定的に制御することができ、その結果、最終冷間圧延によって硬質板に仕上げられた製品板に対して、化学的もしくは電気化学的エッチング等の表面処理を施すにあたっても、安定して良好な表面処理性を得て、エッチング等の表面処理後の表面外観としてムラやストリーク(スジ)などの外観欠陥のない表面品質の良好な板を、確実かつ安定して得ることができる。したがって例えば建材パネル等の外観の色調が均一であることが要求される用途においても、色調のムラのないパネル等を提供することができ、また装飾用としても優れた製品を提供できるなど、種々の要求に応えることができ、また表面処理の工程や条件が変わっても安定して良好な表面品質を有する製品を提供することができる。 According to the method of manufacturing an aluminum alloy plate for surface treatment of the present invention, by using JIS 1000 series aluminum alloy as a raw material and recrystallizing by self-annealing in hot rolling, the subsequent intermediate annealing is omitted. In addition, when finishing into a hard plate by cold rolling, accumulation of hot strain in three passes (upward three passes) from the final pass in hot rolling to two passes before it is calculated as the hot rolling start temperature in each pass. By appropriately regulating under the relationship, the crystal size and crystal orientation density distribution after hot rolling can be stably controlled within a narrow range, and as a result, it is finished into a hard plate by final cold rolling. Even when surface treatment such as chemical or electrochemical etching is applied to the product plate, surface treatment such as etching is obtained stably. Can be a good plate appearance defect-free surface quality, such as unevenness or streaks (streaks) as a surface appearance, can reliably and stably. Therefore, for example, even in applications that require a uniform external color tone, such as building material panels, it is possible to provide a panel with no uneven color tone, and to provide excellent products for decoration. In addition, it is possible to provide a product having stable and good surface quality even if the surface treatment process and conditions are changed.
この発明の方法においては、素材となるアルミニウム合金として、いわゆる純アルミニウム系であるJIS 1000番系のアルミニウム合金を用いる。JIS 1000番系のアルミニウム合金は、表面処理性が優れていて、エッチング等の表面処理後の表面外観が優れているため、この発明ではJIS 1000番系合金を用いることした。ここで、この発明の方法で熱間圧延条件として規定しているLn(Z)値は、変形応力に依存するが、JIS 1000番系以外の合金で積極添加されているMg、Mn、Si、Cu等の合金元素は、単独で1%程度でも添加されれば、晶出物あるいは析出物を生成して、変形応力に影響を及ぼし、ひいてはLn(Z)値に影響を与えてその制御を困難にしてしまうが、JIS 1000番系で規定している程度の含有量であれば、晶出物や生成物の生成も少なく、そのためLn(Z)値を容易かつ適切に制御して、所期の目的を達成することができ、したがってこの点からもJIS 1000番系の合金を用いることが適切である。 In the method of the present invention, a JIS 1000 series aluminum alloy which is a so-called pure aluminum series is used as an aluminum alloy as a material. Since the JIS 1000 series aluminum alloy is excellent in surface treatment property and the surface appearance after the surface treatment such as etching is excellent, in this invention, the JIS 1000 series alloy was used. Here, the Ln (Z) value defined as the hot rolling condition in the method of the present invention depends on the deformation stress, but Mg, Mn, Si, which are positively added in alloys other than JIS 1000 series, If an alloying element such as Cu is added alone even at about 1%, a crystallized product or a precipitate is generated, affecting the deformation stress, and thus affecting the Ln (Z) value. Although it is difficult, if the content is as specified in the JIS 1000 series, there is little formation of crystallized products and products, so the Ln (Z) value can be controlled easily and appropriately. Therefore, it is appropriate to use a JIS 1000 series alloy in this respect as well.
次にこの発明の製造方法について説明する。 Next, the manufacturing method of this invention is demonstrated.
先ず前述のようにJIS 1000番系の合金について、DC鋳造法などの常法に従って鋳造し、鋳塊(スラブ)を得る。鋳塊に対しては、必要に応じて均質化処理を行なってから熱間圧延を行なう。均質化処理を行なう場合の均質化処理条件は特に限定しないが、通常は500〜600℃で1〜10時間程度とする。また均質化処理を行なう場合、均質化処理後に一旦室温まで冷却してから熱間圧延開始温度まで再加熱して熱間圧延を行なっても、あるいは均質化処理後、熱間圧延温度まで冷却して直ちに熱間圧延を行なっても良い。 First, as described above, a JIS 1000 series alloy is cast according to a conventional method such as a DC casting method to obtain an ingot (slab). The ingot is subjected to a homogenization treatment as necessary and then hot-rolled. The homogenization treatment conditions for performing the homogenization treatment are not particularly limited, but are usually 500 to 600 ° C. for about 1 to 10 hours. In addition, when performing homogenization treatment, it may be cooled to room temperature after homogenization treatment and then re-heated to hot rolling start temperature to perform hot rolling, or after homogenization treatment, it may be cooled to hot rolling temperature. Hot rolling may be performed immediately.
熱間圧延の条件は、この発明の方法では極めて重要であり、これを適切かつ厳密に制御することによって、エッチング性等の表面処理性が優れた製品板を安定して得ることが可能となる。 The hot rolling conditions are extremely important in the method of the present invention, and by appropriately and strictly controlling this, it becomes possible to stably obtain a product plate having excellent surface treatment properties such as etching properties. .
この熱間圧延においては、後に改めて説明するように、少なくとも一回は再結晶させて、熱間圧延終了後に少なくとも表層部が微細な再結晶組織となっているように制御することが必要であり、主としてこれらの観点から熱間圧延開始温度を400〜610℃の範囲内に定め、また熱間圧延終了温度を270〜370℃の範囲内に定めている。 In this hot rolling, as will be described later, it is necessary to recrystallize at least once and control so that at least the surface layer portion has a fine recrystallized structure after the hot rolling is completed. From these viewpoints, the hot rolling start temperature is set within a range of 400 to 610 ° C., and the hot rolling end temperature is set within a range of 270 to 370 ° C.
すなわち、先ず熱間圧延開始温度が400℃未満では、熱間圧延中に再結晶が生じにくくなって、製品板の表面処理後の表面にストリークスが発生しやすくなり、また熱間圧延を270℃以上の高温度域で終了させることが困難となる。一方熱間圧延開始温度が610℃を越えれば、熱間圧延中途で鋳塊の前後端のワニ口部切断等で圧延が中断された場合等において、再結晶粒の粗大化(板厚方向で粒径100μmを越える粗大化)を招くおそれが強くなる。ここで、熱間圧延における比較的初期の粗圧延等において生じた再結晶粒は、母結晶粒としてその後の熱間圧延過程で生成される組織の元となり、このような母結晶粒の大きさも熱間圧延終了時の再結晶組織の粒径に影響を与えるから、熱間圧延の比較的初期の粗圧延等における再結晶粒の粗大化も抑制しておく必要がある。そこでこの発明では熱間圧延の開始温度は400〜610℃の範囲内とした。 That is, when the hot rolling start temperature is less than 400 ° C., recrystallization hardly occurs during hot rolling, streaks are likely to occur on the surface after the surface treatment of the product plate, and hot rolling is performed at 270. It becomes difficult to complete the process at a high temperature range of ℃ or higher. On the other hand, if the hot rolling start temperature exceeds 610 ° C., the rolling of the recrystallized grains becomes coarse (in the thickness direction) in the case where the rolling is interrupted by cutting the crocodile mouth at the front and rear ends of the ingot during the hot rolling. There is a strong risk of causing a coarsening exceeding the particle size of 100 μm. Here, the recrystallized grains generated in the relatively early rough rolling in the hot rolling are the basis of the structure generated in the subsequent hot rolling process as the mother crystal grains, and the size of such mother crystal grains is also Since it affects the grain size of the recrystallized structure at the end of hot rolling, it is necessary to suppress the coarsening of recrystallized grains in the relatively early rough rolling of hot rolling. Therefore, in the present invention, the hot rolling start temperature is in the range of 400 to 610 ° C.
一方、この発明の方法においては、熱間圧延終了時(熱間圧延を終了させてコイル状に巻上げ、室温まで冷却させた時点)において、板の表面から板厚方向へ少なくとも30%の位置までの部分の組織が、平均粒径100μm以下の再結晶粒からなる再結晶組織となっていることが必要である。熱間圧延終了温度(最終パス上がり温度)が270℃未満の場合は、この発明で規定するLn(Z)の条件では歪の蓄積が不足し、板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分まで安定して再結晶させることが困難となる。熱間圧延終了温度を270℃以上に規制すれば、板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分まで安定して再結晶させることが可能となるが、熱間圧延終了温度が370℃を越えれば、コイルに巻取ってからも再結晶が成長して再結晶粒が100μmを越えてしまうおそれがある。そこで熱間圧延終了温度は270〜370℃の範囲内とした。 On the other hand, in the method of the present invention, at the end of hot rolling (when hot rolling is finished, coiled and cooled to room temperature), at least 30% in the thickness direction from the surface of the plate. It is necessary that the structure of this part is a recrystallized structure composed of recrystallized grains having an average particle size of 100 μm or less. When the hot rolling finish temperature (final pass rising temperature) is less than 270 ° C., the accumulation of strain is insufficient under the condition of Ln (Z) defined in the present invention, and the thickness of the plate extends from the surface of the plate to the thickness direction of the plate. It becomes difficult to stably recrystallize up to a portion of at least 30% . If the hot rolling end temperature is regulated to 270 ° C. or higher, it is possible to stably recrystallize from the surface of the plate to the position of at least 30% of the plate thickness in the thickness direction of the plate. If the rolling end temperature exceeds 370 ° C., the recrystallized grains may grow after winding on the coil, and the recrystallized grains may exceed 100 μm. Therefore, the hot rolling end temperature is set in the range of 270 to 370 ° C.
なおここで熱間圧延終了後(コイル巻取−冷却後)の熱間圧延板の組織として、その板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分の再結晶粒径が100μmを越えていれば、製品板の肌荒れの原因となり、良好な表面品質が得られなくなる。また、熱間圧延板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分が完全な再結晶組織となっていない場合(その30%の範囲内の部分の少なくとも一部が未再結晶組織である場合)には、この発明の最終目的である表面処理性の確実かつ安定した向上を図れなくなる。 Here, as the structure of the hot rolled sheet after completion of hot rolling (after coil winding and cooling), the recrystallized grains in the portion from the surface of the sheet to the position of at least 30% of the sheet thickness in the thickness direction of the sheet If the diameter exceeds 100 μm, it may cause rough skin of the product plate, and good surface quality cannot be obtained. Further, when the portion from the surface of the hot rolled plate to the position of at least 30% of the plate thickness in the thickness direction of the plate is not a complete recrystallized structure (at least part of the portion within the 30% range is In the case of an unrecrystallized structure), the surface treatment property, which is the final object of the present invention, cannot be improved reliably and stably.
さらにこの発明の方法においては、熱間圧延の開始温度、終了温度を前述のように規制するばかりでなく、熱間圧延の上がり3パスの各パスにおける歪速度と温度の関係を適切に規制することが重要である。この点について以下に説明する。 Furthermore, in the method of the present invention, not only the hot rolling start temperature and end temperature are regulated as described above, but also the relationship between the strain rate and temperature in each of the three passes of hot rolling is appropriately regulated. This is very important. This will be described below.
熱間圧延は、一般に前段としての板圧延(プレート圧延)による粗圧延と、後段としてのコイル圧延による仕上げ圧延とによって行なうのが通常である。一方熱間圧延の終了板厚は、製品の要求性能や用途によって異なるが、通常は2〜10mm程度の板厚に仕上げられることが多い。ここで、1パスで圧延可能な最大の圧下率は、板厚によっても異なるが、コーティング等の問題により85%程度が限界とされている。そこで熱間圧延の仕上げ圧延は、通常は3パス以上の複数のパスで行なう。なおここで、1回のパスとは、多段式連続圧延機により複数段のパスで仕上圧延する場合の各段のパスをも指称することとする。 In general, hot rolling is generally performed by rough rolling by plate rolling (plate rolling) as the former stage and finish rolling by coil rolling as the latter stage. On the other hand, the finished thickness of hot rolling varies depending on the required performance and application of the product, but is usually usually finished to a thickness of about 2 to 10 mm. Here, the maximum rolling reduction that can be rolled in one pass varies depending on the plate thickness, but is limited to about 85% due to problems such as coating. Therefore, the hot rolling finish rolling is usually performed in a plurality of passes of 3 passes or more. In addition, suppose here that the pass of 1 step | paragraph also refers to the pass | pass of each stage | paragraph in the case of carrying out finish rolling by a multistage | paragraph pass with a multistage continuous rolling mill.
上述のような仕上圧延における各パスの圧延での歪速度と温度との関係に着目して本発明者が詳細な実験・検討を重ねた結果、少なくとも最終パスを含む上がり3パスの圧延を、熱間歪蓄積の指標となるZener−Hollomon Parameter(Z値)と、各パスでの圧延開始温度との間の関係が特定の範囲内となるように制御することが、熱間圧延上がりの組織制御に重要であることを認めて見出したのである。すなわちこの発明の方法では、熱間圧延工程の上がり3パスの各パスにおける歪蓄積と回復・再結晶を適切に制御するため、上がり3パスの各パスにおける圧延開始温度Tを280〜480℃の範囲内として、Zn値の自然対数値Ln(Z)と圧延開始温度T(℃)との間に、次の(1)式
−0.0645×T+55.5≦Ln(Z)≦−0.0645×T+59.5
・・・(1)
が満たされるように圧延を行なうこととした。このようなLn(Z)値と熱間圧延開始温度T(℃)との関係を、図1に示す。図1において斜線部分が(1)式の条件を満たす範囲である。
As a result of repeated detailed experiments and examinations by the present inventors paying attention to the relationship between the strain rate and temperature in rolling of each pass in finish rolling as described above, at least three passes of rolling including the final pass, It is possible to control the relationship between the Zener-Holomon Parameter (Z value), which is an index of hot strain accumulation, and the rolling start temperature in each pass to be within a specific range. They found it important to control. That is, in the method of the present invention, in order to appropriately control strain accumulation and recovery / recrystallization in each of the three passes in the hot rolling process, the rolling start temperature T in each of the three passes in the hot rolling process is 280 to 480 ° C. Within the range, between the natural logarithm value Ln (Z) of the Zn value and the rolling start temperature T (° C.), the following equation (1) −0.0645 × T + 55.5 ≦ Ln (Z) ≦ −0. 0645 × T + 59.5
... (1)
It was decided to perform rolling so that The relationship between such Ln (Z) value and hot rolling start temperature T (° C.) is shown in FIG. In FIG. 1, the shaded area is a range that satisfies the condition of the expression (1).
ここで、熱間圧延を最終的に270℃以上で終了させるためには、上がり3パスの各パスにおける圧延開始温度Tを280℃以上とすることが必要である。一方上がり3パスの各パスにおける圧延開始温度Tが480℃を越える場合、上記(1)式を満たすと同時に熱間圧延終了温度を370℃以下とすることが困難となってしまう。そこで上がり3パスにおける各パスでの圧延開始温度は280〜480℃の範囲内とした。 Here, in order to finally terminate the hot rolling at 270 ° C. or higher, it is necessary to set the rolling start temperature T in each of the three passes to be 280 ° C. or higher. On the other hand, when the rolling start temperature T in each pass of three passes exceeds 480 ° C., it becomes difficult to satisfy the above formula (1) and to set the hot rolling end temperature to 370 ° C. or less. Therefore, the rolling start temperature in each pass in three passes is set in the range of 280 to 480 ° C.
一方、上がり3パスのいずれか1以上のパスにおいて前記(1)式の左辺が満たされない場合、すなわちLn(Z)値が−0.0645×T+55.5未満の場合には、1パスごとに回復が生じてしまい、一旦は再結晶した粒がそのまま成長してしまって、100μmを越える粗大な再結晶粒が生成されてしまうのみならず、1パスごとの回復の程度も不安定となるため、結晶方位の分布や密度が安定せず、その結果製品板に対してエッチングを施した際のエッチングムラ発生の原因となる。 On the other hand, when the left side of the above equation (1) is not satisfied in any one or more of the three rising paths, that is, when the Ln (Z) value is less than −0.0645 × T + 55.5, each path Recovery occurs, and once recrystallized grains grow as they are, not only coarse recrystallized grains exceeding 100 μm are generated, but also the degree of recovery for each pass becomes unstable. As a result, the distribution and density of crystal orientation are not stable, and as a result, etching unevenness occurs when the product plate is etched.
一方、上がり3パスのいずれか1以上のパスにおいて前記(1)式の右辺が満たされない場合、すなわちLn(Z)の値が−0.0645×T+59.5を越える場合には、1パスごとの歪の蓄積は充分となるが、最終パス(パス数をNとすれば、第N番目のパス;以下単に“Nパス”と記す)より1パス前のパス(以下“N−1パス”と記す)および最終パスより2パス前のパス(以下“N−2パス”と記す)の各パスにおいて、表面に不均一な再結晶が生じる。このとき再結晶した部分と未再結晶であった部分とでは、Nパス目で再度再結晶する際に、結晶粒の大きさが異なってしまうため、最終的に製品板にエッチングを施した際に梨地のようなムラが生じたり、またエッチング条件によっては、圧延方向で似通った結晶方位が揃ってしまうことに起因してスジ状の模様が発生して、外観品質を損なう。したがって熱間圧延の上がり3パスの各パスにおいては、Ln(Z)値と圧延開始温度T(℃)との間の関係が前記(1)式を満たすことが必要である。 On the other hand, when the right side of the above equation (1) is not satisfied in any one or more of the three rising paths, that is, when the value of Ln (Z) exceeds −0.0645 × T + 59.5, every one path Is sufficient, but a path one pass before the final pass (if the number of passes is N, the Nth pass; hereinafter simply referred to as “N pass”) (hereinafter “N−1 pass”). ) And two passes before the final pass (hereinafter referred to as “N-2 pass”), non-uniform recrystallization occurs on the surface. At this time, when the recrystallized portion and the non-recrystallized portion are recrystallized again at the Nth pass, the size of the crystal grains is different, so when the product plate is finally etched. Depending on the etching conditions, stripe-like patterns are generated depending on the etching conditions, and the appearance quality is deteriorated. Therefore, in each of the three passes after the hot rolling, it is necessary that the relationship between the Ln (Z) value and the rolling start temperature T (° C.) satisfy the above formula (1).
なおここでZ値は、例えば文献(アルミニウム材料の基礎と工業技術(昭和60年5月1日、社団法人軽金属協会発行)の第88頁〜第89頁に示されているように、熱間歪蓄積の指標となるZener−Hollomon Parameter(単位:/秒)を意味し、歪速度をE、活性化エネルギをQ、気体定数をR、温度をTとすれば、次の(2)式
Z=E・exp(Q/RT) ・・・(2)
で求められる値である。
Here, the Z value is, for example, as shown in pages 88 to 89 of the literature (aluminum material basics and industrial technology (issued by the Japan Light Metals Association, May 1, 1985). This means Zener-Holomon Parameter (unit: / second) that is an index of strain accumulation. If strain rate is E, activation energy is Q, gas constant is R, and temperature is T, the following equation (2) Z = E · exp (Q / RT) (2)
This is the value obtained by.
なおこの発明においてZ値の計算にあたっては、活性化エネルギQの値として37,300cal/molの値を用い、気体定数Rとして1.987cal/mol・Kの値を用いた。 In the present invention, in calculating the Z value, a value of 37,300 cal / mol was used as the value of the activation energy Q, and a value of 1.987 cal / mol · K was used as the gas constant R.
以上のように、熱間圧延の開始温度、終了温度を規制するだけではなく、特に熱間圧延上がりの3パスの条件を制御することによって、最終的な製品板の組織制御を行なっており、このような熱間圧延の制御による効果を維持するため、この発明の方法では、熱間圧延後は冷間圧延のみにより製品板とすることとしている。すなわち、熱間圧延後や冷間圧延の中途で、再結晶のための中間焼鈍を改めて行なわないこととしている。なお、冷間圧延の条件は特に限定しないが、通常は最終的にH18〜H24程度の硬質板とするため、20〜97%程度の圧延率で最終冷間圧延を行なえば良い。 As described above, not only the start temperature and end temperature of hot rolling are regulated, but also the structure of the final product plate is controlled by controlling the conditions of the three passes especially after hot rolling, In order to maintain the effect by such control of hot rolling, in the method of the present invention, after hot rolling, a product plate is formed only by cold rolling. That is, intermediate annealing for recrystallization is not performed again after hot rolling or during cold rolling. In addition, although the conditions of cold rolling are not specifically limited, in order to make it finally a hard plate of about H18 to H24, the final cold rolling may be performed at a rolling rate of about 20 to 97%.
表1に示すAおよびBの合金を常法に従って溶製し、DC鋳造法により厚み550mmのスラブに鋳造した。 Alloys A and B shown in Table 1 were melted in accordance with a conventional method, and cast into a slab having a thickness of 550 mm by a DC casting method.
得られたスラブに対して560℃の温度で2時間保持の均質化処理を行なった後、室温まで放冷した。その後圧延面を片面当たり10mmずつ面削した後、460℃まで加熱して2時間加熱した後に熱間圧延を開始した。熱間圧延は1パスあたり10〜900m/minの圧延速度となるような条件で終了板厚2〜5mmまで実施した。熱間圧延後は中間焼鈍を施すことなく板厚0.4mmまで冷間圧延を行ない、硬質材の製品板として仕上げ、外観を評価した。なおここで熱間圧延終了板厚が異なるのは、製品板厚が同じでも要求される機械的性質が異なるために冷間圧延率で調整を行なったためである。 The obtained slab was homogenized by holding at 560 ° C. for 2 hours, and then allowed to cool to room temperature. Thereafter, the rolled surface was chamfered by 10 mm per side, heated to 460 ° C. and heated for 2 hours, and then hot rolling was started. The hot rolling was performed up to an end plate thickness of 2 to 5 mm under conditions such that the rolling speed was 10 to 900 m / min per pass. After hot rolling, it was cold-rolled to a sheet thickness of 0.4 mm without intermediate annealing, finished as a hard product plate, and evaluated for appearance. The reason why the hot-rolling finished sheet thickness is different is that the adjustment is made by the cold rolling rate because the required mechanical properties are different even if the product sheet thickness is the same.
この発明の方法において製品板の表面処理後の外観品質は、熱間圧延終了前の上がり3パスを如何なる条件にて行なうかで決定される。そこでこの実施例では、上がり3パスの各パスの開始時の材料温度および熱間圧延終了時の材料温度(上がり温度)、および各パス開始板厚での歪速度E、およびLn(Z)値を調べた。その結果を表2、表3に示す。 In the method of the present invention, the appearance quality after the surface treatment of the product plate is determined by the conditions under which three passes of rising before the end of hot rolling are performed. In this embodiment, therefore, the material temperature at the start of each of the three passes, the material temperature at the end of hot rolling (rise temperature), and the strain rate E and Ln (Z) value at each pass starting plate thickness. I investigated. The results are shown in Tables 2 and 3.
また製造番号1〜5の場合について、上がり3パスの各パスにおけるLn(Z)値と圧延開始温度T(℃)を、図1に倣って図2に示し、また製造番号6〜10の場合について同様に図3に示した。 Moreover, about the case of manufacturing numbers 1-5, the Ln (Z) value and rolling start temperature T (degreeC) in each pass of 3 going up are shown in FIG. 2 according to FIG. 1, and the case of manufacturing numbers 6-10 The same is shown in FIG.
以上の過程において、熱間圧延上がり板の表面について、平均結晶粒径の測定を行なった。ここで、実際に表面処理して使用される場合に外観に影響を及ぼすのは板のごく表面である。そこで研磨をなるべく少なくするため、バフで5μm程度(圧延目が消える程度)に研磨した後、電解研磨で仕上げ、研磨後にバーカー氏液による陽極酸化処理を施し、その後に偏光顕微鏡により表面を観察して、結晶粒を測定した。測定は写真上で切断法により圧延方向と垂直な方向に引いた線を横切る粒界の数を数えて平均粒径を求め、表4中に示した。 In the above process, the average crystal grain size was measured for the surface of the hot rolled plate. Here, it is the very surface of the plate that affects the appearance when it is actually surface-treated. Therefore, in order to reduce polishing as much as possible, it is polished to about 5 μm with buff (to the extent that the rolling marks disappear), then finished by electrolytic polishing, and after polishing, anodized with Barker's solution, and then the surface is observed with a polarizing microscope. The crystal grains were measured. The measurement was performed by counting the number of grain boundaries crossing a line drawn in the direction perpendicular to the rolling direction by a cutting method on the photograph, and the average grain size was determined and shown in Table 4.
また、熱間圧延上がり板について、Cu方位とS方位の結晶方位分布密度の測定を板の表面で行なった。方位密度の分布の測定は、リガク(株)のX線回折装置を用い、{200}、{220}、{111}の不完全極点図を作成し、これらを元にODF(三次元結晶方位解析)を行なって調べた。なおこれらの解析においては、アルミニウム粉末から作られたランダム方位を持つ試料を測定して得られたデータを{200}、{220}、{111}の不完全極点図解析の際に使う規格化ファイルとし、これによりランダム方位を持つ試料に対する倍数としてCuおよびS方位密度、すなわち{112}<111>および{123}<634>方位の密度を求め、その結果を表4中に示した。 Moreover, about the hot rolled up board, the crystal orientation distribution density of Cu orientation and S orientation was measured on the surface of the board. The distribution of orientation density is measured by using an X-ray diffractometer manufactured by Rigaku Corporation to create incomplete pole figures of {200}, {220}, {111}, and ODF (three-dimensional crystal orientation) based on them. Analysis). In these analyses, data obtained by measuring a sample having a random orientation made from aluminum powder is normalized for use in incomplete pole figure analysis of {200}, {220}, and {111}. As a file, the Cu and S azimuth densities, ie, {112} <111> and {123} <634> azimuth densities, were obtained as multiples of the samples having random orientations, and the results are shown in Table 4.
また、最終的に得られた冷間圧延板について、その表面処理性を調べた。ここで表面処理性は、冷間圧延板の表面を、エッチング液として純水(500ml)+塩酸(500ml)+硝酸(500ml)+フッ酸(5ml)の混合液を用いてマクロエッチングし、スジやムラの有無を目視により評価した。評価手法としては、目視でムラおよびスジの発生がともにない場合を合格(○印)、ムラがあった場合を不合格(△印)とし、またスジが生じた場合も不合格(×印)と評価し、その結果を表3中に示した。 Moreover, the surface treatment property was investigated about the finally obtained cold rolled sheet. Here, the surface treatment property is obtained by macro-etching the surface of the cold rolled plate using a mixed solution of pure water (500 ml) + hydrochloric acid (500 ml) + nitric acid (500 ml) + hydrofluoric acid (5 ml) as an etching solution. The presence or absence of unevenness was visually evaluated. As an evaluation method, a case where neither unevenness nor streaks are visually observed is acceptable (◯ mark), a case where unevenness is present is rejected (△ mark), and a case where a streak occurs is also rejected (× mark). The results are shown in Table 3.
製造番号1〜5は、いずれもこの発明で規定する範囲内の条件で圧延したものであり、これらの場合はいずれもエッチング後の表面にスジやムラがないことが判明した。そしてこれらのうち、製造番号1の場合は、平均結晶粒径は80μmとやや大きめだが、S方位、Cu方位が充分に成長していることから、バランス良くエッチングされた。また製造番号2〜4の場合は、S方位が発達しており、良いエッチング特性を示した。さらに製造番号5の場合は、S方位、Cu方位の発達はやや低いものの結晶粒径を細かくすることができ、それにより安定したエッチング特性を示した。 Production numbers 1 to 5 were all rolled under the conditions specified in the present invention, and in these cases, it was found that there were no streaks or unevenness on the surface after etching. Of these, in the case of production number 1, the average crystal grain size was slightly large at 80 μm, but the S orientation and the Cu orientation were sufficiently grown, so that the etching was performed with a good balance. In the case of production numbers 2 to 4, the S orientation was developed and showed good etching characteristics. Further, in the case of production number 5, although the development of the S orientation and the Cu orientation was somewhat low, the crystal grain size could be made finer, thereby showing stable etching characteristics.
一方、製造番号6〜10の例は、いずれかの条件がこの発明で規定する範囲を外れたものでありこれらの場合にはエッチング後の表面にムラもしくはスジが発生してしまった。すなわち、先ず製造番号6の比較例では、S方位およびCu方位がそれなりに発達していたが、Z値の高い領域からN−2パス目の圧延が開始されたことと、その際の温度が422℃以上と高かったことにより、N−1パス目の開始時に一度部分再結晶した模様で、その影響と思われるスジ状のムラが観察された。 On the other hand, in the examples of production numbers 6 to 10, one of the conditions was outside the range defined in the present invention, and in these cases, unevenness or streaks occurred on the surface after etching. That is, first, in the comparative example of production number 6, the S orientation and the Cu orientation were developed as such, but the N-2 pass rolling was started from the region where the Z value was high, and the temperature at that time was Due to the high temperature of 422 ° C. or higher, streak-like unevenness that seems to be the effect was observed in the pattern that was partially recrystallized once at the start of the N-1th pass.
また製造番号7の例は、Z値の低い領域で圧延してなるべく細かい結晶粒となることを狙ったが、Z値が低過ぎたため、368℃と高い温度で熱間圧延を終了したにもかかわらず、エッチング後に強いスジがあらわれてしまった。なおこの製造番号7の例について、熱間圧延板の断面のミクロ組織を観察したところ、図4に示すように再結晶したのはごくわずかな表面だけであって、大部分は未再結晶の組織となっていることが判明した。さらに製造番号8の例は、製造番号7の例の失敗に基づき、なるべくZ値が高くなる条件で圧延を行なった。この例では、結晶方位密度はS方位が18、Cu方位が12とかなり発達しており、比較的均一にエッチングされそうに思われたが、結晶粒が平均で105μmと粗大なため、最終板でも結晶粒が粗大となり、結晶粒ごとのエッチング速度のわずかな差が凹凸としてあらわれ、エッチング後の表面のムラがひどくなってしまった。そしてまた製造番号9の例も、微細粒を狙ってなるべく低いZ値の領域で圧延を実施したが、熱間圧延板の断面ミクロ組織は、図5に示すように全厚未再結晶となり、エッチング後の表面にスジが発生した。さらに製造番号10の例は、バランス良く圧延できたが、熱間圧延終了温度(上がり温度)が265℃と低く、そのため図6に示すように、熱間圧延板の断面のミクロ組織で部分的にのみ再結晶するような組織となってしまい、エッチング後の表面にスジが生じてしまった。 Moreover, although the example of the production number 7 aimed at rolling in the area | region with a low Z value and became as fine a crystal grain as possible, since the Z value was too low, even if hot rolling was complete | finished at 368 degreeC and high temperature, Regardless, a strong streak appeared after etching. As for the example of production number 7, the microstructure of the cross section of the hot-rolled sheet was observed. As shown in FIG. 4, only a very small surface was recrystallized, and the majority was unrecrystallized. It turned out to be an organization. Further, in the example of production number 8, rolling was performed under the condition that the Z value was as high as possible based on the failure of the example of production number 7. In this example, the crystal orientation density was considerably developed with the S orientation of 18 and the Cu orientation of 12, which seemed to be etched relatively uniformly. However, since the average grain size was 105 μm, the final plate However, the crystal grains became coarse, and a slight difference in the etching rate for each crystal grain appeared as irregularities, resulting in severe unevenness of the surface after etching. And the example of production number 9 was also rolled in the region of the Z value as low as possible aiming for fine grains, the cross-sectional microstructure of the hot-rolled sheet became full thickness unrecrystallized as shown in FIG. Streaks occurred on the surface after etching. Furthermore, although the example of production number 10 was able to be rolled with good balance, the hot rolling finish temperature (rising temperature) was as low as 265 ° C. Therefore, as shown in FIG. 6, it was partially in the microstructure of the cross section of the hot rolled plate. This resulted in a structure that recrystallized only on the surface, and streaks were formed on the surface after etching.
Claims (1)
−0.0645×T+55.5≦Ln(Z)≦−0.0645×T+59.5
を満たすように圧延を行なって、270〜370℃の範囲内の温度で熱間圧延を終了させ、板の表面から板の厚み方向に板厚の少なくとも30%の位置までの部分の組織が、平均結晶粒径100μm以下の再結晶組織となっている熱間圧延上り板を得、その後冷間圧延を施すことを特徴とする、表面処理性に優れたアルミニウム合金板の製造方法。 About JIS 1000 series aluminum alloy ingot, it heats to the temperature within the range of 400-610 degreeC, and starts hot rolling, and, for each pass of uphill 3 passes among each pass of the hot rolling, each pass The rolling start temperature T in the range of 280 to 480 ° C., and the Ln (Z) value in each pass (Note: Z indicates Zener-Holomon Parameter) is the rolling start temperature T (° C.) of each pass. In accordance with the following formula: −0.0645 × T + 55.5 ≦ Ln (Z) ≦ −0.0645 × T + 59.5
The rolling is performed so as to satisfy the conditions, the hot rolling is finished at a temperature within the range of 270 to 370 ° C., and the structure of the portion from the surface of the plate to the position of at least 30% of the plate thickness in the thickness direction of the plate is A method for producing an aluminum alloy sheet excellent in surface treatability, characterized in that a hot rolled up board having a recrystallized structure with an average crystal grain size of 100 µm or less is obtained and then cold rolled.
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