JP5278494B2 - Method for producing 6000 series aluminum alloy plate excellent in paint bake hardenability - Google Patents
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本発明は、塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法に関し、特に、自動車ボディパネル等、成形加工ならびに塗装焼付け処理を施して用いられる、塗装焼付け硬化性に優れた６０００系アルミニウム合金板およびその製造方法に関するものである。 The present invention relates to a method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability, and in particular, a 6000 series aluminum excellent in paint bake hardenability, which is used after being subjected to forming processing and paint bake treatment, such as automobile body panels. The present invention relates to an alloy plate and a manufacturing method thereof.
近年、自動車の燃費向上を目的とした車体軽量化の要望が高まっており、軽量化手段の一つとして自動車ボディパネル等へのアルミニウム合金板が使用されている。熱処理型のＡｌ−Ｍｇ−Ｓｉ系合金（６０００系アルミニウム合金といい、単に、６０００系合金ともいう。）は、塗装焼付け工程の熱処理により降伏強度が上昇する性質（塗装焼付け硬化性という。）を有するため、板厚の薄肉化ひいては車体の軽量化に有利であり、ボディパネル材として使われることが多くなってきている。 In recent years, there has been an increasing demand for lighter vehicle bodies for the purpose of improving the fuel efficiency of automobiles, and aluminum alloy plates for automobile body panels and the like have been used as one of means for reducing the weight. A heat treatment type Al—Mg—Si alloy (referred to as a 6000 series aluminum alloy, also simply referred to as a 6000 series alloy) has a property of increasing the yield strength by heat treatment in a paint baking process (referred to as paint bake hardenability). Therefore, it is advantageous for reducing the thickness of the plate and thus reducing the weight of the vehicle body, and it is increasingly used as a body panel material.
従来、６０００系合金の塗装焼付け硬化性については、溶体化・焼入れ後に熱処理を加えることによって降伏強度を上昇させる方法が種々開示されている。 Conventionally, regarding the bake hardenability of 6000 series alloys, various methods for increasing the yield strength by applying a heat treatment after solution treatment and quenching have been disclosed.
例えば、特許文献１では、溶体化焼入れ処理後、７２時間以内に４０〜１２０℃の温度で８〜３６時間の最終熱処理を行う発明が開示されている。 For example, Patent Document 1 discloses an invention in which a final heat treatment is performed for 8 to 36 hours at a temperature of 40 to 120 ° C. within 72 hours after the solution hardening treatment.
また、特許文献２では、溶体化処理後室温以上の５０〜１３０℃に温度に焼き入れて、その温度に１〜４８時間の長時間熱処理を行った後、さらに１４０〜１８０℃の温度範囲で３〜１０分間の低温加熱処理を行う発明が開示されている。 Moreover, in patent document 2, after solution-treating, it hardens to the temperature of 50-130 degreeC more than room temperature, and after performing the long-time heat processing for 1 to 48 hours at that temperature, in the temperature range of 140-180 degreeC further. An invention for performing low-temperature heat treatment for 3 to 10 minutes is disclosed.
また、特許文献３でも、溶体化焼き入れ後６０分以内に４０〜１２０℃の温度で５０時間以上の熱処理を行う発明が開示されている。 Patent Document 3 also discloses an invention in which heat treatment is performed for 50 hours or more at a temperature of 40 to 120 ° C. within 60 minutes after solution hardening.
また、本系合金は製造工程中の溶体化処理をはじめとする高温下での処理によって、板表面にＭｇＯの濃化層が形成されることが知られている。自動車ボディの組み立てにおける接着工程において、板表面にＭｇＯ濃化層が存在すると、ＭｇＯ濃化層と下地のアルミとの結合が弱いために接着性が劣ってしまうという問題があった。また脱脂工程においても水濡れ性が悪くなるために均一な化成処理が行われず、その結果塗装後耐食性が劣化してしまうという問題もある。接着性や塗装後耐食性を向上させる必要が生じた場合は、この合金表面に形成されるＭｇＯ濃化層を除去することが行われる。その方法としては、酸に浸漬する方法（特許文献４）、アルカリ溶液に浸漬する方法（特許文献５）、ｐＨが５〜８の水溶液に浸漬する方法（特許文献６）が開示されている。しかし、いずれの方法も材質を造り込む工程とは別に表面調整のための上記処理を行うものであり、コスト増という問題があった。 In addition, it is known that a concentrated layer of MgO is formed on the surface of the present alloy by a treatment at a high temperature such as a solution treatment in the manufacturing process. In the bonding process in assembling an automobile body, if an MgO concentrated layer is present on the plate surface, the bond between the MgO concentrated layer and the underlying aluminum is weak, resulting in poor adhesion. Further, in the degreasing process, water wettability is deteriorated, so that a uniform chemical conversion treatment is not performed, and as a result, there is a problem that the corrosion resistance after coating is deteriorated. When it is necessary to improve adhesion and post-coating corrosion resistance, the MgO concentrated layer formed on the alloy surface is removed. As the method, a method of immersing in an acid (Patent Document 4), a method of immersing in an alkaline solution (Patent Document 5), and a method of immersing in an aqueous solution having a pH of 5 to 8 (Patent Document 6) are disclosed. However, each method performs the above-described treatment for surface adjustment separately from the step of building the material, and there is a problem of an increase in cost.
しかしながら、上記特許文献１〜３に記載の発明は、自動車ボディパネル用材料として塗装焼付け時に大きな強度上昇を図り、かつ板製造後から成形加工までの室温放置中の自然時効による強度上昇を抑えるためには、いずれの場合も溶体化処理以降に長時間の熱処理を行う必要があり、生産性を犠牲にして製造しなければならないという問題がある。自動車ボディパネル向けの６０００系アルミニウム合金の需要は近年増加しつつあり、今後のさらなる需要増加に対応していくためには生産性に優れた製造方法が必要とされるようになってきた。 However, the inventions described in the above-mentioned Patent Documents 1 to 3 are intended to greatly increase the strength when baking a paint as a material for an automobile body panel, and to suppress the increase in strength due to natural aging during standing at room temperature from the production of the plate to the molding process However, in any case, it is necessary to perform heat treatment for a long time after the solution treatment, and there is a problem that it must be manufactured at the expense of productivity. The demand for 6000 series aluminum alloys for automobile body panels has been increasing in recent years, and in order to respond to the further increase in demand in the future, a manufacturing method with excellent productivity has been required.
また、上記特許文献４〜６に記載の発明のいずれも、材質を造り込む工程とは別に表面調整のための上記処理を行うものであり、生産性が悪化したり生産コストが嵩むという問題があった。 In addition, any of the inventions described in Patent Documents 4 to 6 performs the above-described processing for surface adjustment separately from the step of building the material, and there is a problem that productivity deteriorates and production cost increases. there were.
そこで、本発明は、上記従来技術の生産性の問題を有利に解決できる、特に自動車ボディパネルの外板等に好適な、塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法を提供することを目的とするものである。 Accordingly, the present invention provides a method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability, particularly suitable for an outer plate of an automobile body panel, which can advantageously solve the above-mentioned productivity problems. It is for the purpose.
また、板表面に存在するＭｇＯ濃化層をも製造工程内で除去し、良好な接着性をも併せ持たせることが可能な６０００系アルミニウム合金板の製造方法を提供することを目的とする。 It is another object of the present invention to provide a method for producing a 6000 series aluminum alloy plate that can remove the MgO enriched layer present on the plate surface within the production process and also have good adhesion.
６０００系合金における時効硬化性は、微細な析出物が高密度に形成されることによって生じる。そこで、本発明者らは、塗装焼き付けという１７０〜１８０℃程度で２０〜３０分の短時間の熱処理によって大きな強度上昇量を得るためには、塗装焼き付け処理前の材料はどのような状態にあるべきかについて鋭意検討を行った。 Age hardening in a 6000 series alloy is caused by the formation of fine precipitates at a high density. Therefore, in order to obtain a large increase in strength by short-time heat treatment at about 170 to 180 ° C., that is, about 170 to 180 ° C., the present inventors are in any state of the material before the coating baking process. We conducted an intensive study on what should be done.
塗装焼き付け処理のような温度で形成される析出物は、６０００系合金の場合ＭｇとＳｉから構成される金属間化合物（β”相と呼ばれる）である。このβ”相を板の製造段階で微細かつ高密度に形成させておくことができれば、塗装焼付け処理段階でこのβ”相を成長させて大きな強度上昇を得ることができるだけでなく、板製造後の室温放置中の経時変化をも抑制することができる。 In the case of a 6000 series alloy, a precipitate formed at a temperature such as a paint baking process is an intermetallic compound composed of Mg and Si (referred to as a β ″ phase). If it can be formed finely and with high density, this β ”phase can be grown at the paint baking process stage to obtain a large increase in strength, and also suppresses changes over time during standing at room temperature after plate production. can do.
本発明者らは、この微細高密度β”組織を短時間で形成させる方法についてさらに詳細に検討した。その結果、β”相の形成はＭｇおよびＳｉの拡散で律速される反応であり、β”相形成温度を高めればＭｇおよびＳｉの拡散が容易となり、β”相の形成を短時間で達成し得ること（以下、この高温でのβ”相析出熱処理を高温予備時効処理という。）、そして成分を適切に選択すれば、従来技術のように低温で長時間の熱処理を行うのとほぼ同等の塗装焼付け硬化性と室温放置中の経時変化抑制効果が得られることを見出した。 The present inventors examined in more detail a method for forming this fine high-density β ″ structure in a short time. As a result, the formation of the β ″ phase is a rate-controlled reaction due to diffusion of Mg and Si, and β “Diffusion of Mg and Si is facilitated by increasing the phase formation temperature, and β” phase formation can be achieved in a short time (hereinafter, this “β” phase precipitation heat treatment at high temperature is referred to as high temperature pre-aging treatment). Then, it has been found that if the components are appropriately selected, the paint bake hardenability and the effect of suppressing the change with time during standing at room temperature can be obtained as in the case of conventional heat treatment at a low temperature for a long time.
さらに、高温予備時効処理中のβ”相の析出を一層促進し、より短い処理時間で大きな塗装焼き付け硬化性を得るためには、高温予備時効処理を行う前に焼き入れ凍結空孔量を増やした状態にしておくこと、またβ”相析出の駆動力であるＭｇおよびＳｉの過飽和度が大きく確保される低温で短時間保持してさらに微細な析出物を形成させておくと、高温予備時効処理でのβ”相析出促進に対して非常に効果的であることを見出した。本発明者らは、これらの知見をもとに従来に比べて大幅な生産性向上を可能とする本発明を成すに至った。 Furthermore, in order to further promote the precipitation of β ”phase during the high temperature pre-aging treatment and obtain a large paint bake hardenability in a shorter processing time, the quenching freezing void amount is increased before performing the high temperature pre-aging treatment. In addition, it is possible to maintain a high degree of pre-aging by maintaining a high temperature pre-aging by keeping it at a low temperature for a short time at a low temperature at which the supersaturation degree of Mg and Si, which is the driving force for β ″ phase precipitation, is large. The present inventors have found that it is very effective for promoting the β ″ phase precipitation in the treatment. The present inventors have made it possible to greatly improve the productivity based on these findings as compared with the prior art. It came to make.
上述のような高温において短時間で形成されたβ”析出物密度は、低温長時間で形成された場合よりも低い傾向にある。しかしながら低密度ではあるが比較的大きい針状の析出物であるため、塗装焼付け処理によって耐力上昇が得られやすい状態にあるというのが高温予備時効処理によって得られるβ”析出状態の特徴である。この析出状態を定量的に表現する方法について本発明者は鋭意検討を行った。本発明によって得られたβ”析出組織は非常に微細な針状析出物から構成されており、この微細析出物の観察を行うには、通常の透過電子顕微鏡法では観察は困難である。そこで、このβ”析出物を成長させて観察を容易にすることを考え、熱処理中にβ”析出物が新たに形成されるよりも、熱処理前に存在した微細なβ”析出物が成長する現象が支配的であるような、適切な熱処理条件を実験的に見出した。すなわち、塗装焼付け温度に相当する温度である１８０℃で９時間の熱処理を施すと、β”析出物は数十ｎｍ程度の針状となり、明視野像観察による通常の透過電子顕微鏡法により２０万倍程度の比較的低倍率でも十分に観察が行えるようになることがわかった。また、β”針状析出物はアルミ母相の｛１００｝面に対して平行に析出するという特徴を考慮して、β”析出物の存在状況をより的確に観察するために透過電子顕微鏡観察の際に薄膜試料に対する電子線の入射方向を＜００１＞と平行とする。本発明の合金に対して上記の熱処理を施した板より薄膜試料を作製して、［００１］方向に電子線を入射して透過電子顕微鏡観察を行った例を図１に示す。写真は、透過電子線を用いて結像した明視野像である。写真中には［１００］と［０１０］方向に平行に針状の析出物が明瞭に観察される。また黒い点状のコントラストを示すものは、紙面に対して垂直、すなわち［００１］方向に平行に存在する針状析出物に相当する。この透過電子顕微鏡観察結果をもとに析出物の密度を簡便に調査する方法についても種々検討を行った。その結果、［００１］方向に平行に存在する針状析出物に相当する黒い点状コントラストの数を測定し、［１００］と［０１０］方向に平行な針状析出物はほぼ同等の確率で存在することを利用して、黒い点の数を３倍して３方向の析出物数を比較的間単に見積る方法を考案した。そして、この方法を用いて２０万倍の倍率で１６視野測定すれば、諸性能を規定するに足る析出物密度を求めることができることを実験的に明らかにした。 The density of β ″ precipitate formed in a short time at a high temperature as described above tends to be lower than that formed in a low temperature and a long time. However, it is a low-density but relatively large needle-like precipitate. Therefore, it is a feature of the β ”precipitation state obtained by the high-temperature pre-aging treatment that the yield strength can be easily increased by the paint baking treatment. The present inventor has intensively studied a method for quantitatively expressing the precipitation state. The β ″ precipitate structure obtained by the present invention is composed of very fine needle-like precipitates, and it is difficult to observe these fine precipitates by ordinary transmission electron microscopy. Considering the fact that this β ″ precipitate is grown to facilitate observation, the phenomenon that the fine β ″ precipitate existing before the heat treatment grows rather than the new β ″ precipitate formed during the heat treatment. Appropriate heat treatment conditions were found experimentally such that is dominant. That is, when heat treatment is performed at 180 ° C., which is a temperature corresponding to the coating baking temperature, for 9 hours, β ″ precipitates become needles of about several tens of nanometers, and 200,000 are obtained by ordinary transmission electron microscopy using bright field image observation. It has been found that sufficient observation is possible even at a relatively low magnification of about twice. In consideration of the feature that β ″ acicular precipitates are precipitated parallel to the {100} plane of the aluminum matrix. In order to more accurately observe the presence of β ″ precipitates, the incident direction of the electron beam to the thin film sample is made parallel to <001> in the observation with a transmission electron microscope. A thin film sample was prepared from a heat-treated plate, and an electron beam was incident in the [001] direction and observed with a transmission electron microscope, as shown in Fig. 1. The photograph was imaged using a transmission electron beam. It is a bright field image, with [100] and [ 10] Needle-like precipitates are clearly observed parallel to the direction, and black dots having contrast are perpendicular to the paper surface, that is, needle-like precipitates existing parallel to the [001] direction. Various studies were also conducted on a method for simply examining the density of the precipitate based on the observation result of the transmission electron microscope, and as a result, it corresponds to the acicular precipitate existing in parallel with the [001] direction. The number of black dot-shaped contrasts is measured, and the number of black dots is tripled to 3 directions by utilizing the fact that acicular precipitates parallel to the [100] and [010] directions exist with almost the same probability. We have devised a method for estimating the number of precipitates in a relatively short period of time, and if this method is used to measure 16 fields of view at a magnification of 200,000 times, it is possible to obtain a precipitate density sufficient to define various performances. Clarified experimentally.
また、このβ”析出物密度が同じであっても、析出物の平均サイズが異なれば耐力を変化する。すなわち機械的性質を規定し得るようなβ”析出状態を記述するために、耐力を用いる方法を検討した。しかし、本系合金は製造後に常温で保管された場合、溶質原子のクラスターが形成され耐力が製造直後から上昇してしまうという問題がある。そこで、クラスターは適切な熱処理を施すことによって再固溶させることできる（この熱処理は復元処理と呼ばれる）特徴を活用し、適切な復元処理によってクラスターの影響を排除した後の耐力を測定すれば、板のβ”析出状態を規定し得る、製造直後に相当する耐力を求めることができることを見出した。 Also, even if this β ″ precipitate density is the same, the yield strength changes if the average size of the precipitates is different. In other words, the yield strength is described to describe the β ″ precipitation state that can define the mechanical properties. The method used was examined. However, when this alloy is stored at room temperature after production, there is a problem that solute atom clusters are formed and the yield strength is increased immediately after production. Therefore, if the cluster can be re-dissolved by performing an appropriate heat treatment (this heat treatment is called a restoration process), and the strength after removing the influence of the cluster by an appropriate restoration process is measured, It has been found that the yield strength can be determined immediately after production, which can define the β ″ precipitation state of the plate.
すなわち、透過電子顕微鏡観察写真から上述の方法によって求めたβ”析出物密度と適切な復元処理後の耐力を用いれば、塗装焼付け硬化性を決定するβ”析出状態を規定することができる。 That is, by using the β ″ precipitate density obtained by the above-described method from a transmission electron microscope observation photograph and the proof strength after an appropriate restoration treatment, the β ″ precipitation state that determines the bake hardenability can be defined.
また、本発明の製造方法のうち、高温予備時効前に低温予備時効を施す場合、温水を用いて低温予備時効処理を行うのが有効な方法の一つである。この場合に処理温度は６０〜１００℃に限定されるが、この温水のｐＨを４〜７に調整することによって、材質造りこみと同時に板表面のＭｇＯ濃化層を除去することができ、接着性や塗装後耐食性を同時に改善することができるようになる。この際、板を温水中に浸漬してもよいし、板に対して温水をスプレー等により噴霧しても構わない。 Further, in the production method of the present invention, when low temperature pre-aging is performed before high temperature pre-aging, it is one of effective methods to perform low temperature pre-aging treatment using hot water. In this case, the treatment temperature is limited to 60 to 100 ° C., but by adjusting the pH of this hot water to 4 to 7, the MgO concentrated layer on the plate surface can be removed simultaneously with the material building, And corrosion resistance after painting can be improved at the same time. At this time, the plate may be immersed in warm water, or warm water may be sprayed on the plate by spraying or the like.
本発明の要旨は以下のとおりである。
（１）質量％で、Ｍｇ：０．２〜１．０％、Ｓｉ：０．５〜１．５％を含有し、残部がＡｌ及び不可避不純物からなる成分組成を有し、熱間圧延および冷間圧延によって所望の板厚とした圧延板を、４８０〜５８０℃の温度で５分以下保持した後５℃／ｓ以上の冷却速度で冷却する溶体化焼入れ処理を行い、次いで、６０〜１２０℃の温度域で５秒〜１２０分または１２０〜１４０℃の温度域で５秒〜５分保持する低温予備時効処理を行い、次いで、１４０〜１５０℃の温度域で５分〜３０分間保持、１５０〜２４０℃の温度域で３０秒〜３０分間保持、２４０〜２５０℃の温度域で３０秒〜１０分間保持のうちいずれか一つの高温予備時効処理を施すことを特徴とする、塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（２）成分組成が質量％で、さらに、Ｍｎ：０．０１〜０．３％、Ｃｒ：０．００１〜０．１％の１種または２種を含有することを特徴とする、（１）記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（３）成分組成が質量％で、さらに、Ｔｉ：０．００５〜０．１５％、Ｂ ：０．０００１〜０．０５％、Ｆｅ：０．０３〜０．４％、Ｚｎ：０．０３〜２．５％の１種または２種以上を含有することを特徴とする、（１）または（２）記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（４）成分組成が質量％で、さらに、Ｃｕ：０．１〜１．０％を含有することを特徴とする、請求項（１）〜（３）いずれかの塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（５）成分組成が質量％で、さらに、Ｓｎ：０．０１〜０．３％を含有することを特徴とする、（１）〜（４）いずれかの塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（６） 前記溶体化焼入れ処理の焼入れ温度を５０℃以下とすることを特徴とする、上記（１）〜（５）のいずれかに記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。
（７） 前記溶体化焼入れ処理の工程と前記高温予備時効処理の工程との間で、前記低温予備時効処理に代えて、不純物元素の総含有量が１０００ｐｐｍ以下であり、ｐＨを４〜７に調整した６０〜１００℃の温水を用いて５秒〜５分の低温予備時効処理を行うことを特徴とする、（１）〜（５）のいずれかに記載の塗装焼付け硬化性ならびに接着性に優れた６０００系アルミニウム合金板の製造方法。
The gist of the present invention is as follows.
(1) By mass%, Mg: 0.2-1.0%, Si: 0.5-1.5%, the balance has a component composition consisting of Al and inevitable impurities , A rolled sheet having a desired sheet thickness by cold rolling is held at a temperature of 480 to 580 ° C. for 5 minutes or less, and then subjected to a solution hardening treatment for cooling at a cooling rate of 5 ° C./s or more, and then 60 to 120 Perform low temperature pre-aging treatment for 5 seconds to 120 minutes in the temperature range of 5 ° C or 5 seconds to 5 minutes in the temperature range of 120 to 140 ° C, and then hold in the temperature range of 140 to 150 ° C for 5 minutes to 30 minutes. Baking and hardening of paint , characterized in that any one of high temperature pre-aging treatment is performed in a temperature range of 150 to 240 ° C. for 30 seconds to 30 minutes and in a temperature range of 240 to 250 ° C. for 30 seconds to 10 minutes. Of 6000 series aluminum alloy plate with excellent properties .
(2) The component composition is mass%, and further contains one or two of Mn: 0.01 to 0.3% and Cr: 0.001 to 0.1%. ) A method for producing a 6000 series aluminum alloy plate having excellent paint bake hardenability.
(3) The component composition is mass%, and Ti: 0.005-0.15%, B: 0.0001-0.05%, Fe: 0.03-0.4%, Zn: 0.03 The method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability according to (1) or (2), which comprises 1 to 2.5% or two or more.
(4) The component composition is mass%, and further contains Cu: 0.1 to 1.0%, which is excellent in paint bake hardenability according to any one of claims (1) to (3) A method for producing a 6000 series aluminum alloy plate.
(5) Component composition is mass%, and further contains Sn: 0.01 to 0.3%, (6000) which is excellent in paint bake curability of any one of (1) to (4) A method for producing an aluminum alloy plate .
(6 ) The quenching temperature of the solution hardening treatment is 50 ° C. or lower, and the 6000 series aluminum alloy plate excellent in paint bake hardenability according to any one of (1) to (5) above Production method.
( 7 ) Instead of the low temperature preliminary aging treatment, the total content of impurity elements is 1000 ppm or less, and the pH is set to 4 to 7 between the solution quenching treatment step and the high temperature preliminary aging treatment step. It is characterized by performing a low temperature pre-aging treatment for 5 seconds to 5 minutes using adjusted warm water of 60 to 100 ° C., (1) to (5) A method for producing an excellent 6000 series aluminum alloy plate .
本発明により、自動車のエンジンフード、トランクリッド等のパネル材として好適な、高い塗装焼付け硬化性を有する６０００系アルミニウム合金板およびその生産性に優れた製造方法を提供することが可能になるとともに、良好な接着性をも兼備することができるため、産業上の貢献が極めて顕著である。特に（１）〜（７）で製造された合金板は１８０ＭＰａ以上の塗装焼付け硬化後の強度を得ることができる。 According to the present invention, it is possible to provide a 6000 series aluminum alloy plate having high paint bake hardenability and a manufacturing method excellent in its productivity, which is suitable as a panel material for automobile engine hoods, trunk lids, and the like. Since it can also have good adhesiveness, the industrial contribution is very remarkable. In particular, the alloy plate produced in (1) to (7) can obtain strength after paint bake hardening of 180 MPa or more .
本発明者らは、６０００系アルミニウム合金板の塗装焼付け硬化性を支配するβ”相形成挙動について鋭意検討を行った結果見出した知見に基づき、溶体化処理後の熱処理パターンおよび合金成分を適切に規定することによって、溶体化処理後の短時間の熱処理で良好な塗装焼付け硬化性を得ることが可能な本発明を成すに至った。 Based on the knowledge found out as a result of intensive studies on the β "phase formation behavior that governs the bake hardenability of 6000 series aluminum alloy sheets, the present inventors appropriately set the heat treatment pattern and alloy components after solution treatment. By prescribing, the present invention has been achieved in which good paint bake hardenability can be obtained by a short heat treatment after the solution treatment.
以下、本発明について詳細に説明する。
先ず、合金成分の限定理由を以下に示す。
Hereinafter, the present invention will be described in detail.
First, the reasons for limiting the alloy components are shown below.
Ｍｇ、Ｓｉは、本発明の必須の基本成分であり、優れた塗装焼付け硬化性を得るために含有させる。本発明の熱処理においてはＭｇが０．２％未満、Ｓｉが０．５％未満では、塗装焼付け時に形成されるβ”相（Ｍｇ、Ｓｉからなる金属間化合物）の量が少なく、十分な強度上昇が得られない。また、Ｍｇが１．０％超、Ｓｉが１．５％超では、板製造過程で粒界及び粒内に粗大なＭｇ2Ｓｉ相が形成され、加工性が大きく低下する。そのため、Ｍｇ量を０．２〜１．０％、Ｓｉ量を０．５〜１．５％の範囲とした。 Mg and Si are essential basic components of the present invention, and are contained in order to obtain excellent paint bake hardenability. In the heat treatment of the present invention, when Mg is less than 0.2% and Si is less than 0.5%, the amount of β ″ phase (intermetallic compound composed of Mg and Si) formed during baking is small and sufficient strength In addition, when Mg exceeds 1.0% and Si exceeds 1.5%, coarse Mg 2 Si phases are formed in the grain boundaries and in the grains during the plate manufacturing process, and the workability is greatly reduced. Therefore, the Mg amount is set to 0.2 to 1.0% and the Si amount is set to 0.5 to 1.5%.
本発明は、必要に応じて以下に示す元素を含有させてもよい。 The present invention may contain the following elements as required.
Ｍｎ、Ｃｒは、最終板の結晶粒を微細化して肌荒れを防止し、成形性を向上させる元素である。Ｍｎ量が０．３％、Ｃｒ量が０．１％を超えると、粗大な金属間化合物が形成され、かえって成形性が損なわれてしまう。一方、Ｍｎが０．０１％未満、Ｃｒが０．００１％未満では、結晶粒が粗大化して肌荒れを生じてしまう場合がある。したがってＭｎ量を０．０１〜０．１５％、Ｃｒ量を０．００１〜０．１％の範囲とした。 Mn and Cr are elements that refine the crystal grains of the final plate to prevent rough skin and improve formability. When the amount of Mn is 0.3% and the amount of Cr exceeds 0.1%, a coarse intermetallic compound is formed, and on the contrary, formability is impaired. On the other hand, if Mn is less than 0.01% and Cr is less than 0.001%, crystal grains may be coarsened to cause rough skin. Therefore, the Mn content is in the range of 0.01 to 0.15%, and the Cr content is in the range of 0.001 to 0.1%.
また、本発明では、Ｔｉ、Ｂ、Ｆｅ、Ｚｎの１種又は２種以上を必要に応じて含有させても良い。 Moreover, in this invention, you may contain 1 type, or 2 or more types of Ti, B, Fe, and Zn as needed.
Ｔｉ、Ｂは、微量添加により鋳塊の結晶粒を微細化し、成形性、肌荒れ等を改善する効果を有する。Ｔｉが０．００５％未満、Ｂが０．０００１％未満では鋳塊の結晶粒を微細化する効果がやや不十分である。また、Ｔｉが０．１５％、Ｂが０．０５％を超えると粗大な晶出物を形成し、成形性が劣化することがある。そのため、Ｔｉ量を０．００５〜０．１５％、Ｂ量を０．０００１〜０．０５％の範囲とすることが好ましい。 Ti and B have the effect of refining crystal grains of the ingot by adding a small amount and improving formability, rough skin, and the like. When Ti is less than 0.005% and B is less than 0.0001%, the effect of refining the crystal grains of the ingot is slightly insufficient. On the other hand, if Ti exceeds 0.15% and B exceeds 0.05%, a coarse crystallized product may be formed, and the formability may deteriorate. Therefore, it is preferable that the Ti amount is in the range of 0.005 to 0.15% and the B amount is in the range of 0.0001 to 0.05%.
Ｆｅは、強度向上と結晶粒の微細化によって成形性を向上させる元素であるが、その効果は、Ｆｅ量が０．０３％未満ではやや不十分である。一方、Ｆｅ量が０．４％を超えると粗大晶出物が生成し、成形性を低下させることがある。したがって、Ｆｅ量を０．０３〜０．４％の範囲とすることが好ましい。 Fe is an element that improves formability by improving strength and refining crystal grains, but the effect is somewhat insufficient when the Fe content is less than 0.03%. On the other hand, if the amount of Fe exceeds 0.4%, a coarse crystallized product is generated, and the formability may be lowered. Therefore, it is preferable to make the amount of Fe into the range of 0.03-0.4%.
Ｚｎは、強度向上により成形性を向上させる効果を有する。Ｚｎ量が０．０３％未満では、効果がやや不十分であり、２．５％を超えると強度上昇が大きく、成形性を損なうことがある。そのため、Ｚｎ量を０．０３〜２．５％の範囲とすることが好ましい。 Zn has the effect of improving moldability by improving strength. If the amount of Zn is less than 0.03%, the effect is slightly insufficient, and if it exceeds 2.5%, the strength increases greatly and the moldability may be impaired. Therefore, it is preferable to make Zn content into the range of 0.03-2.5%.
Ｃｕは、成形性、特に張出し性、深絞り性の向上に寄与する元素である。Ｃｕ量が０．１％未満では、十分な成形性向上効果が得られず、１．０％超では、耐食性がやや低下し、ヘム曲げ性を損なうことがある。そのため、Ｃｕ量を０．１〜１．０％の範囲とすることが好ましい。 Cu is an element that contributes to improving the formability, particularly the stretchability and deep drawability. If the amount of Cu is less than 0.1%, sufficient effect of improving formability cannot be obtained, and if it exceeds 1.0%, the corrosion resistance may be slightly lowered and the hem bendability may be impaired. Therefore, it is preferable to make Cu amount into the range of 0.1 to 1.0%.
Ｓｎは、室温放置中の自然時効による強度上昇を抑制し、製造直後の成形加工性を長期間にわたって保持する効果を有する。Ｓｎが０．０１％未満ではその効果が小さく、また０．３％を超えるとその効果が飽和して増大しない。そのため、Ｓｎの添加量を０．０１〜０．３％とした。またＳｎの効果を有効に活用するためにはＡｌ母相中にＳｎを均一に固溶させることが重要であり、そのためには溶解鋳造時にＳｎを、Ａｌ―Ｓｎ母合金として添加することが望ましい。なお、Ａｌ―Ｓｎ母合金中のＳｎ含有量については特に規定する必要はない。 Sn suppresses an increase in strength due to natural aging during standing at room temperature, and has the effect of maintaining the molding processability immediately after production for a long period of time. If Sn is less than 0.01%, the effect is small, and if it exceeds 0.3%, the effect is saturated and does not increase. Therefore, the amount of Sn added is set to 0.01 to 0.3%. In order to effectively use the effect of Sn, it is important to uniformly dissolve Sn in the Al matrix, and for that purpose, it is desirable to add Sn as an Al—Sn master alloy during melt casting. . The Sn content in the Al—Sn master alloy need not be specified.
上記元素の他、不可避的不純物が含有されるが、本発明の効果を損なわない範囲の量であれば許容される。 In addition to the above elements, inevitable impurities are contained, but the amount is within the range that does not impair the effects of the present invention.
製造直後の製品に対して１８０℃×９ｈの熱処理を施した後のβ”析出物密度の規定理由について説明する。なお、析出物密度の測定は上述の［課題を解決するための手段］の欄で詳細に説明した方法で行う。 The reason for defining the β ″ precipitate density after heat treatment of 180 ° C. × 9 h for the product immediately after production will be described. The measurement of the precipitate density is based on the above [Means for Solving the Problems]. The method described in detail in the column is used.
β”析出物密度が３０００個／μｍ2未満では、良好な塗装焼付け効果性が得られない。また７０００個／μｍ2超の析出物密度では優れた塗装焼付け効果性を示すが、低温長時間の予備時効処理では得られるものの、高温短時間予備時効処理では得られ難い。そこで、β”析出物密度は３０００〜７０００個／μｍ2とした。なお、塗装焼付け硬化性と生産性の観点から、４０００〜６０００個／μｍ2が好ましい。 If the β ″ precipitate density is less than 3000 / μm 2 , good paint baking effect cannot be obtained. Also, if the precipitate density exceeds 7000 / μm 2 , excellent paint baking effect is exhibited, but low temperature and long time However, it is difficult to obtain by high-temperature short-time pre-aging treatment. Therefore, the β ″ precipitate density was set to 3000 to 7000 / μm 2 . From the viewpoint of productivity and painting-baking hardenability, is preferably 4000 to 6000 pieces / [mu] m 2.
また、復元処理後の耐力の規定理由について説明する。先ず適切な復元処理条件を以下の方法により見出さなければならない。復元処理の目安としては、オイルバスを用いて１８０〜２８０℃の温度に急熱して数秒から数分保持した後水冷する。クラスターが復元されたかどうかは次ぎの方法によって確認できる。復元処理前の析出状態と復元処理直後の析出状態を示差走査熱量計を用いて測定する。図２に測定結果例を示す。クラスターの存在を示す１５０〜２７０℃程度の範囲に認められる吸熱ピーク面積が０．３ｃａｌ／ｇ以下となり、２７０〜３００℃あたりに認められるβ”の析出に対応したピーク面積が復元処理前の状態と０．１ｃａｌ／ｇ以下の範囲で変わっていなければ、β”析出状態をほぼ変えずにクラスターを再固溶させることができたと考えられる。この条件によって復元処理を施した後の耐力が９０ＭＰａ未満では良好な塗装焼付け硬化性が得られず、１４０ＭＰａ超では塗装焼付け硬化性は十分に得られるが、室温保管中のクラスター形成による耐力上昇を考慮するとこの値では高すぎ、室温経時変化後は形状凍結性やヘム曲げ性が劣る恐れがある。そこで、９０〜１４０ＭＰａの範囲とした。 Also, the reason for specifying the proof stress after the restoration process will be described. First, an appropriate restoration process condition must be found by the following method. As a standard for the restoration process, the oil bath is used to rapidly heat to a temperature of 180 to 280 ° C., hold for several seconds to several minutes, and then cool with water. The following method can be used to check whether the cluster has been restored. The precipitation state before the restoration treatment and the precipitation state immediately after the restoration treatment are measured using a differential scanning calorimeter. FIG. 2 shows an example of measurement results. The endothermic peak area observed in the range of about 150 to 270 ° C. indicating the presence of the cluster is 0.3 cal / g or less, and the peak area corresponding to the precipitation of β ″ observed around 270 to 300 ° C. is the state before the restoration treatment If it is not changed within the range of 0.1 cal / g or less, it is considered that the β "precipitation state was hardly changed and the cluster could be dissolved again. If the yield strength after the restoration treatment is less than 90 MPa under this condition, good paint bake hardenability cannot be obtained. Considering this value, this value is too high, and there is a possibility that the shape freezing property and the hem bendability are inferior after the room temperature aging. Therefore, the range was 90 to 140 MPa.
次ぎに、本発明の製造方法に関して詳細に説明する。 Next, the production method of the present invention will be described in detail.
本発明のアルミニウム合金板は、従来の一般的な方法にしたがって溶解、鋳造、熱間圧延、冷間圧延によって製造された板に対して、本発明で規定した溶体化処理および高温予備時効処理、必要に応じて、さらに、その前処理としての低温予備時効処理を施すことによって製造される。ただし、鋳片に均質化焼鈍を施しても良く、また冷間圧延の途中に中間焼鈍を行ってもかまわない。 The aluminum alloy plate of the present invention is a solution produced by high temperature pre-aging treatment as defined in the present invention for a plate produced by melting, casting, hot rolling, cold rolling according to a conventional general method, If necessary, it is further produced by performing a low temperature pre-aging treatment as a pretreatment. However, the slab may be subjected to homogenization annealing, or intermediate annealing may be performed during the cold rolling.
先ず、溶体化処理について説明を行う。従来の一般的な方法にしたがって得られた冷間圧延板に対して溶体化処理を施すが、溶体化処理温度は４８０℃未満ではＭｇ2ＳｉやＳｉ相の固溶が不十分であり、塗装焼付け硬化性が低下するだけでなく、ヘム曲げ性、成形性も劣化する。一方、溶体化処理温度が５８０℃超では、共晶融解が起きる場合がありヘム曲げ性及び成形性の低下を招く恐れがあり、また、結晶粒の粗大化による肌荒れが生じやすくなり好ましくない。溶体化処理温度に到達後、保持せずに直ちに冷却しても良いが、５分以内の所定時間保持することによりＭｇ2ＳｉやＳｉ相の固溶が促進され、塗装焼付け硬化性、ヘム曲げ性、成形性が向上するため、５分以内の所定時間の保持が好ましい。しかし、溶体化処理温度での保持時間が５分を超えると、溶質の固溶は飽和し、結晶粒が粗大化する恐れがあり好ましくない。 First, the solution treatment will be described. Although the solution treatment is performed on the cold-rolled sheet obtained according to the conventional general method, the solution treatment temperature is less than 480 ° C., and solid solution of Mg 2 Si or Si phase is insufficient. Not only is the bake hardenability lowered, but the hem bendability and moldability are also deteriorated. On the other hand, if the solution treatment temperature is higher than 580 ° C., eutectic melting may occur, which may lead to a decrease in hem bendability and formability, and rough skin due to coarsening of crystal grains tends to occur. After reaching the solution treatment temperature, it may be cooled immediately without being held, but holding for a predetermined time within 5 minutes promotes solid solution of Mg 2 Si and Si phase, paint bake hardenability, hem bending Since the property and moldability are improved, it is preferable to hold for a predetermined time within 5 minutes. However, if the retention time at the solution treatment temperature exceeds 5 minutes, the solid solution of the solute is saturated and the crystal grains may become coarse, which is not preferable.
溶体化処理後の冷却速度は、５℃／ｓ未満では冷却過程で結晶粒界にＭｇ2Ｓｉ相やＳｉ相等が析出し、ヘム曲げ性、成形性、塗装焼付け硬化性が劣化するため、下限を５℃／ｓとした。粒界析出を抑制し、溶質原子の過飽和度を十分に確保する点で好ましい下限は１０℃／ｓ以上である。冷却速度の上限は特に規定はしないが、冷却速度が速すぎると板の形状を損なうため、（１）〜（７）の発明においては板が変形しやすい４００℃までは３０℃／ｓ以下、４００℃以下は３００℃／ｓ以下で冷却することが好ましい。 If the cooling rate after solution treatment is less than 5 ° C / s, the Mg 2 Si phase, Si phase, etc. will precipitate at the grain boundaries during the cooling process, and the hem bendability, formability and paint bake hardenability will deteriorate. Was set to 5 ° C./s. A preferable lower limit is 10 ° C./s or more in terms of suppressing grain boundary precipitation and sufficiently ensuring the degree of supersaturation of solute atoms. The upper limit of the cooling rate is not particularly specified, but if the cooling rate is too high, the shape of the plate is impaired. Therefore, in the inventions of ( 1 ) to ( 7 ), the plate is easily deformed up to 400 ° C, up to 30 ° C / s, is 400 ° C. or less arbitrariness preferred to cool below 300 ° C. / s.
溶体化処理、焼入れ処理後に行う高温予備時効処理温度は１４０℃未満では十分な塗装焼付け硬化性が確保できるようなβ”相を短時間に形成させることができない。また、２５０℃超では初期強度が高くなり過ぎて、成形性、ヘム曲げ性等の加工性が劣化してしまう。また、保持時間については１４０℃から１５０℃で５分未満、１５０℃〜２５０℃で３０秒未満では十分な塗装焼付け硬化性が確保できない。一方、１４０℃から２４０℃では３０分，２４０℃から２５０℃では１０分超の保持を行うと初期強度が高くなり過ぎて、成形性やヘム曲げ性等の加工性が劣化してしまうばかりでなく、本発明が目的とする生産性を損なう。上記の理由により、高温予備時効処理条件は、１４０〜１５０℃では５〜３０分保持，１５０℃から２４０℃では３０秒〜３０分，２４０〜２５０℃の温度範囲において３０秒〜１０分間保持することを条件とした。 If the temperature of the high temperature pre-aging treatment after solution treatment and quenching is less than 140 ° C., a β ″ phase that can ensure sufficient bake hardenability cannot be formed in a short time. As a result, the processability such as formability, hem bendability, etc. deteriorates, and it is sufficient that the holding time is from 140 ° C. to 150 ° C. for less than 5 minutes and from 150 ° C. to 250 ° C. for less than 30 seconds. Paint bake hardenability cannot be ensured, while holding at 140 ° C to 240 ° C for 30 minutes and 240 ° C to 250 ° C for more than 10 minutes will increase the initial strength, resulting in processing such as formability and hem bendability. As a result, the high temperature pre-aging treatment conditions are maintained at 140 to 150 ° C. for 5 to 30 minutes, and from 150 to 24 ° C. ℃, 30 seconds to 30 minutes, and the condition to hold 30 seconds to 10 minutes in the temperature range of 240 to 250 ° C..
次ぎに、溶体化焼入れ処理の工程と高温予備時効処理の工程との間に差し挟む、高温予備時効処理におけるβ”相析出を促進するための低温予備時効処理条件の限定理由について説明する。 Next, the reason for limiting the low temperature pre-aging conditions for promoting β ″ phase precipitation in the high temperature pre-aging process, which is sandwiched between the solution hardening process and the high temperature pre-aging process, will be described.
この低温予備時効処理温度が６０℃未満では、クラスター（６０００系アルミニウム合金において常温近傍で形成される溶質原子の集合体で、この相が形成されると塗装焼付け硬化性が阻害される。）が形成されてしまい、引き続き行う高温予備時効処理でのβ”相の析出促進ならびに析出組織の微細化効果が不十分となってしまう。また、１４０℃超で５分超、１２０℃超で１２０分超、の保持をしても高温予備時効処理でのβ”相の析出促進効果が十分に得られない。保持時間については５秒未満では上述の効果が確保できず、一方、６０〜１２０℃で１２０分超、１２０〜１４０℃で５分超、の保持を行うと高温予備時効処理後の初期強度が高くなり過ぎて、成形性やヘム曲げ性等の加工性が劣化してしまうばかりでなく、本発明が目的とする生産性を損なう。上記の理由により、低温予備時効処理条件は６０〜１２０℃において５秒〜１２０分間、１２０〜１４０℃において５秒〜５分間保持することとした。この低温予備時効処理後に再加熱して前述の高温予備時効処理を施す。低温予備時効温度から高温予備時効温度までの加熱速度は特に規定しないが、生産性の点からは速い方が望ましい。 When this low temperature pre-aging temperature is less than 60 ° C., clusters (aggregates of solute atoms formed in the vicinity of room temperature in a 6000 series aluminum alloy. When this phase is formed, the bake hardenability of coating is hindered). In the subsequent high temperature pre-aging treatment, the precipitation of β ″ phase and the effect of refining the precipitate structure become insufficient. Further, the temperature exceeds 140 ° C. for more than 5 minutes, and the temperature exceeding 120 ° C. for 120 minutes. Even if it is kept above, the effect of promoting the precipitation of β ″ phase in the high temperature pre-aging treatment cannot be obtained sufficiently. Regarding the holding time, if the holding time is less than 5 seconds, the above-mentioned effect cannot be ensured. On the other hand, if holding is performed at 60 to 120 ° C. for more than 120 minutes and 120 to 140 ° C. for more than 5 minutes, the initial strength after high temperature pre-aging treatment is increased. When it becomes too high, workability such as formability and hem bendability is deteriorated, and productivity aimed at by the present invention is impaired. For the above reasons, the low temperature preliminary aging treatment conditions were held at 60 to 120 ° C. for 5 seconds to 120 minutes and at 120 to 140 ° C. for 5 seconds to 5 minutes. After the low-temperature pre-aging treatment, the above-described high-temperature pre-aging treatment is performed by reheating. Although the heating rate from the low temperature pre-aging temperature to the high temperature pre-aging temperature is not particularly defined, it is desirable that the heating rate is high from the viewpoint of productivity.
また、この低温予備時効処理を施す場合に、温水を用いて行うのが有効な方法の一つであり、板を温水中に浸漬してもよいし、また温水を板に対して噴霧してもよい。温水での低温予備時効を行う際、処理温度は６０〜１００℃に限定されるが、この温水のｐＨや不純物濃度を調整することによって、上述のような材質造りこみと同時に板表面のＭｇＯ濃化層を除去して接着性をも向上させることができる。ｐＨが４未満ではＭｇＯ濃化層だけではなく、下地のＡｌも溶出してしまい、ｐＨが７超ではＭｇＯ濃化層の除去が不十分である。そこで、ｐＨの範囲を４〜７と規定した。また、不純物元素の総含有量が１０００ｐｐｍ超であると、ＭｇＯ濃化層の溶解力が不足してしまうとともに板表面が汚染されてしまう。そこで、１０００ｐｐｍ以下と規定した。 In addition, when performing this low temperature preliminary aging treatment, it is one of the effective methods to use hot water, and the plate may be immersed in warm water, or the hot water is sprayed on the plate. Also good. When performing the low temperature preliminary aging with warm water, the treatment temperature is limited to 60 to 100 ° C. By adjusting the pH and impurity concentration of the warm water, the MgO concentration on the plate surface at the same time as the material building as described above is performed. The adhesive layer can also be improved by removing the chemical layer. If the pH is less than 4, not only the MgO concentrated layer but also the underlying Al is eluted, and if the pH exceeds 7, the removal of the MgO concentrated layer is insufficient. Therefore, the pH range was defined as 4-7. Further, if the total content of impurity elements exceeds 1000 ppm, the dissolving power of the MgO concentrated layer is insufficient and the plate surface is contaminated. Therefore, it was defined as 1000 ppm or less.
次ぎに、溶体化焼入れ処理の焼入れ温度条件について説明する。 Next, quenching temperature conditions for the solution hardening treatment will be described.
溶体化焼入れ処理後の焼入れ温度は、次工程となる高温予備時効処理または低温予備時効処理の処理温度域とすれば、追加の加熱、冷却処理を省略できるため好ましい。 It is preferable that the quenching temperature after the solution quenching process is within the processing temperature range of the high-temperature pre-aging treatment or the low-temperature pre-aging treatment, which will be the next step, because additional heating and cooling processes can be omitted.
また、溶体化焼入れ処理の焼入れ温度を５０℃以下とすれば、焼入れ凍結空孔量を増やして引き続き行う高温予備時効処理におけるβ”相析出促進効果が十分に得られ好ましい。一旦２５℃以下に５分以内の保持すれば更に良い。溶体化焼入れ処理の焼入れ温度が５０℃超では、前記のような効果は十分に得られない。溶体化焼入れ処理の焼入れ温度の下限は特に限定しないが、工業的に可能な範囲で低温ほど望ましい。なお、この５０℃以下の温度域では前記のクラスターが形成されてしまうので、この温度域に保持しないことが望ましい。そして，２５℃以下にすると更に高温予備時効処理におけるβ”相析出促進効果が十分に得られ、その時間が５分程度ならばクラスター形成は少なく塗装焼付け硬化性を大きく阻害する恐れは少ない。この溶体化焼入れ処理後５０℃以下まで冷却した後に再加熱して高温予備時効処理または低温予備時効処理を施すが、この際の加熱速度も上述のように特に規定しないが、クラスターの形成や生産性の点から速い方が望ましい。 Further, if the quenching temperature in the solution quenching process is set to 50 ° C. or less, the β ″ phase precipitation promoting effect can be sufficiently obtained in the high-temperature pre-aging treatment that is continuously performed by increasing the quenching freezing void amount. The above effect is not sufficiently obtained when the quenching temperature of the solution hardening treatment exceeds 50 ° C. Although the lower limit of the quenching temperature of the solution hardening treatment is not particularly limited, It is desirable that the temperature is as low as possible within the industrially possible range.Because the above clusters are formed in this temperature range of 50 ° C. or lower, it is desirable not to maintain this temperature range. If the β ″ phase precipitation promoting effect in the preliminary aging treatment is sufficiently obtained and the time is about 5 minutes, the cluster formation is small and there is little possibility of greatly hindering the paint bake hardenability. After this solution quenching treatment, it is cooled to 50 ° C. or lower and then reheated to give a high temperature pre-aging treatment or a low temperature pre-aging treatment. The heating rate at this time is not particularly specified as described above. Faster is desirable from the viewpoint of sex.
表１に示す成分組成を有する６０００系アルミニウム合金を溶解し、ＤＣ鋳造法により鋳造した。得られた鋳塊に５３０℃で１０時間の均質化焼鈍を施した後、５１０℃で熱間圧延を開始し、２５０℃で板厚を５ｍｍとして熱間圧延を終了した。その後１ｍｍまで冷間圧延を行い、表２に示す条件で溶体化処理および予備時効処理を施した。これらのアルミニウム合金板を、室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価した。また、本合金の主用途である自動車ボディパネル用材料として必要なヘム曲げ性および成形性についても評価を行った。 A 6000 series aluminum alloy having the component composition shown in Table 1 was melted and cast by a DC casting method. The obtained ingot was subjected to homogenization annealing at 530 ° C. for 10 hours, and then hot rolling was started at 510 ° C., and the hot rolling was finished at 250 ° C. with a plate thickness of 5 mm. Thereafter, cold rolling was performed to 1 mm, and solution treatment and preliminary aging treatment were performed under the conditions shown in Table 2. These aluminum alloy plates were naturally aged at room temperature for 1 month, and then evaluated for tensile properties and paint bake hardenability. We also evaluated the hem bendability and formability required for automotive body panel materials, which are the main uses of this alloy.
引張特性は、板圧延方向（Ｌ方向）、圧延方向から４５°の方向（Ｄ方向）、圧延方向に直角な方向（Ｃ方向）を長手とする、ＪＩＳ Ｚ ２２０１に準拠した５号試験片を採取して、ＪＩＳ Ｚ ２２４１に準拠して引張試験を行い、３方向の面内異方性を考慮した平均値で評価した。 Tensile properties are obtained by measuring No. 5 test piece in accordance with JIS Z 2201, which has a plate rolling direction (L direction), a direction 45 ° from the rolling direction (D direction), and a direction perpendicular to the rolling direction (C direction) as the longitudinal direction. The samples were collected and subjected to a tensile test in accordance with JIS Z 2241, and evaluated with an average value considering in-plane anisotropy in three directions.
塗装焼付け硬化性は、Ｃ方向を長手として、引張試験機で２％の塑性歪を与えた後、１７０℃で２０分の熱処理を行い、再び引張試験を行い、０．２％耐力を測定し、熱処理後の耐力が１８０ＭＰａ以上のものを良好として評価した。 The paint bake hardenability is determined by measuring the 0.2% proof stress by applying a 2% plastic strain with a tensile tester with the C direction as the longitudinal direction, then performing a heat treatment at 170 ° C for 20 minutes, performing a tensile test again. The one having a proof stress after heat treatment of 180 MPa or more was evaluated as good.
ヘム曲げ性は、Ｌ方向、Ｄ方向、Ｃ方向を長手とするＪＩＳ Ｚ ２２０１に準拠した５号試験片に、引張試験機により各試験片に５％の予歪を与え、その後ＪＩＳ Ｚ ２２４８に準拠して、曲げ半径Ｒを板厚の０．５倍として１８０°まで曲げた後、更に１ｍｍ厚の板を挟んで密着させるように曲げて、曲げ部の頂点近傍における割れ発生の有無で評価した。曲げ表面にカラーチェックを施して、ルーペを用いて割れを目視観察した。なお、カラーチェックは、ＪＩＳ Ｚ ２３４３に準拠した浸透探傷試験である。３方向で割れ発生の認められない場合をヘム曲げ性良好として○印を付し、１方向でも割れが認められた場合は不良とし、×印を付した。 The hem bendability is determined by applying a pre-strain of 5% to each test piece with a tensile tester on a No. 5 test piece based on JIS Z 2201 having the L direction, D direction, and C direction as the longitudinal direction. In accordance with this, the bending radius R is 0.5 times the plate thickness, bent to 180 °, and then bent so as to be in close contact with a 1 mm thick plate, and evaluated by the presence or absence of cracks near the apex of the bent portion. did. A color check was performed on the bent surface, and the cracks were visually observed using a loupe. The color check is a penetrant flaw detection test based on JIS Z 2343. A case where cracks were not observed in three directions was marked as ◯ with good hem bendability, and a case where cracks were also observed in one direction was marked as poor, and a mark x was given.
成形性は、塩化ビニルフィルムとワックスを組み合わせた潤滑条件において、φ１００ｍｍの球頭張出試験を行い、破断限界高さにより評価した。この破断限界高さが３４ｍｍ以上を良好とした。 The moldability was evaluated by performing a bulge head test with a diameter of 100 mm under lubrication conditions in which a vinyl chloride film and a wax were combined, and evaluating the limit height at break. This breaking limit height was determined to be 34 mm or more.
表３に評価結果を示す。 Table 3 shows the evaluation results.
合金Ｎｏ．３〜９は、合金成分および製造条件が本発明の範囲内であり、塗装焼付け硬化性に優れ、良好なヘム曲げ性と成形性を示した。一方、合金Ｎｏ．１２はＭｇ、Ｓｉ量が本発明の範囲よりも少ないため、塗装焼付け硬化性が低く、成形性にも劣る。合金Ｎｏ．１３は、Ｓｉ量およびＣｒ量が本発明の範囲よりも多く、第２相粒子が多くなりヘム曲げ性が低下した。合金Ｎｏ．１４は、Ｓｉ量が本発明の範囲よりも少ないため、塗装焼付け硬化性が低く、成形性にも劣る。合金Ｎｏ．１５は、Ｍｇ添加量が本発明の範囲よりも多く、Ｓｉ量が少ないために、塗装焼付け硬化性およびヘム曲げ性が低い。合金Ｎｏ．１６は、Ｍｇの添加量が本発明の範囲よりも少ないため、塗装焼付け硬化性が低く、成形性も低い。合金Ｎｏ．１７は、Ｍｇ、Ｓｉ、Ｃｕ、Ｍｎ量が本発明範囲よりも多く、第２相粒子数が多くなり、ヘム曲げ性が低下した。合金Ｎｏ．１８はＦｅ、Ｓｎ添加量が本発明範囲よりも多く、第２相粒子数が増えたために、ヘム曲げ性が低下した。 Alloy No. In Nos. 3 to 9 , the alloy components and the production conditions were within the scope of the present invention, the paint bake hardenability was excellent, and good hem bendability and formability were exhibited. On the other hand, Alloy No. No. 12 has a lower amount of Mg and Si than the range of the present invention, so the paint bake curability is low and the moldability is also poor. Alloy No. In No. 13, the amount of Si and Cr was larger than the range of the present invention, the second phase particles increased, and the hem bendability decreased. Alloy No. No. 14 has a Si content less than the range of the present invention, and therefore has low paint bake curability and inferior moldability. Alloy No. No. 15 has a Mg addition amount larger than the range of the present invention and a small Si amount, so that the paint bake hardenability and the hem bendability are low. Alloy No. No. 16 has an additive amount of Mg that is less than the range of the present invention, so that the paint bake curability is low and the moldability is also low. Alloy No. In No. 17, the amount of Mg, Si, Cu, Mn was larger than the range of the present invention, the number of second phase particles was increased, and the hem bendability was lowered. Alloy No. No. 18 had more Fe and Sn additions than the range of the present invention, and the number of second phase particles increased, resulting in a decrease in hem bendability.
表１の本発明合金６および８をＤＣ鋳造法により鋳造し、実施例１と同様の製造方法により１ｍｍの冷間圧延板とした。この冷間圧延板に対して、表４に示す条件で溶体化処理および予備時効処理を施した。このようにして作製したアルミニウム合金板を、室温で１ヶ月間自然時効させた後、実施例１と同様な方法で引張特性、塗装焼付け硬化性、ヘム曲げ性、成形性を評価して、その結果を表５に示した。 Inventive alloys 6 and 8 in Table 1 were cast by a DC casting method, and a 1 mm cold-rolled plate was produced by the same production method as in Example 1. The cold rolled sheet was subjected to solution treatment and preliminary aging treatment under the conditions shown in Table 4. After the aluminum alloy plate thus produced was naturally aged at room temperature for 1 month, the tensile properties, paint bake hardenability, hem bendability and formability were evaluated in the same manner as in Example 1. The results are shown in Table 5.
製造番号ク〜シは、製造条件が本発明の範囲内であり、塗装焼付け硬化性に優れ、良好なヘム曲げ性と成形性を示した。 The production numbers of KU to SH were within the scope of the present invention, were excellent in paint bake curability, and exhibited good hem bendability and formability.
一方、製造番号エは予備時効温度が本発明範囲よりも低く、また製造番号オは予備時効温度が本発明範囲よりも高いために塗装焼付け硬化性が劣った。製造番号オはヘム曲げ性も低下した。製造番号スは予備時効時間が本発明範囲よりも長いために初期強度が高くなりすぎ、ヘム曲げ性、成形性が低かった。製造番号セは、溶体化温度が本発明範囲よりも低いために、また製造番号ソは溶体化処理後の冷却速度が本発明範囲よりも小さいために、塗装焼付け硬化性、ヘム曲げ性、成形性が低下した。 On the other hand, the production number D had a preliminary aging temperature lower than the range of the present invention, and the production number O had a preliminary aging temperature higher than the range of the present invention, so the paint bake curability was inferior. The production number O also decreased hem bendability. Since the pre-aging time of the production number was longer than the range of the present invention, the initial strength was too high, and the hem bendability and moldability were low. The production number S is because the solution temperature is lower than the range of the present invention, and the production number S0 is the cooling rate after the solution treatment is smaller than the range of the present invention. Decreased.
表１の本発明合金１〜１１をＤＣ鋳造法により鋳造し、実施例１と同様の製造方法により１ｍｍの冷間圧延板とした。この冷間圧延板に対して、表６に示す条件で溶体化処理および予備時効処理を施した。このようにして作製した、製造直後のアルミニウム合金板の引張試験を行い、また１８０℃×９ｈの熱処理を施し、透過電子顕微鏡観察を行って析出物密度を評価した。一方、室温で１ヶ月間自然時効させた後、実施例１と同様な方法で引張特性、塗装焼付け硬化性、ヘム曲げ性、成形性を評価した。また、各試料に対して適切な条件で復元処理を施してクラスターの影響を排除した後に引張試験を行って耐力を求めた。この耐力値は製造直後に引張試験を行って得た値とほぼ一致した。以上の結果を表７に示した。表７における合金３、４、８、９は、製造条件が本発明の範囲内であり、塗装焼付け硬化性に優れ、良好なヘム曲げ性と成形性を示した。一方、合金５、１０、１１は高温予備時効温度が本発明範囲よりも高く、保持時間も短いために析出物密度が本発明範囲よりも低くなってしまい、塗装焼付け硬化性が劣った。また合金７は予備時効温度が本発明範囲よりも低いために復元処理後耐力が低く、塗装焼付け硬化性が劣ってしまった。 Inventive alloys 1 to 11 in Table 1 were cast by a DC casting method, and 1 mm cold-rolled plates were produced by the same production method as in Example 1. The cold-rolled sheet was subjected to solution treatment and preliminary aging treatment under the conditions shown in Table 6. A tensile test was performed on the aluminum alloy plate produced immediately after manufacturing as described above, heat treatment at 180 ° C. × 9 h was performed, and observation with a transmission electron microscope was performed to evaluate the precipitate density. On the other hand, after natural aging at room temperature for 1 month, tensile properties, paint bake hardenability, hem bendability and moldability were evaluated in the same manner as in Example 1. In addition, each sample was subjected to a restoration process under appropriate conditions to eliminate the influence of the cluster, and then a tensile test was performed to determine the yield strength. This proof stress value almost coincided with the value obtained by conducting a tensile test immediately after production. The above results are shown in Table 7. Alloys 3, 4 , 8 , and 9 in Table 7 had production conditions within the scope of the present invention, were excellent in paint bake hardenability, and exhibited good hem bendability and formability. On the other hand, Alloys 5, 10, and 11 had a high temperature pre-aging temperature higher than the range of the present invention and a short holding time, so that the density of precipitates was lower than the range of the present invention and the paint bake hardenability was poor. Moreover, since the pre-aging temperature of the alloy 7 was lower than the range of the present invention, the yield strength after the restoration treatment was low, and the paint bake hardenability was inferior.
表１の本発明合金１をＤＣ鋳造法により鋳造し、実施例１と同様の製造方法により１ｍｍの冷間圧延板とした。この冷間圧延板に対して、５２０℃×２０ｓの溶体化処理を施した後、表８に示す条件で焼入れ処理および低温予備時効処理を施し、２００℃×１００ｓの高温予備時効処理を行った。このようにして作製した各アルミニウム合金板を室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価、ならびに接着性の評価を行った。評価に用いた接着剤は自動車の構造接着に一般的に使用されている一液硬化型エポキシ系の接着剤とした。接着性試験としてはＪＩＳＫ６８５４に従った剥離試験とＪＩＳＫ６８５０に従った引張せん断試験を行った。接着性の評価は、剥離形態の観察に基づいて行った。アルミニウム合金板表面と接着剤間の密着力が十分に確保されおり、接着剤層の内部で凝集破壊が生じて破壊しているものを良◎、アルミニウム合金板と接着剤との界面剥離が部分的に生じているが、界面剥離面積率が５０％未満のものを可○、５０％以上界面剥離が生じているものを不可△とする３段階の評価を行った。評価結果を表９に示す。本発明例の(1)〜(3)は、良好な塗装焼付け硬化性を有するとともに、良好な接着性を示した。また、比較例(4)は、温水中で低温予備時効処理を行ったが、ｐＨが本発明範囲を超えて高かったために、塗装焼付け硬化性は良好であったが、十分な接着性が得られなかった。比較例(5)は、不純物濃度が本発明範囲を超えて高かったために、接着性が不十分であった。比較例(6)は大気中で低温予備時効処理を行ったために、十分な接着性を得ることができなかった。 The alloy 1 of the present invention shown in Table 1 was cast by a DC casting method, and a 1 mm cold-rolled plate was produced by the same production method as in Example 1. The cold-rolled sheet was subjected to a solution treatment at 520 ° C. × 20 s, then subjected to a quenching treatment and a low temperature pre-aging treatment under the conditions shown in Table 8, and a high temperature pre-aging treatment at 200 ° C. × 100 s was performed. . Each aluminum alloy plate thus produced was naturally aged at room temperature for 1 month, and then evaluated for tensile properties, paint bake hardenability, and adhesion. The adhesive used for the evaluation was a one-part curable epoxy adhesive generally used for structural bonding of automobiles. As the adhesion test, a peel test according to JISK6854 and a tensile shear test according to JISK6850 were performed. Evaluation of adhesiveness was performed based on observation of a peeling form. Adhesive strength between the surface of the aluminum alloy plate and the adhesive is sufficiently secured, and it is good if the adhesive layer is broken due to cohesive failure inside, part of the interface peeling between the aluminum alloy plate and the adhesive is partial However, a three-stage evaluation was performed in which an interface peeling area ratio of less than 50% was acceptable, and an interface peeling of 50% or more was deemed unacceptable. Table 9 shows the evaluation results. Examples (1) to (3) of the present invention had good paint bake hardenability and good adhesion. Further, Comparative Example (4) was subjected to a low temperature pre-aging treatment in warm water, but because the pH was higher than the range of the present invention, the paint bake curability was good, but sufficient adhesion was obtained. I couldn't. In Comparative Example (5), the impurity concentration was high beyond the range of the present invention, so that the adhesiveness was insufficient. In Comparative Example (6), a low temperature pre-aging treatment was performed in the atmosphere, so that sufficient adhesion could not be obtained.
Ａｌ−０．６Ｍｇ−１．０Ｓｉ成分組成を有する６０００系アルミニウム合金を溶解し、ＤＣ鋳造法により鋳造した。得られた鋳塊に５３０℃で１０時間の均質化焼鈍を施した後、５１０℃で熱間圧延を開始し、２５０℃で板厚を５ｍｍとして熱間圧延を終了した。その後１ｍｍまで冷間圧延を行い、表１０に示す溶体化処理条件を変化させた条件で溶体化処理および予備時効処理を施した。これらのアルミニウム合金板を、室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価した。 A 6000 series aluminum alloy having an Al-0.6Mg-1.0Si component composition was melted and cast by a DC casting method. The obtained ingot was subjected to homogenization annealing at 530 ° C. for 10 hours, and then hot rolling was started at 510 ° C., and the hot rolling was finished at 250 ° C. with a plate thickness of 5 mm. Thereafter, cold rolling was performed to 1 mm, and solution treatment and preliminary aging treatment were performed under the conditions in which the solution treatment conditions shown in Table 10 were changed. These aluminum alloy plates were naturally aged at room temperature for 1 month, and then evaluated for tensile properties and paint bake hardenability.
引張特性は、板圧延方向（Ｌ方向）、圧延方向から４５°の方向（Ｄ方向）、圧延方向に直角な方向（Ｃ方向）を長手とする、ＪＩＳ Ｚ ２２０１に準拠した５号試験片を採取して、ＪＩＳ Ｚ ２２４１に準拠して引張試験を行い、３方向の面内異方性を考慮した平均値で評価した。尚、耐力は成形性の観点より１４０ＭＰａ以下のものを良好として評価した。塗装焼付け硬化性は、Ｃ方向を長手として、引張試験機で２％の塑性歪を与えた後、１７０℃で２０分の熱処理を行い、再び引張試験を行い、２％耐力を測定し、熱処理後の耐力が１９０ＭＰａ以上のものを良好として評価した。この実施例を表１１に示す。 Tensile properties are obtained by measuring No. 5 test piece in accordance with JIS Z 2201, which has a plate rolling direction (L direction), a direction 45 ° from the rolling direction (D direction), and a direction perpendicular to the rolling direction (C direction) as the longitudinal direction. The samples were collected and subjected to a tensile test in accordance with JIS Z 2241, and evaluated with an average value considering in-plane anisotropy in three directions. In addition, the proof stress was evaluated as good at 140 MPa or less from the viewpoint of moldability. Paint bake hardenability is set to the C direction as the longitudinal direction, 2% plastic strain is given with a tensile tester, heat treatment is performed at 170 ° C. for 20 minutes, tensile test is performed again, 2% proof stress is measured, heat treatment Those having a yield strength of 190 MPa or more were evaluated as good. This example is shown in Table 11.
Ａｌ−０．６Ｍｇ−１．０Ｓｉ成分組成を有する６０００系アルミニウム合金を溶解し、ＤＣ鋳造法により鋳造した。得られた鋳塊に５３０℃で１０時間の均質化焼鈍を施した後、５１０℃で熱間圧延を開始し、２５０℃で板厚を５ｍｍとして熱間圧延を終了した。その後１ｍｍまで冷間圧延を行い、表１２に示す溶体化処理後の焼入れ条件を変化させた条件で溶体化処理および予備時効処理を施した。これらのアルミニウム合金板を、室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価した。 A 6000 series aluminum alloy having an Al-0.6Mg-1.0Si component composition was melted and cast by a DC casting method. The obtained ingot was subjected to homogenization annealing at 530 ° C. for 10 hours, and then hot rolling was started at 510 ° C., and the hot rolling was finished at 250 ° C. with a plate thickness of 5 mm. Thereafter, cold rolling was performed to 1 mm, and solution treatment and preliminary aging treatment were performed under the conditions in which the quenching conditions after the solution treatment shown in Table 12 were changed. These aluminum alloy plates were naturally aged at room temperature for 1 month, and then evaluated for tensile properties and paint bake hardenability.
引張特性は、板圧延方向（Ｌ方向）、圧延方向から４５°の方向（Ｄ方向）、圧延方向に直角な方向（Ｃ方向）を長手とする、ＪＩＳ Ｚ ２２０１に準拠した５号試験片を採取して、ＪＩＳ Ｚ ２２４１に準拠して引張試験を行い、３方向の面内異方性を考慮した平均値で評価した。尚、耐力は成形性の観点より１４０ＭＰａ以下のものを良好として評価した。塗装焼付け硬化性は、Ｃ方向を長手として、引張試験機で２％の塑性歪を与えた後、１７０℃で２０分の熱処理を行い、再び引張試験を行い、２％耐力を測定し、熱処理後の耐力が１９０ＭＰａ以上のものを良好として評価した。この実施例を表１３に示す。 Tensile properties are obtained by measuring No. 5 test piece in accordance with JIS Z 2201, which has a plate rolling direction (L direction), a direction 45 ° from the rolling direction (D direction), and a direction perpendicular to the rolling direction (C direction) as the longitudinal direction. The samples were collected and subjected to a tensile test in accordance with JIS Z 2241, and evaluated with an average value considering in-plane anisotropy in three directions. In addition, the proof stress was evaluated as good at 140 MPa or less from the viewpoint of moldability. Paint bake hardenability is set to the C direction as the longitudinal direction, 2% plastic strain is given with a tensile tester, heat treatment is performed at 170 ° C. for 20 minutes, tensile test is performed again, 2% proof stress is measured, heat treatment Those having a yield strength of 190 MPa or more were evaluated as good. This example is shown in Table 13.
Ａｌ−０．６Ｍｇ−１．０Ｓｉ成分組成を有する６０００系アルミニウム合金を溶解し、ＤＣ鋳造法により鋳造した。得られた鋳塊に５３０℃で１０時間の均質化焼鈍を施した後、５１０℃で熱間圧延を開始し、２５０℃で板厚を５ｍｍとして熱間圧延を終了した。その後１ｍｍまで冷間圧延を行い、表１４に示す低温予備時効条件を変化させた条件で溶体化処理および予備時効処理を施した。これらのアルミニウム合金板を、室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価した。 A 6000 series aluminum alloy having an Al-0.6Mg-1.0Si component composition was melted and cast by a DC casting method. The obtained ingot was subjected to homogenization annealing at 530 ° C. for 10 hours, and then hot rolling was started at 510 ° C., and the hot rolling was finished at 250 ° C. with a plate thickness of 5 mm. Thereafter, cold rolling was performed to 1 mm, and solution treatment and preliminary aging treatment were performed under the conditions where the low temperature preaging conditions shown in Table 14 were changed. These aluminum alloy plates were naturally aged at room temperature for 1 month, and then evaluated for tensile properties and paint bake hardenability.
引張特性は、板圧延方向（Ｌ方向）、圧延方向から４５°の方向（Ｄ方向）、圧延方向に直角な方向（Ｃ方向）を長手とする、ＪＩＳ Ｚ ２２０１に準拠した５号試験片を採取して、ＪＩＳ Ｚ ２２４１に準拠して引張試験を行い、３方向の面内異方性を考慮した平均値で評価した。尚、耐力は成形性の観点より１４０ＭＰａのものを良好として評価した。塗装焼付け硬化性は、Ｃ方向を長手として、引張試験機で２％の塑性歪を与えた後、１７０℃で２０分の熱処理を行い、再び引張試験を行い、２％耐力を測定し、熱処理後の耐力が１９０ＭＰａ以上のものを良好として評価した。この実施例を表１５に示す。 Tensile properties are obtained by measuring No. 5 test piece in accordance with JIS Z 2201, which has a plate rolling direction (L direction), a direction 45 ° from the rolling direction (D direction), and a direction perpendicular to the rolling direction (C direction) as the longitudinal direction. The samples were collected and subjected to a tensile test in accordance with JIS Z 2241, and evaluated with an average value considering in-plane anisotropy in three directions. The proof stress was evaluated as 140 MPa from the viewpoint of moldability. Paint bake hardenability is set to the C direction as the longitudinal direction, 2% plastic strain is given with a tensile tester, heat treatment is performed at 170 ° C. for 20 minutes, tensile test is performed again, 2% proof stress is measured, heat treatment Those having a yield strength of 190 MPa or more were evaluated as good. This example is shown in Table 15.
Ａｌ−０．６Ｍｇ−１．０Ｓｉ成分組成を有する６０００系アルミニウム合金を溶解し、ＤＣ鋳造法により鋳造した。得られた鋳塊に５３０℃で１０時間の均質化焼鈍を施した後、５１０℃で熱間圧延を開始し、２５０℃で板厚を５ｍｍとして熱間圧延を終了した。その後１ｍｍまで冷間圧延を行い、表１６に示す高温予備時効条件を変化させた条件で溶体化処理および予備時効処理を施した。これらのアルミニウム合金板を、室温で１ヶ月間自然時効させた後、引張特性、塗装焼付け硬化性を評価した。 A 6000 series aluminum alloy having an Al-0.6Mg-1.0Si component composition was melted and cast by a DC casting method. The obtained ingot was subjected to homogenization annealing at 530 ° C. for 10 hours, and then hot rolling was started at 510 ° C., and the hot rolling was finished at 250 ° C. with a plate thickness of 5 mm. Thereafter, cold rolling was performed to 1 mm, and solution treatment and preliminary aging treatment were performed under the conditions where the high temperature preaging conditions shown in Table 16 were changed. These aluminum alloy plates were naturally aged at room temperature for 1 month, and then evaluated for tensile properties and paint bake hardenability.
引張特性は、板圧延方向（Ｌ方向）、圧延方向から４５°の方向（Ｄ方向）、圧延方向に直角な方向（Ｃ方向）を長手とする、ＪＩＳ Ｚ ２２０１に準拠した５号試験片を採取して、ＪＩＳ Ｚ ２２４１に準拠して引張試験を行い、３方向の面内異方性を考慮した平均値で評価した。尚、耐力は成形性の観点より１４０ＭＰａのものを良好として評価した。塗装焼付け硬化性は、Ｃ方向を長手として、引張試験機で２％の塑性歪を与えた後、１７０℃で２０分の熱処理を行い、再び引張試験を行い、２％耐力を測定し、熱処理後の耐力が１９０ＭＰａ以上のものを良好として評価した。この実施例を表１７に示す。 Tensile properties are obtained by measuring No. 5 test piece in accordance with JIS Z 2201, which has a plate rolling direction (L direction), a direction 45 ° from the rolling direction (D direction), and a direction perpendicular to the rolling direction (C direction) as the longitudinal direction. The samples were collected and subjected to a tensile test in accordance with JIS Z 2241, and evaluated with an average value considering in-plane anisotropy in three directions. The proof stress was evaluated as 140 MPa from the viewpoint of moldability. Paint bake hardenability is set to the C direction as the longitudinal direction, 2% plastic strain is given with a tensile tester, heat treatment is performed at 170 ° C. for 20 minutes, tensile test is performed again, 2% proof stress is measured, heat treatment Those having a yield strength of 190 MPa or more were evaluated as good. This example is shown in Table 17.
Claims (7)
Ｍｇ：０．２〜１．０％、
Ｓｉ：０．５〜１．５％
を含有し、残部がＡｌ及び不可避不純物からなる成分組成を有し、
熱間圧延および冷間圧延によって所望の板厚とした圧延板を、４８０〜５８０℃の温度で５分以下保持した後５℃／ｓ以上の冷却速度で冷却する溶体化焼入れ処理を行い、次いで、６０〜１２０℃の温度域で５秒〜１２０分または１２０〜１４０℃の温度域で５秒〜５分保持する低温予備時効処理を行い、次いで、１４０〜１５０℃の温度域で５分〜３０分間保持、１５０〜２４０℃の温度域で３０秒〜３０分間保持、２４０〜２５０℃の温度域で３０秒〜１０分間保持のうちいずれか一つの高温予備時効処理を施すことを特徴とする、塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。 % By mass
Mg: 0.2-1.0%
Si: 0.5 to 1.5%
And the balance has a component composition consisting of Al and inevitable impurities ,
A rolled sheet having a desired thickness by hot rolling and cold rolling is held at a temperature of 480 to 580 ° C. for 5 minutes or less and then cooled at a cooling rate of 5 ° C./s or more, and then a solution hardening treatment is performed. , A low temperature pre-aging treatment for 5 seconds to 120 minutes in a temperature range of 60 to 120 ° C. or 5 seconds to 5 minutes in a temperature range of 120 to 140 ° C., and then in a temperature range of 140 to 150 ° C. for 5 minutes to It is characterized by performing a high temperature pre-aging treatment of any one of holding for 30 minutes, holding for 30 seconds to 30 minutes in a temperature range of 150 to 240 ° C, and holding for 30 seconds to 10 minutes in a temperature range of 240 to 250 ° C. , A method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability.
Ｍｎ：０．０１〜０．３％、
Ｃｒ：０．００１〜０．１％
の１種または２種を含有することを特徴とする、請求項１記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。 Ingredient composition is mass%,
Mn: 0.01 to 0.3%
Cr: 0.001 to 0.1%
The method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability according to claim 1, wherein one or two of the above are contained.
Ｔｉ：０．００５〜０．１５％、
Ｂ ：０．０００１〜０．０５％、
Ｆｅ：０．０３〜０．４％、
Ｚｎ：０．０３〜２．５％
の１種または２種以上を含有することを特徴とする、請求項１または２記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。 Ingredient composition is mass%,
Ti: 0.005 to 0.15%,
B: 0.0001 to 0.05%,
Fe: 0.03-0.4%,
Zn: 0.03-2.5%
The method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability according to claim 1 or 2, characterized by containing one or more of the following.
Ｃｕ：０．１〜１．０％
を含有することを特徴とする、請求項１〜３いずれかの一項記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。 Ingredient composition is mass%,
Cu: 0.1 to 1.0%
The method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability according to any one of claims 1 to 3, comprising :
Ｓｎ：０．０１〜０．３％
を含有することを特徴とする、請求項１〜４いずれかの一項記載の塗装焼付け硬化性に優れた６０００系アルミニウム合金板の製造方法。 Ingredient composition is mass%,
Sn: 0.01-0.3%
The method for producing a 6000 series aluminum alloy plate excellent in paint bake hardenability according to any one of claims 1 to 4, comprising :
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| CN110373576A (en) * | 2019-08-07 | 2019-10-25 | 安庆市泽烨新材料技术推广服务有限公司 | A kind of cable Al-alloy and preparation method thereof |
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| EP2631317A1 (en) * | 2012-02-23 | 2013-08-28 | AMAG rolling GmbH | Annealable aluminium alloy and method for improving artificial ageing ability |
| JP5839588B2 (en) * | 2012-10-02 | 2016-01-06 | 株式会社神戸製鋼所 | Press forming method for automotive panel material |
| JP6315582B2 (en) * | 2014-08-27 | 2018-04-25 | 株式会社神戸製鋼所 | Aluminum alloy sheet for forming |
| CN105369072A (en) * | 2015-09-23 | 2016-03-02 | 广州市美伦建材有限公司 | Forming method for light metal plate |
| JP6306123B2 (en) * | 2016-03-30 | 2018-04-04 | 株式会社神戸製鋼所 | Aluminum alloy plate and method for producing aluminum alloy plate |
| CN109722572B (en) * | 2018-12-30 | 2020-06-23 | 精美铝业有限公司 | High-performance aluminum alloy for power transmission and transformation equipment and preparation method thereof |
| CN114703407B (en) * | 2022-03-11 | 2022-10-11 | 吉林大学 | High-performance Al-Mg-Si-Cu-Sn aluminum alloy and preparation method thereof |
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| JPH05230604A (en) * | 1992-02-20 | 1993-09-07 | Furukawa Alum Co Ltd | Manufacture of aluminum alloy for baking and hardening formation |
| JPH05230605A (en) * | 1992-02-20 | 1993-09-07 | Furukawa Alum Co Ltd | Manufacture of aluminum alloy for baking and hardening formation |
| JPH08253832A (en) * | 1995-03-14 | 1996-10-01 | Furukawa Electric Co Ltd:The | Aluminum-magnesium-silicon type aluminum alloy sheet minimal in secular change and excellent in baking hardenability and its production |
| JPH0941062A (en) * | 1995-07-27 | 1997-02-10 | Furukawa Electric Co Ltd:The | Alum.-magnesium-silicon type alum. alloy sheet material for automotive body sheet small in secular change and excellent in baking hardenability and its production |
| JP3752140B2 (en) * | 2000-10-03 | 2006-03-08 | 株式会社神戸製鋼所 | Al-Mg-Si Al alloy plate with excellent bending workability |
| JP2003231955A (en) * | 2002-02-07 | 2003-08-19 | Nippon Steel Corp | Process for manufacturing aluminum alloy plate with excellent hemmability and bake-hardening property |
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