JP2017214656A - Manufacturing method of 7000 series aluminum alloy member excellent in stress corrosion crack resistance - Google Patents

Manufacturing method of 7000 series aluminum alloy member excellent in stress corrosion crack resistance Download PDF

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JP2017214656A
JP2017214656A JP2017113827A JP2017113827A JP2017214656A JP 2017214656 A JP2017214656 A JP 2017214656A JP 2017113827 A JP2017113827 A JP 2017113827A JP 2017113827 A JP2017113827 A JP 2017113827A JP 2017214656 A JP2017214656 A JP 2017214656A
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aluminum alloy
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series aluminum
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stress corrosion
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橋本 成一
Seiichi Hashimoto
成一 橋本
隆広 志鎌
Takahiro Shikama
隆広 志鎌
恒武 津吉
Tsunetake Tsuyoshi
恒武 津吉
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Kobe Steel Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide an aluminum alloy member having high strength and excellent in stress corrosion crack resistance without generation of cracking by conducting an impregnation process on a 7000 series aluminum alloy extrusion material.SOLUTION: A 7000 series aluminum alloy extrusion material containing Zn:3.0 to 8.0 mass%, Mg:0.4 to 2.5 mass%, Cu:0.05 to 2.0 mass% and Ti:0.005 to 0.2 mass% and manufactured by press hardening is heated at temperature rise rate of 0.4°C/sec. held at a temperature range of 200 to 550°C for over 0 sec. to 60 sec. or less, then applied to a restoration treatment for cooling at cooling rate of 0.5°C/sec. or more and an impregnation treatment in 72 hours after the restoration treatment, and then an aging treatment is conducted on whole.SELECTED DRAWING: Figure 1

Description

本発明は、高強度の7000系アルミニウム合金押出形材の長手方向に沿った少なくとも一部領域に、潰し加工を施して部材化した7000系アルミニウム合金部材の製造方法に関し、特に耐応力腐食割れ性に優れた7000系アルミニウム合金部材の製造方法に関する。   The present invention relates to a method for producing a 7000 series aluminum alloy member obtained by crushing at least a partial region along the longitudinal direction of a high-strength 7000 series aluminum alloy extruded shape, particularly stress corrosion cracking resistance. The present invention relates to a method for producing an excellent 7000 series aluminum alloy member.

特許文献1〜3には、対向配置された一対のフランジとそれらに連結された複数のウエブからなるアルミニウム合金押出形材の端部領域に、フランジ面に対し垂直方向に潰し加工を施し、ドアビームやバンパーリインフォース等の自動車用補強部材を製造することが記載されている。このような潰し加工は、加工精度及びコスト面から時効処理後に行うことが望ましいとされ、特許文献2には、プレス焼き入れした6000系アルミニウム合金押出形材について、時効処理後に潰し加工を行うことが記載されている。   In Patent Documents 1 to 3, an end region of an aluminum alloy extruded shape member composed of a pair of opposed flanges and a plurality of webs connected to the flanges is crushed in a direction perpendicular to the flange surface, and a door beam And manufacturing a reinforcing member for automobiles such as bumper reinforcement. Such crushing processing is desirably performed after aging treatment from the viewpoint of processing accuracy and cost, and Patent Document 2 discloses that crushing processing is performed after aging treatment on a press-quenched 6000 series aluminum alloy extruded shape. Is described.

一方、Zn、Mg、Cuなどの合金元素量が多く、時効処理したとき他の合金系に比して高強度化される7000系アルミニウム合金押出形材では、時効処理後の成形性が悪く、時効処理後に潰し加工を行うと、潰し加工率(断面高さの減少率)が小さくても、曲げ変形するウエブに亀裂が発生する。なお、この傾向は高合金側でより顕著である。このため、例えば特許文献4では、押出後のT1調質の状態で潰し加工を行い、その後に時効処理を行うことが望ましいと記載されている。
しかし、7000系アルミニウム合金押出形材は、プレス焼き入れ後、時効処理前の材料(T1調質)でも、自然時効によって硬化し、成形性が低下する。その成形性を改善するため、例えば特許文献5〜7に記載されているように、従来より、自然時効により硬化した7000系アルミニウム合金の強度を低下させる復元処理が行われている。
On the other hand, in the 7000 series aluminum alloy extruded shape that has a large amount of alloy elements such as Zn, Mg, Cu, etc., and is strengthened compared to other alloy systems when subjected to aging treatment, the formability after aging treatment is poor, When crushing is performed after the aging treatment, even if the crushing rate (reduction rate of the cross-sectional height) is small, a crack is generated in the web that is bent and deformed. This tendency is more remarkable on the high alloy side. For this reason, for example, Patent Document 4 describes that it is desirable to perform crushing in a T1 tempered state after extrusion, and then perform an aging treatment.
However, the 7000 series aluminum alloy extruded shape is cured by natural aging even after press quenching and before aging treatment (T1 tempering), and the formability is lowered. In order to improve the formability, for example, as described in Patent Documents 5 to 7, a restoration treatment for reducing the strength of a 7000 series aluminum alloy hardened by natural aging has been conventionally performed.

特許第3465862号公報Japanese Patent No. 3465862 特許第4111651号公報Japanese Patent No. 4111651 特開平7−25296号公報Japanese Patent Laid-Open No. 7-25296 特開2003−118367号公報JP 2003-118367 A 特開平7−305151号公報Japanese Patent Laid-Open No. 7-305151 特開平10−168553号公報JP-A-10-168553 特開2007−119853号公報JP 2007-119853 A

確かに、この復元処理をT1調質の7000系アルミニウム合金押出形材に適用すると、同形材は強度が低下し、成形性が向上する。しかし、ウエブの板厚が1.5〜4mmの実用材を用い、これに潰し加工を行った場合、潰し加工率の大きさによっては、ウエブの曲げ外側に亀裂が発生し、これは従来の復元処理では解消できない。同時に、潰し加工後のウエブに高い引張残留応力が付与され、耐応力腐食割れ性が低下するという問題もある。   Certainly, when this restoration process is applied to a T1 tempered 7000 series aluminum alloy extruded shape, the shape of the same shape is reduced and the formability is improved. However, when a practical material having a web thickness of 1.5 to 4 mm is used and subjected to a crushing process, a crack is generated on the outside of the web depending on the size of the crushing rate. It cannot be resolved by the restoration process. At the same time, there is a problem in that a high tensile residual stress is imparted to the web after crushing and the stress corrosion cracking resistance is lowered.

本発明は、このような問題に鑑みてなされてもので、7000系アルミニウム合金押出形材の長手方向に沿った少なくとも一部の領域に、押出方向に対し垂直方向の潰し加工を施して部材化した7000系アルミニウム合金部材において、潰し加工による亀裂の発生を防止し、同時に引張残留応力を低減して耐応力腐食割れ性を改善することを目的とする。   Since the present invention is made in view of such problems, at least a part of the 7000 series aluminum alloy extruded profile along the longitudinal direction is subjected to a crushing process perpendicular to the extrusion direction to form a member. An object of the 7000 series aluminum alloy member is to prevent the occurrence of cracks due to crushing, and at the same time to reduce the tensile residual stress and improve the stress corrosion cracking resistance.

本発明に係る耐応力腐食割れ性に優れた7000系アルミニウム合金部材の製造方法は、Zn:3.0〜8.0質量%、Mg:0.5〜2.5質量%、Cu:0.05〜2.0質量%、Ti:0.005〜0.2質量%を含有し、さらに、Mn:0.01〜0.3質量%、Cr:0.01〜0.3質量%、Zr:0.01〜0.3質量%の1種又は2種以上を含有し、残部Al及び不可避不純物からなる組成を有し、複数の板で構成されプレス焼き入れされた7000系アルミニウム合金押出形材の長手方向に沿った少なくとも一部の領域に、押出方向に対し垂直方向の潰し加工を施して部材化するもので、前記7000系アルミニウム合金押出形材の少なくとも前記領域(潰し加工を施す領域)に対し、0.4℃/秒以上の昇温速度で加熱し、200〜550℃の温度範囲に0秒を超え60秒以下保持し、次いで0.5℃/秒以上の冷却速度で冷却する復元処理を施し、復元処理後72時間以内に、1.5mm≦t≦4.0mm、3t/2≦R≦10tとなる条件で前記潰し加工を施し、潰し加工後、部材全体に時効処理を施すことを特徴とする。
前記7000系アルミニウム合金押出形材は、典型的には、対向配置された一対のフランジとそれらを連結する1又は2以上のウエブからなる。その場合、通常、前記ウエブが潰し加工により最も大きく曲げ変形を受ける板となる。
The manufacturing method of the 7000 series aluminum alloy member excellent in stress corrosion cracking resistance according to the present invention is Zn: 3.0 to 8.0 mass%, Mg: 0.5 to 2.5 mass%, Cu: 0.00. 0.5 to 2.0 mass%, Ti: 0.005 to 0.2 mass%, Mn: 0.01 to 0.3 mass%, Cr: 0.01 to 0.3 mass%, Zr : 7000 series aluminum alloy extruded form containing one or more of 0.01 to 0.3% by mass, having a composition consisting of the balance Al and inevitable impurities, and composed of a plurality of plates and press-hardened At least part of the region along the longitudinal direction of the material is subjected to crushing in a direction perpendicular to the extrusion direction to form a member. At least the region of the 7000 series aluminum alloy extruded shape (region to be crushed) ) With a heating rate of 0.4 ° C / second or more In the temperature range of 200 to 550 ° C., a restoration process is performed in which the temperature is maintained for more than 0 seconds and not more than 60 seconds and then cooled at a cooling rate of 0.5 ° C./second or more. The crushing process is performed under the conditions of t ≦ 4.0 mm and 3t / 2 ≦ R ≦ 10t, and after the crushing process, the entire member is subjected to an aging treatment.
The 7000 series aluminum alloy extruded profile typically comprises a pair of opposed flanges and one or more webs connecting them. In that case, the web is usually a plate that undergoes the largest bending deformation by crushing.

本発明によれば、プレス焼き入れされた7000系アルミニウム合金押出形材の長手方向に沿った少なくとも一部の領域に対し潰し加工を施して部材化する場合に、高強度で、亀裂の発生がなく、引張残留応力を低減して耐応力腐食割れ性が改善された7000系アルミニウム合金部材を提供することができる。   According to the present invention, when forming a member by crushing at least a partial region along the longitudinal direction of the press-quenched 7000 series aluminum alloy extruded shape, high strength and generation of cracks are caused. Therefore, it is possible to provide a 7000 series aluminum alloy member in which the tensile residual stress is reduced and the stress corrosion cracking resistance is improved.

7000系アルミニウム合金押出形材におけるY(=σrs/σ0.2)とX(=[Mg]+[Zn])の関係を示すグラフである。It is a graph which shows the relationship between Y (= (sigma) rs / (sigma) 0.2 ) and X (= [Mg] + [Zn]) in a 7000 series aluminum alloy extrusion shape material. 実施例で作製した7000系アルミニウム合金押出形材の断面図(2A)、及び潰し加工の試験方法を説明する側面図(2B)である。It is sectional drawing (2A) of 7000 series aluminum alloy extrusion shape material produced in the Example, and a side view (2B) explaining the test method of a crushing process.

以下、本発明に係る7000系アルミニウム合金部材及びその製造方法について、具体的に説明する。
(アルミニウム合金の組成)
まず、本発明に係る7000系アルミニウム合金の組成について説明する。ただし、この組成自体は7000系アルミニウム合金として公知のものである。
Zn:3.0〜8.0質量%
Mg:0.4〜2.5質量%
ZnとMgは金属間化合物であるMgZn2を形成して、7000系アルミニウム合金の強度を向上させる元素である。Zn含有量が3.0質量%未満又はMg含有量が0.4質量%未満では、実用材として必要な200MPa以上の耐力が得られない。一方、Zn含有量が8.0質量%を越え又はMg含有量が2.5質量%を越えると、押出形材に対し潰し加工前に所定の復元処理を行っても、潰し加工による亀裂の発生を防止できず、同時に、潰し加工により付与される引張残留応力を低減できず、耐応力腐食割れ性が顕著に低下する。高強度化及び軽量化の観点からは、Zn含有量、Mg含有量はより高合金側、例えばそれぞれ5.0〜8.0質量%、1.0〜2.5質量%、合計で6.0〜10.5質量%が望ましい。
Hereinafter, the 7000 series aluminum alloy member and the manufacturing method thereof according to the present invention will be specifically described.
(Aluminum alloy composition)
First, the composition of the 7000 series aluminum alloy according to the present invention will be described. However, this composition itself is known as a 7000 series aluminum alloy.
Zn: 3.0-8.0 mass%
Mg: 0.4 to 2.5% by mass
Zn and Mg are elements that improve the strength of the 7000 series aluminum alloy by forming MgZn2 which is an intermetallic compound. When the Zn content is less than 3.0 mass% or the Mg content is less than 0.4 mass%, the proof stress of 200 MPa or more necessary as a practical material cannot be obtained. On the other hand, if the Zn content exceeds 8.0% by mass or the Mg content exceeds 2.5% by mass, cracks due to the crushing process may occur even if the extruded shape is subjected to a predetermined restoration process before crushing. Generation | occurrence | production cannot be prevented, but the tensile residual stress provided by crushing cannot be reduced simultaneously, and stress corrosion cracking resistance falls remarkably. From the viewpoint of increasing the strength and reducing the weight, the Zn content and the Mg content are higher on the alloy side, for example, 5.0 to 8.0 mass% and 1.0 to 2.5 mass%, respectively, for a total of 6. 0-10.5 mass% is desirable.

Cu:0.05〜2.0質量%
Cuは7000系アルミニウム合金の強度を向上させる元素である。Cu含有量が0.05質量%未満では十分な強度向上効果がなく、一方、2.0質量%を越えると押出加工性の低下を招く。Cu含有量は、望ましくは0.5〜1.5質量%である。
Ti:0.005〜0.2質量%
Tiは7000系アルミニウム合金の鋳造時に結晶粒を微細化して、押出形材の成形性(潰し加工性)を向上させる作用があり、0.005質量%以上添加する。一方、0.2質量%を越えるとその作用が飽和し、かつ粗大な金属間化合物が晶出して、かえって成形性を低下させる。
Cu: 0.05-2.0 mass%
Cu is an element that improves the strength of the 7000 series aluminum alloy. When the Cu content is less than 0.05% by mass, there is no sufficient strength improvement effect, while when it exceeds 2.0% by mass, the extrusion processability is lowered. The Cu content is desirably 0.5 to 1.5 mass%.
Ti: 0.005 to 0.2% by mass
Ti has the effect of refining crystal grains during casting of a 7000 series aluminum alloy to improve the formability (crushing workability) of the extruded profile, and is added in an amount of 0.005% by mass or more. On the other hand, when the content exceeds 0.2% by mass, the action is saturated and a coarse intermetallic compound is crystallized, which deteriorates the formability.

Mn:0.01〜0.3質量%
Cr:0.01〜0.3質量%
Zr:0.01〜0.3質量%
Mn,Cr,Zrは7000系アルミニウム合金押出形材の再結晶を抑制して、結晶組織を微細再結晶又は繊維状組織とし、耐応力腐食割れ性を向上させる作用があるため、その1種又は2種以上を上記範囲内で添加する。
不可避不純物
7000系アルミニウム合金の主要な不可避不純物として、Fe及びSiが挙げられる。7000系アルミニウム合金の諸特性を低下させないため、Fe:0.35質量%以下、Si:0.3質量%以下に制限される。
Mn: 0.01 to 0.3% by mass
Cr: 0.01-0.3 mass%
Zr: 0.01 to 0.3% by mass
Mn, Cr, Zr has the effect of suppressing the recrystallization of the 7000 series aluminum alloy extruded shape and making the crystal structure a fine recrystallized or fibrous structure and improving the stress corrosion cracking resistance. Two or more kinds are added within the above range.
Inevitable impurities Fe and Si are the main inevitable impurities of the 7000 series aluminum alloy. In order not to deteriorate various properties of the 7000 series aluminum alloy, the content is limited to Fe: 0.35 mass% or less and Si: 0.3 mass% or less.

(アルミニウム合金部材の製造方法)
本発明に係る7000系アルミニウム合金部材は、上記組成を有し、複数の板から構成される7000系アルミニウム合金押出形材をプレス焼き入れで製造した後(通常、数十日〜数ヶ月の保管期間がある)、同形材の長手方向に沿った全部又は一部の領域に対し、0.4℃/秒以上の昇温速度で加熱し、200〜550℃の温度範囲に0秒を超え60秒以下保持し、次いで0.5℃/秒以上の冷却速度で冷却する復元処理を施し、復元処理後72時間以内に、前記領域に押出方向に対し垂直方向の潰し加工を、前記複数の板のうち最も大きく曲げ変形を受けた板の板厚をtとし、曲げ内側半径の最小値をRとしたとき、1.5mm≦t≦4.0mm、3t/2≦R≦10tとなる条件で施し、さらに部材全体に時効処理を施すことにより製造することができる。
(Method for producing aluminum alloy member)
The 7000 series aluminum alloy member according to the present invention has the above composition and is manufactured by press-quenching a 7000 series aluminum alloy extruded section composed of a plurality of plates (usually storage for several tens of days to several months). The whole or part of the region along the longitudinal direction of the isomorphic material is heated at a temperature rising rate of 0.4 ° C./second or more, and the temperature range of 200 to 550 ° C. exceeds 0 second and exceeds 60 seconds. A restoration process is performed in which the sheet is held for 2 seconds or less and then cooled at a cooling rate of 0.5 ° C./second or more. Within 72 hours after the restoration process, the areas are crushed in a direction perpendicular to the extrusion direction. Where t is the thickness of the plate that has undergone the largest bending deformation, and R is the minimum value of the inner radius of bending, with the conditions of 1.5 mm ≦ t ≦ 4.0 mm and 3t / 2 ≦ R ≦ 10 t Made by applying aging treatment to the entire component It can be.

素材である押出形材は、典型的には対向配置された一対のフランジとそれらを連結する1又は2以上のウエブからなり、これには例えば断面口型、日型、目型などほか、さらにフランジがウエブの左右に突出したものなどが含まれる。フランジ又はウエブは板状であるが、これには多少湾曲したものも含まれる。この押出形材を、一対のフランジが互いに接近する方向に潰し加工した場合、ウエブが最も大きく(大きい曲率で)曲げ変形を受けた板となる。以下、潰し加工により最も大きく曲げ変形を受ける板をウエブと称することにする。
本発明において、押出形材のウエブの板厚tを1.5mm≦t≦4.0mmと比較的厚めに規定したのは、本発明に係る7000系アルミニウム合金部材の用途として、主としてドアビームやバンパーリインフォース等の自動車用補強部材を想定したためである。
The extruded shape material is typically composed of a pair of opposed flanges and one or more webs connecting them, including, for example, a cross-sectional mouth shape, a date shape, an eye shape, and the like. This includes flanges protruding to the left and right of the web. The flange or web is plate-like, but this includes one that is somewhat curved. When this extruded profile is crushed in a direction in which the pair of flanges approach each other, the web is the plate that is subjected to the largest bending deformation (with a large curvature). Hereinafter, a plate that undergoes the largest bending deformation by crushing is referred to as a web.
In the present invention, the sheet thickness t of the extruded profile web is defined to be relatively thick as 1.5 mm ≦ t ≦ 4.0 mm because the application of the 7000 series aluminum alloy member according to the present invention mainly includes door beams and bumpers. This is because an automobile reinforcing member such as reinforcement is assumed.

プレス焼き入れで製造された押出形材は、自然時効により金属間化合物が析出し、硬化しているが、潰し加工の前に前記復元処理を受けることで金属間化合物が再固溶し、押出形材は軟化し、成形性(潰し加工性)が向上する。これにより、押出形材を潰し加工したとき、曲げ変形したウエブの曲げ外側に亀裂が発生するのを防止し、同時に、同ウエブに発生する引張残留応力を低減することができる。   Extruded shapes produced by press quenching have intermetallic compounds precipitated and hardened by natural aging, but the intermetallic compounds are re-dissolved by undergoing the restoration process before crushing, and extruded. The shape material is softened and the moldability (crushing workability) is improved. As a result, when the extruded shape member is crushed, it is possible to prevent cracks from occurring on the outer side of the bent web, and at the same time, to reduce the tensile residual stress generated in the web.

前記復元処理において、昇温速度が0.4℃/秒未満では、昇温過程において金属間加工物の析出が促進され、復元処理の効果が得られない。保持温度(実体温度)が200℃未満では、自然時効で析出した金属間化合物が再固溶せず、むしろ析出が促進されて粗大化し、一方、保持温度が550℃を越えると、押出形材がO材化し、いずれにしても時効処理後に必要な強度が得られない。保持時間は少なくとも0秒を越えることが必要である。要するに、押出形材が保持温度に到達後、同温度に所定時間保持してから冷却してもよく、直ちに冷却してもよい。保持時間の上限は特に限定的ではないが、例えば60秒以内の短時間で済ます方が生産効率の点で望ましく、さらに10秒以内、5秒以内のより短時間が望ましい。加熱手段として例えば高周波誘導加熱装置又は硝石炉を利用することができる。
また、保持温度からの冷却速度が0.5℃/秒未満の緩冷却では、冷却過程で再び金属間化合物の析出が生じ、この復元処理の効果が弱まり又は失われる。なお、従来の復元処理では、冷却過程の冷却速度について特に考慮されていなかった。
In the restoration process, if the rate of temperature rise is less than 0.4 ° C./second, precipitation of the intermetallic workpiece is promoted during the temperature raising process, and the effect of the restoration process cannot be obtained. When the holding temperature (substance temperature) is less than 200 ° C., the intermetallic compound precipitated by natural aging does not re-dissolve, but rather the precipitation is accelerated and coarsened, whereas when the holding temperature exceeds 550 ° C., the extruded shape However, in any case, the required strength cannot be obtained after the aging treatment. The holding time needs to exceed at least 0 seconds. In short, after the extruded profile reaches the holding temperature, it may be cooled after being held at the same temperature for a predetermined time, or may be cooled immediately. Although the upper limit of the holding time is not particularly limited, for example, it is preferable in terms of production efficiency that a short time of 60 seconds or less is desirable, and a shorter time of 10 seconds or less and 5 seconds or less is more desirable. As the heating means, for example, a high frequency induction heating device or a glass furnace can be used.
Further, when the cooling rate from the holding temperature is less than 0.5 ° C./second, the intermetallic compound is precipitated again in the cooling process, and the effect of the restoration treatment is weakened or lost. In the conventional restoration process, the cooling rate in the cooling process is not particularly considered.

上記復元処理後、押出形材が自然時効により再硬化する前に潰し加工を行う。具体的には、復元処理後、72時間以内に潰し加工を行うことが望ましい。潰し加工後のウエブの曲げ内側半径の最小値をRとしたとき、1.5t≦Rを満たす潰し加工率であれば、曲げ変形したウエブの曲げ外側に亀裂が発生するのを防止でき、同時にウエブに発生する引張残留応力の増大が防止できる。しかし、R<1.5tでは、押出形材を潰し加工する前に上記復元処理を行っても、ウエブの曲げ外側に亀裂が発生するのを防止できない。同時に、ウエブに発生する引張残留応力が増大するのを防止できず、部材の耐応力腐食割れ性が低下する。一方、R>10tでは、押出形材を潰し加工する前に上記復元処理を行わなくても(押出形材がT1状態でも)亀裂の発生がない。   After the restoration process, the extruded profile is crushed before it is re-cured by natural aging. Specifically, it is desirable to perform crushing within 72 hours after the restoration process. When the minimum value of the bending inner radius of the web after crushing is R, if the crushing rate satisfies 1.5 t ≦ R, it is possible to prevent cracks from occurring on the outer side of the bent web, and at the same time An increase in the tensile residual stress generated in the web can be prevented. However, if R <1.5t, cracks cannot be prevented from occurring on the outer side of the web even if the restoration process is performed before the extruded profile is crushed. At the same time, it is impossible to prevent an increase in the tensile residual stress generated in the web, and the stress corrosion cracking resistance of the member is lowered. On the other hand, when R> 10t, cracks do not occur even if the restoration process is not performed before the extruded profile is crushed (even if the extruded profile is in the T1 state).

潰し加工後の時効処理は、通常の7000系アルミニウム合金で行われている周知の条件でよい。この時効処理により、製品である7000系アルミニウム合金部材において、200MPa以上の強度(0.2%耐力値)が確保される。
上記製造方法で製造された7000系アルミニウム合金部材は、高強度材であるにも関わらず、潰し加工を施した領域のウエブに亀裂の発生がなく、ウエブの引張残留応力σsrと部材の0.2%耐力値σ0.2の比Y(σsr/σ0.2)が、7000系アルミニウム合金のMg含有量[Mg]とZn含有量[Zn] の合計X(=[Mg]+[Zn])との間で、下記式(1)を満たし、優れた耐応力腐食割れ性を示す。
Y≦−0.1X+1.4 ・・・(1)
The aging treatment after the crushing process may be performed under the well-known conditions performed with a normal 7000 series aluminum alloy. By this aging treatment, a strength (0.2% proof stress value) of 200 MPa or more is ensured in the product 7000 series aluminum alloy member.
Although the 7000 series aluminum alloy member manufactured by the above-described manufacturing method is a high-strength material, the web in the area subjected to the crushing process does not generate cracks, and the tensile residual stress σsr of the web is reduced to 0. The ratio Y (σsr / σ 0.2 ) of the 2% proof stress value σ 0.2 is the sum X of Mg content [Mg] and Zn content [Zn] of the 7000 series aluminum alloy (= [Mg] + [Zn ]), The following formula (1) is satisfied, and excellent stress corrosion cracking resistance is exhibited.
Y ≦ −0.1X + 1.4 (1)

図1に示すグラフは、ZnとMgの合計含有量X(=[Zn]+[Mg])と、引張残留応力σrsと0.2%耐力σ0.2の比Y(σrs/σ0.2)からなるX−Y座標に、後述する実施例のデータをプロット(△、□)したものであり、図中のラインは、Y=−0.1X+1.4で表される直線である。図1において、△は実施例のNo.1〜6に相当し、これらは全てY≦−0.1X+1.4の領域に入り、表2に示すとおり、耐応力腐食割れ性に優れている。一方、□はNo.7〜14に相当し、全てY>−0.1X+1.4の領域に入り、表2に示すとおり、耐応力腐食割れ性が劣る。また、表2に示すとおり、Y≦−0.1X+1.4の領域に入るNo.1〜6はいずれもウエブに亀裂がなく、Y>−0.1X+1.4の領域に入るNo.7〜14はいずれもウエブに亀裂が生じている。
なお、図1において、Yの分母である0.2%耐力(σ0.2)は、後述する実施例に示すように、プレス焼き入れで製造された押出材を自然時効させた後、復元処理及び拡管加工を行うことなく時効処理した箇所の0.2%耐力である。
The graph shown in FIG. 1, the total content of Zn and Mg X (= [Zn] + [Mg]), tensile residual stresses Shigumars and 0.2% proof stress sigma 0.2 ratio Y (σrs / σ 0. 2 ) are plotted (Δ, □) of data of examples described later on XY coordinates, and the line in the figure is a straight line represented by Y = −0.1X + 1.4. In FIG. 1 to 6 and these all fall within the range of Y ≦ −0.1X + 1.4 and are excellent in stress corrosion cracking resistance as shown in Table 2. On the other hand, □ indicates no. It corresponds to 7 to 14, all enter the region of Y> −0.1X + 1.4, and as shown in Table 2, the stress corrosion cracking resistance is inferior. In addition, as shown in Table 2, No. 1 entering the region of Y ≦ −0.1X + 1.4. Nos. 1 to 6 have no cracks in the web and No. 1 in the range of Y> −0.1X + 1.4. In all of Nos. 7 to 14, the web is cracked.
In FIG. 1, the 0.2% proof stress (σ 0.2 ), which is the denominator of Y, is restored after natural aging of the extruded material produced by press quenching, as shown in the examples described later. It is 0.2% proof stress of the part age-treated without performing processing and pipe expansion processing.

表1に示す7000系アルミニウム合金を熱間押出成形し、押出直後にオンラインでファン空冷(プレス焼き入れ)し、図2Aに示すように、対向配置された一対のフランジ(内側フランジ1,外側フランジ2)と、これらを垂直に接続する2個のウエブ3,4からなる断面略口型(突出フランジあり)の押出形材を製造した。この押出形材はドアビームを想定したもので、高さ30.0mm、外側フランジ1の板厚4.0mm、幅40.0mm、内側フランジ2の板厚4.0mm、幅50.0mm、両ウエブ3,4の板厚2.0mm又は4.0mm、外側フランジ1は両ウエブ3,4から左右に各5mm突出し、内側フランジ2は両ウエブ3,4から左右に各10mm突出している。   7000 series aluminum alloy shown in Table 1 is hot-extrusion molded, and fan air cooling (press quenching) is performed on-line immediately after extrusion, and a pair of opposed flanges (inner flange 1, outer flange) as shown in FIG. 2) and an extruded profile having a substantially mouth-shaped cross section (with a protruding flange) composed of two webs 3 and 4 that connect them vertically. This extruded shape is assumed to be a door beam. Height 30.0mm, outer flange 1 thickness 4.0mm, width 40.0mm, inner flange 2 thickness 4.0mm, width 50.0mm, both webs 3 and 4 have a thickness of 2.0 mm or 4.0 mm, the outer flange 1 protrudes from both webs 3 and 4 by 5 mm to the left and right, and the inner flange 2 protrudes from both webs 3 and 4 by 10 mm to the left and right.

プレス焼き入れ後のNo.1〜14の押出形材を所定長さに切断して、No.1〜14のそれぞれについて2本ずつの試験材(押出形材)を採取し、室温で20日間放置して自然時効させた後、高周波誘導加熱装置を用い、表1に示す種々の昇温速度、到達温度(実体温度)、保持時間、及び冷却速度で復元処理を施した(No.11のみ施さず)。復元処理は試験材の長手方向に沿った一部領域(端部領域)にのみ施した。   No. after press quenching Nos. 1 to 14 are cut into a predetermined length, Two test materials (extruded shapes) for each of 1 to 14 were collected, allowed to stand at room temperature for 20 days and allowed to naturally age, and then various heating rates shown in Table 1 using a high-frequency induction heating device. Then, the restoration process was performed at the ultimate temperature (substance temperature), the holding time, and the cooling rate (only No. 11 was applied). The restoration process was performed only on a partial region (end region) along the longitudinal direction of the test material.

Figure 2017214656
Figure 2017214656

復元処理後、表1に示す時間経過した後、図2Bに示すように、試験材5を水平台6上に置き、水平台6の上方に配置された潰し加工用治具7で垂直にプレスし、同時に図示しない水平加工治具(特許文献3に記載された水平負荷用治具9参照)でウエブ3,4に内向きの負荷を加え、試験材5の復元処理した端部領域(No.11のみ復元処理していない領域)を、潰し加工用治具7の傾斜面7aで上下方向に潰し加工した。潰し加工により試験材5のウエブ3,4が曲げ変形し、中空部の内側に張り出した。この潰し加工において、潰し加工用治具7のストロークを一定とし、水平台6上で試験材5の長手方向(図2Bにおいて左右方向)の位置を調整することにより、No.1〜14の試験材5(各2本)の潰し加工率、すなわちウエブ3,4の曲げ半径を調整した。
潰し加工後、No.1〜14の試験材(各2本)全体に130℃×8時間の時効処理を施した。
時効処理後、No.1〜14の一方の試験材を用い、下記要領で引張試験、ウエブの曲げ外側の亀裂発生の有無の検査、ウエブの曲げ内側半径(最小値R)の測定、及びウエブの引張残留応力の測定を行った。また、No.1〜14のもう1つの試験材を用い、耐応力腐食割れ性試験を行った。その結果を表2に示す。
After the restoration process, after the time shown in Table 1 has elapsed, as shown in FIG. 2B, the test material 5 is placed on the horizontal base 6 and vertically pressed by the crushing processing jig 7 disposed above the horizontal base 6. At the same time, an inward load is applied to the webs 3 and 4 with a horizontal processing jig (not shown) (see horizontal load jig 9 described in Patent Document 3), and the end region (No. ..., Only the .11 region that has not been restored is crushed in the vertical direction by the inclined surface 7 a of the crushing jig 7. The webs 3 and 4 of the test material 5 were bent and deformed by the crushing process, and protruded inside the hollow portion. In this crushing process, the stroke of the crushing jig 7 is made constant, and the position in the longitudinal direction (left and right direction in FIG. 2B) of the test material 5 is adjusted on the horizontal table 6. The crushing rate of 1 to 14 test materials 5 (two each), that is, the bending radius of the webs 3 and 4 was adjusted.
After crushing, no. Aging treatment of 130 ° C. × 8 hours was performed on the whole of 1 to 14 test materials (two each).
After aging treatment, no. Using one of the test materials 1 to 14, a tensile test, an inspection for the presence or absence of cracks on the outer side of the web, the measurement of the inner radius of bending (minimum value R), and the measurement of the tensile residual stress of the web Went. No. Using another test material of 1 to 14, a stress corrosion cracking resistance test was conducted. The results are shown in Table 2.

(引張試験)
試験材5の復元処理していない領域からJIS5号試験片を採取し、JISZ2241に規定する金属材料試験方法に準じて引張試験を行い、0.2%耐力(σ0.2)を測定した。
(亀裂発生の有無)
試験材5の潰し加工した領域のウエブ3,4を目視で観察し、ウエブ3,4の曲げ外側における亀裂発生の有無を検査した。亀裂は主として試験材5の潰し加工した端面近傍に生じていた。
(曲げ内側半径の最小値R)
試験材5の潰し加工した端面においてウエブ3,4の曲げ内側半径が最も小さくなることから、同端面においてウエブ3,4の曲げ内側半径を測定した。
(Tensile test)
A JIS No. 5 test piece was collected from a region of the test material 5 not subjected to the restoration treatment, and subjected to a tensile test according to the metal material test method specified in JISZ2241, and 0.2% proof stress (σ 0.2 ) was measured.
(Presence or absence of cracks)
The webs 3 and 4 in the crushed region of the test material 5 were visually observed, and the presence or absence of cracks on the outside of the webs 3 and 4 was inspected. Cracks occurred mainly in the vicinity of the crushed end face of the test material 5.
(Minimum bending radius R)
Since the bending inner radius of the webs 3 and 4 is the smallest at the crushed end surface of the test material 5, the bending inner radius of the webs 3 and 4 was measured at the same end surface.

(ウエブの引張残留応力)
残留応力の測定法は切断法により次の手順で行った。測定対象位置として、図2に示す潰し加工開始位置A、端部位置B、及び中間位置Cを選定し(いずれも高さ中央位置)、これら測定対象位置表面をサンドペーパーで研磨後、アセトン洗浄し、この研磨部位に歪みゲージを瞬間接着剤で接着し、24時間室温放置後、歪みゲージのリード線を歪み計に接続してゼロ点設定をし、歪みゲージの周囲を金属のこぎりで10mm角に切断して応力開放し、切断後の歪み量εを計測し、次式にて残留応力値σrsを算出した。σrs=−E×ε(E;ヤング率)、ここでE=68894N/mmとした。
なお、No.1〜14の試験材全てにおいて、潰し加工開始位置Aで測定した引張残留応力値が最大値となった。これは、潰し加工開始位置Aにおいて最も材料の拘束が大きく、一方、端部位置B及び中間位置Cでは材料の拘束が比較的小さく、潰し加工による歪みが解放されたためではないかと推測される。従って、表2に記載した残留応力値σrsは、潰し加工開始位置Aで測定した値である。
(Tensile residual stress of web)
The residual stress was measured by the following procedure using a cutting method. As the measurement target positions, the crushing start position A, the end position B, and the intermediate position C shown in FIG. 2 are selected (all at the height center position), and these measurement target position surfaces are polished with sandpaper and then washed with acetone. Then, a strain gauge is bonded to this polished part with a momentary adhesive, left at room temperature for 24 hours, the strain gauge lead wire is connected to a strain gauge, a zero point is set, and the periphery of the strain gauge is 10 mm square with a metal saw. The stress was released by cutting, the strain amount ε after cutting was measured, and the residual stress value σrs was calculated by the following equation. σrs = −E × ε (E; Young's modulus), where E = 68894 N / mm 2 .
In addition, No. In all the test materials 1 to 14, the tensile residual stress value measured at the crushing start position A was the maximum value. This is presumably because the material restraint is the largest at the crushing start position A, while the material restraint is relatively small at the end position B and the intermediate position C, and the distortion due to the crushing process is released. Therefore, the residual stress value σrs shown in Table 2 is a value measured at the crushing processing start position A.

(耐応力腐食割れ性)
クロム酸促進法による耐応力腐食割れ試験を行った。潰し加工した試験材を用いて、90℃の試験溶液に最大16時間まで浸漬し、応力腐食割れを目視で観察した。また、試験溶液は、蒸留水に参加クロム36g、2クロム酸カリウム30g及び食塩3g(1リットルあたり)を加えて作製した。試験は1時間毎に試験材を溶液から取り出し、割れ発生の有無を確認し、割れ無し又は割れ発生までの時間が12時間以上であったものを耐応力腐食割れ性が優れる(○)と評価し、割れ発生までの時間が12時間未満であったものを劣る(×)と評価した。なお、応力腐食割れは全て潰し加工開始位置A(図2(b)参照)の付近で生じていた。
(Stress corrosion cracking resistance)
The stress corrosion cracking test by the chromic acid acceleration method was conducted. Using the crushed test material, it was immersed in a test solution at 90 ° C. for a maximum of 16 hours, and stress corrosion cracking was visually observed. The test solution was prepared by adding 36 g of chromium added to distilled water and 30 g of potassium dichromate and 3 g of sodium chloride (per liter). Tests were taken out of the solution every hour to check for cracks, and those with no cracks or cracks that took 12 hours or more were evaluated as having excellent stress corrosion cracking resistance (◯). Then, the case where the time until the occurrence of cracking was less than 12 hours was evaluated as inferior (x). All stress corrosion cracking occurred near the crushing start position A (see FIG. 2B).

Figure 2017214656
Figure 2017214656

残留応力値(σrs)と0.2%耐力値(σ0.2)から、両者の比Y(=σrs/σ0.2)を算出した。また、Zn含有量[Zn]とMg含有量[Mg]から、ZnとMgの合計含有量X(=[Zn]+[Mg])、及び前記式(1)の右辺(−0.1X+1.4)の値を算出した。以上の算出結果を基に、X,Yの値が前記関係式(1)を満たす場合を○と判定し、満たさない場合を×と判定した。以上の算出結果及び判定結果を表2に示す。
表1,2から、本発明に規定する合金組成を有し、本発明に規定する条件で復元処理及び潰し加工を行ったNo.1〜6の試験材は、潰し加工後のウエブに亀裂がなく、時効処理後の耐力値が200MPa以上で、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たし、いずれも耐応力腐食割れ性が優れる。
Residual stress value from (σrs) and 0.2% proof stress (sigma 0.2), was calculated both the ratio Y (= σrs / σ 0.2) . Further, from the Zn content [Zn] and the Mg content [Mg], the total content X (= [Zn] + [Mg]) of Zn and Mg, and the right side (−0.1X + 1. The value of 4) was calculated. Based on the above calculation results, a case where the values of X and Y satisfy the relational expression (1) was determined as ◯, and a case where the values did not satisfy the relationship was determined as x. Table 2 shows the above calculation results and determination results.
From Tables 1 and 2, No. 1 having an alloy composition defined in the present invention and subjected to restoration treatment and crushing under the conditions defined in the present invention. The test materials 1 to 6 have no cracks in the web after crushing, the proof stress after aging treatment is 200 MPa or more, and Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg ]) Satisfy | fills said Formula (1), and all are excellent in stress corrosion cracking resistance.

一方、No.7の試験材は、Zn及びMgの含有量が過剰で、潰し加工によりウエブに亀裂が入り、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性が劣る。
No.8の試験材は、復元処理の冷却速度が遅いため復元処理の効果が失われ、潰し加工によりウエブに亀裂が入り、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性が劣る。
No.9の試験材は、復元処理の到達温度が低いため復元処理の効果がなく、時効処理により耐力が向上せず、比較的低Zn、Mgであるにも関わらず、潰し加工によりウエブに亀裂が入るのを防止できなかった。また、Y(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性も劣る。
On the other hand, no. In the test material No. 7, the contents of Zn and Mg were excessive, the web was cracked by crushing, and Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg]) were The formula (1) is not satisfied, and the stress corrosion cracking resistance is inferior.
No. 8 of the test material, restoration effects for restoration process the cooling rate is slow processing is lost, the web to be cracked by crushing processing, and Y (= σrs / σ 0.2) and X (= [Zn] + [Mg] does not satisfy the formula (1), and the stress corrosion cracking resistance is poor.
No. The test material of No. 9 has no effect of the restoration process due to the low arrival temperature of the restoration process, and the aging process does not improve the yield strength, and the web is cracked by the crushing process despite being relatively low in Zn and Mg. I couldn't prevent it from entering. Further, Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg]) do not satisfy the formula (1), and the stress corrosion cracking resistance is inferior.

No.10の試験材は、R/tが小さすぎる(潰し加工率が高すぎる)ため、復元処理の条件は適正であったが、比較的低Zn,Mgであるにも関わらず、潰し加工による亀裂の発生を防止できなかった。また、Y(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性も劣る。
No.11の試験材は、復元処理を行っていないため、潰し加工によりウエブに亀裂が発生した。また、Y(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性も劣る。
No.12の試験材は、復元処理から潰し加工を行うまでの時間が長いため、復元処理の効果が失われ、潰し加工によりウエブに亀裂が入り、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性が劣る。
No. Since the test material of No. 10 had R / t too small (the crushing rate was too high), the conditions for the restoration treatment were appropriate, but despite the relatively low Zn and Mg, cracks caused by crushing Could not be prevented. Further, Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg]) do not satisfy the formula (1), and the stress corrosion cracking resistance is inferior.
No. Since the test material of No. 11 was not restored, cracks occurred in the web by crushing. Further, Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg]) do not satisfy the formula (1), and the stress corrosion cracking resistance is inferior.
No. Since the test material No. 12 takes a long time from the restoration process to the crushing process, the effect of the restoration process is lost, the web is cracked by the crushing process, and Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg]) does not satisfy the formula (1), and the stress corrosion cracking resistance is poor.

No.13の試験材は、復元処理の昇温速度が小さいため復元処理の効果が得られず、潰し加工によりウエブに亀裂が入り、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性が劣る。
No.14の試験材は、復元処理の冷却速度が小さいため復元処理の効果が失われ、潰し加工によりウエブに亀裂が入り、かつY(=σrs/σ0.2)とX(=[Zn]+[Mg])が前記式(1)を満たさず、耐応力腐食割れ性が劣る。
No. In the test material No. 13, since the temperature increase rate of the restoration process is small, the effect of the restoration process is not obtained, the web is cracked by crushing, and Y (= σrs / σ 0.2 ) and X (= [Zn) ] + [Mg]) does not satisfy the formula (1), and the stress corrosion cracking resistance is poor.
No. The test material No. 14 loses the effect of the restoration process due to the low cooling rate of the restoration process, the web is cracked by crushing, and Y (= σrs / σ 0.2 ) and X (= [Zn] + [Mg] does not satisfy the formula (1), and the stress corrosion cracking resistance is poor.

1,2 フランジ
3,4 ウエブ
5 試験材(押出形材)
7 潰し加工用治具
1, 2 Flange 3, 4 Web 5 Test material (extrusion profile)
7 Crushing jig

Claims (2)

Zn:3.0〜8.0質量%、Mg:0.4〜2.5質量%、Cu:0.05〜2.0質量%、Ti:0.005〜0.2質量%を含有し、さらに、Mn:0.01〜0.3質量%、Cr:0.01〜0.3質量%、Zr:0.01〜0.3質量%の1種又は2種以上を含有し、残部Al及び不可避不純物からなる組成を有し、複数の板で構成され、プレス焼き入れで製造された7000系アルミニウム合金押出形材の長手方向に沿った少なくとも一部の領域に、押出方向に対し垂直方向の潰し加工を施して部材化する7000系アルミニウム合金部材の製造方法において、潰し加工の前に、前記押出形材の少なくとも前記領域に対し、0.4℃/秒以上の昇温速度で加熱し、200〜550℃の温度範囲に0秒を超え60秒以下保持し、次いで0.5℃/秒以上の冷却速度で冷却する復元処理を施し、復元処理後72時間以内に、前記複数の板のうち最も大きく曲げ変形を受けた板の板厚をtとし、曲げ内側半径の最小値をRとしたとき、1.5mm≦t≦4.0mm、3t/2≦R≦10tとなる条件で前記潰し加工を施し、潰し加工後、部材全体に時効処理を施すことを特徴とする耐応力腐食割れ性に優れた7000系アルミニウム合金部材の製造方法。 Zn: 3.0-8.0 mass%, Mg: 0.4-2.5 mass%, Cu: 0.05-2.0 mass%, Ti: 0.005-0.2 mass% Furthermore, Mn: 0.01 to 0.3% by mass, Cr: 0.01 to 0.3% by mass, Zr: 0.01 to 0.3% by mass, or one or more, and the balance A composition composed of Al and inevitable impurities, composed of a plurality of plates, and perpendicular to the extrusion direction at least in a region along the longitudinal direction of a 7000 series aluminum alloy extruded profile manufactured by press quenching In a manufacturing method of a 7000 series aluminum alloy member that is crushed in a direction to form a member, before crushing, at least the region of the extruded shape member is heated at a temperature increase rate of 0.4 ° C./second or more. And hold in the temperature range of 200 to 550 ° C. for more than 0 seconds and not more than 60 seconds. The sheet is subjected to a restoration process of cooling at a cooling rate of 0.5 ° C./second or more, and within 72 hours after the restoration process, the thickness of the plate that has undergone the largest bending deformation among the plurality of plates is defined as t, When the minimum value of the radius is R, the crushing process is performed under the conditions of 1.5 mm ≦ t ≦ 4.0 mm and 3t / 2 ≦ R ≦ 10 t, and after the crushing process, the entire member is subjected to an aging treatment. A method for producing a 7000 series aluminum alloy member having excellent stress corrosion cracking resistance. 前記7000系アルミニウム合金押出形材が、対向配置された一対のフランジとそれらを連結する1又は2以上のウエブからなり、前記最も大きく曲げ変形を受けた板が前記ウエブであることを特徴とする請求項1に記載された耐応力腐食割れ性に優れた7000系アルミニウム合金部材の製造方法。 The 7000 series aluminum alloy extruded profile consists of a pair of flanges arranged opposite to each other and one or more webs connecting them, and the plate that has undergone the greatest bending deformation is the web. The manufacturing method of the 7000 series aluminum alloy member excellent in the stress corrosion cracking resistance described in Claim 1.
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