TWI609973B - 沃斯田鐵系不鏽鋼箔 - Google Patents

沃斯田鐵系不鏽鋼箔 Download PDF

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Publication number
TWI609973B
TWI609973B TW105126257A TW105126257A TWI609973B TW I609973 B TWI609973 B TW I609973B TW 105126257 A TW105126257 A TW 105126257A TW 105126257 A TW105126257 A TW 105126257A TW I609973 B TWI609973 B TW I609973B
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Taiwan
Prior art keywords
stainless steel
steel foil
orientation
less
foil
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TW105126257A
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English (en)
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TW201713779A (zh
Inventor
Hiroto Unno
Naoya SAWAKI
Naoki Fujimoto
Masahiro Fukuda
Tomohiro Uno
Toru Inaguma
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Nippon Steel & Sumikin Materials Co Ltd
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Publication of TW201713779A publication Critical patent/TW201713779A/zh
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C21D9/48—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals deep-drawing sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
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    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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Abstract

本發明提供一種沃斯田鐵系不鏽鋼箔，其即使是板厚在60μm以下的極薄不鏽鋼箔，其鼓膨成形性仍高且對鼓膨成形上的變形異向性仍小。 本發明之沃斯田鐵系不鏽鋼箔，其特徵在於：其板厚在5μm以上且60μm以下，再結晶率為90%以上且100%以下，並且在測定視野内具有下述面積率合計在20%以下的集合組織：自{112}＜111＞方位起算方位差在10°以内的結晶方位之面積率、自{110}＜112＞方位起算方位差在10°以内結晶方位之面積率，以及自{110}＜001＞方位起算方位差在10°以内結晶方位之面積率。

Description

沃斯田鐵系不鏽鋼箔
本發明是有關於一種沃斯田鐵系不鏽鋼箔。特別是，有關一種儘管板厚極薄仍具有良好成形性之沃斯田鐵系不鏽鋼箔。
隨著電子機器之小型化、輕量化，電子機器可攜帶化、移動化的進展，搭載在許多的電子機器之 鋰離子電池等，係被要求電池的小型化、輕量化。特別是在智慧型手機等的電子機器所被要求之電池的小型化、輕量化，係要求時代最尖端水準的規格。
前，適合智慧型手機的鋰離子電池之電池殼體，係使用將罐型的鋁薄板和樹脂薄膜層疊而成之鋁箔。特別是以提升單位體積的電容量密度作為目的而使用許多樹脂薄膜層疊鋁箔。最近，以進一步小型輕量化作為目的，係被要求更薄的外部裝飾材。但是，為基材之鋁箔中，若是使其薄化，在製造過程就容易發生有孔洞，無法確保水分阻障性，又，薄化引起扎刺強度和剛性低落，而有無法確保對來自外部的衝撃和電池的內部膨脹的強度之問題。因此，在鋁箔係逐漸能夠看出對進一步小型化之限度。
因此，強度和剛性比鋁更高的不鏽鋼箔逐漸受到關注。但是，由於與鋁相比，不鏽鋼比重高，在適用於尋求小型化及輕量化之電子機器之電池殼體上，板厚極薄(例如，60μm以下)不鏽鋼箔是必要的。特別是，為謀求電池容量增大，在尋求板厚在60μm以下時被加工性高，例如，成形成為四方罐形状下亦可以均一成形的不鏽鋼箔。
作為極薄的不鏽鋼箔，在專利文獻1係揭示一種厚度25μm以下的不鏽鋼箔。成為極薄的不鏽鋼箔時，係從蝕刻端面在輥軋方向伴隨著裂紋而產生空隙。專利文獻1係揭示該發明為限制5μm以上的夾雜物之個數用以消除上述情形。
又，專利文獻2~4係作為將不鏽鋼箔應用在電池用殼體之例子。各自係揭示以下的例子，在專利文獻2係將厚度20~100μm的不鏽鋼箔，在專利文獻3係將厚度100μm的不鏽鋼箔，專利文獻4係將厚度40~150μm的不鏽鋼箔，進行壓製加工而作為電池用外部裝飾材。
[習知技術文獻] 專利文獻 　　專利文獻1：日本特開2000-273586號公報 　　專利文獻2：日本特開2004-52100號公報 　　專利文獻3：日本特開2013-41788號公報 　　專利文獻4：日本特開2012-92361號公報 　　專利文獻5：日本特開2007-168184號公報
發明概要 發明欲解決之問題 通常，極薄的不鏽鋼箔，係如使用在HDD(Hard Disk Drive)用磁頭彈簧片組件(head gimbal assembly)之彈簧用等，不進行輥軋後退火，而是輥軋後直接，或者施予諸如拉伸退火等使其拉伸強度與耐力提高之熱處理後、進行沖切加工和蝕刻加工。專利文獻1的技術係解決在此種蝕刻加工時所產生的技術問題。
但是，極薄不鏽鋼箔適用於電池殼時，該電池殼是藉由極薄不鏽鋼箔作壓製加工形成的。一般而言，壓製成形可成分成是深衝成形與鼓膨成形。深衝成形，如圓筒深衝為代表者，在材料流入方向上受到拉伸變形，在與流入方向呈垂直之寬方向上壓受到壓縮變形之變形。另一方面，鼓膨成形是箔之板厚方向在垂直面内(以下稱輥軋面)上等2軸拉伸變形之成形。若形成電池殼之類形四方罐形狀時，由於進行鼓膨成形，特別是，由於構成角隅部的不鏽鋼箔之部分是最受到拉伸變形。因此，若配向在變形不利方位上的結晶粒在該部分存在較多時，即使施加壓製加工也不會有充分的變形，而導致斷裂等情事發生。因此，對在輥軋面内任意方向上進行拉伸加工的不鏽鋼箔而言，相較於在特定方位中顯示出良好之拉伸成形性，在任意方位中顯示出某一程度良好之拉伸成形性，即，顯示出小的異向性且良好拉伸成形性，此是期望的事情事。
基於此種狀況，本發明者精心檢討之後的結果發現：若是對處理條件未有任何考量就對不鏽鋼箔施行習知退火處理(例如，輝面退火等)的話，構成不鏽鋼箔結晶粒會朝向粗大化進展，同時此等結晶粒之結晶方位是不欲地集積在特定方位上。一般認為若是朝向特定結晶方式的結晶粒方位集積的話，對於鼓膨成形變形之異向性就會不欲地增大，該不鏽鋼箔之均一成形就變得困難，成形深度亦變小。
在專利文獻2中，係記載將厚度20~100μm的不鏽鋼箔進行壓製加工而應用在電池殼體之例子。但是，專利文獻2中，並未認知到結晶方位之集積方面的問題。因此，若退火温度高，朝向結晶方位集積，專利文獻2之不鏽鋼箔被認為對鼓膨成形變形之異向性是高的。
在專利文獻3中，亦是記載厚度100μm的不鏽鋼箔在電池殼體的應用例。但是，厚度100μm之不鏽鋼箔由於是比較的厚的，被加工性雖高，但因殼的厚度低減而增加電池容量的效果是低的。
在專利文獻4中，係記載將厚度40~150μm的不鏽鋼箔應用在電池外裝材之例子。專利文獻4之技術為、氮化不鏽鋼箔的表層可控制壓製加工時因加工引起的麻田散鐵的生成。藉此，可以說明其確保不鏽鋼箔與樹脂之熱融著部之耐剝離性且抑制壓製加工後樹脂之白化。再者，亦可說明，由於其可抑制因加工引起的麻田散鐵變態而形成表面凹凸，維持表面之平滑性，故壓製會變得良好。
本發明者精心檢討之後的結果：若氮化不鏽鋼箔表層，該部分會硬化，故在壓製加工時容易發生有裂痕{龜裂}。特別是，不鏽鋼箔之板厚若在60μm以下，因表層氮化而成之硬化部分的影響就相對的變大，而不能忽視。即，經表層氮化之極薄不鏽鋼箔若壓製加工，會發生有表面龜裂，無法得到統分的加工成形性。因此，一般認為雖不鏽鋼箔的厚度可變薄，但成形深度會變小。即，電池容量增大效果是少的。
又，專利文獻4中，實施例之板厚幾乎為100μm，故如上所，無法期待其可因厚度低減而有電池容量増大的效果。再者，板厚40μm之實施例則說明成形性惡化之鋼板的許容範圍。此外，其又沒有比此等實施例更薄之板厚的實施例，專利文獻4中記載之技術可以說是無法兼具有不鏽鋼箔厚度作極成薄化以及增大成形深度。
本發明有鑑於上述狀況而完成者，且其目的在於提供一種沃斯田鐵系不鏽鋼箔，其即使是板厚在60μm以下的極薄不鏽鋼箔，其鼓膨成形性仍高且對鼓膨成形上的變形異向性仍小。
又，板厚之下限雖沒有特別限定之必要，但因施予輥軋後之箔的板厚在現實面上的臨界値為5μm左右，故本發明之沃斯田鐵系不鏽鋼箔的厚度作成5～60μm。
用以解決問題之手段 為了解決上述問題，本發明者等進行專心研討而得到以下的見解。 (1)沃斯田鐵系不鏽鋼而言，配向於特定方位(集積)之結晶粒比例若設定在特定範圍以下，即沃斯田鐵系不鏽鋼中，是藉由使差排密度減少且使該結晶粒方位為隨機性的，可使得其對鼓膨成形變形異向性降低，成形深度增大。 (2)為使差排密度減少且使在結晶粒方位為隨機性，導入較多構成輥軋時強軋縮後再結晶時生成核之生成尺寸的差排，其後進行退火，使差排密度減少而再結晶，且再結晶結晶粒會停留在微細的狀態，此是必要的。 (3)較佳的是，藉由確保板厚方向之結晶粒數為3個以上，可確保塑性變形能力(例如，良好之鼓膨成形性)。又，按照板厚而決定板厚方向的結晶粒數之下限即可。 (4)為了抑制表面硬化所致之斷裂(裂紋)，盡力抑制表層氮化係重要的。 (5)藉由確保板厚方向的結晶粒之數目為3個以上，進而將表層的氮濃度設為1.0質量%以下，亦能夠確保耐電解液性。亦即，為了提高耐電解液性，抑制壓製加工後在角隅部之不鏽鋼箔表面的表面粗糙，來保持與樹脂皮膜的密著性係重要的。
本發明係基於該等見解而完成者，且本發明之態樣係如下所示。 (1)一種沃斯田鐵系不鏽鋼箔，其特徵在於：其板厚在5μm以上且60μm以下，並且 前述不鏽鋼箔的再結晶率為90%以上且100%以下， 前述不鏽鋼箔在測定視野内具有下述面積率合計在20%以下的集合組織：自{112}＜111＞方位起算方位差在10°以内的結晶方位之面積率、自{110}＜112＞方位起算方位差在10°以内結晶方位之面積率，以及自{110}＜001＞方位起算方位差在10°以内結晶方位之面積率。 (2)如(1)之沃斯田鐵系不鏽鋼箔，其中前述板厚為5μm以上且25μm以下。 (3)如(1)或(2)項記載之沃斯田鐵系不鏽鋼箔，其中在板厚方向具有結晶粒3個以上。 (4)如(1)到(3)中任一項記載之沃斯田鐵系不鏽鋼箔，其中表層的氮濃度在1.0質量%以下。 (5)如(1)至(4)項中任一項記載之沃斯田鐵系不鏽鋼箔，其中前述沃斯田鐵系不鏽鋼箔的至少一表面層積有樹脂薄膜。 發明效果
本發明可提供一種沃斯田鐵系不鏽鋼箔，其即使是板厚在60μm以下的極薄不鏽鋼箔，其鼓膨成形性仍高，且對於鼓膨成形變形之異向性仍小。本發明之沃斯田鐵系不鏽鋼箔適用於以小型輕量化為目標之鋰離子電池的電池殼。
較佳實施例之詳細說明 以下詳細地說明本發明。 (1.沃斯田鐵系不鏽鋼) [不鏽鋼的材質] 本發明之沃斯田鐵系不鏽鋼箔若是由沃斯田鐵系不鏽鋼構成的話，是沒有特別限制，沃斯田鐵系不鏽鋼是以具有以下所示組成範圍為宜。該組成範圍是以質量%計，含有C:0.080%以下、Si:2.0%以下、Mn:2.0%以下、P:0.045%以下、S:0.030%以下、Ni:5.0%以上11.0%以下、Cr:15.0%以上20.0%以下、Mo:0.30%以下、N：0.05%以下、Cu: 0.50%以上2.50%以下、殘餘部是由Fe與不可避的不純物構成。亦可使用市售沃斯田鐵系不鏽鋼作為上述沃斯田鐵系不鏽鋼。
[板厚：5～60μm] 本發明之沃斯田鐵系不鏽鋼箔係以板厚為5~60μm者作為對象。為了擴大該不鏽鋼箔適用於電池殼時電池容量之増大效果，板厚限定在60μm以下。板厚可以限定為較佳是50μm以下，更佳是40μm以下，又更佳是25μm以下。又，板厚的下限係沒有特別限定，但是考慮製造技術的限度，係以將板厚5μm設作下限。即便板厚5μm，亦能夠享受本發明所得到的效果。
[再結晶率為90%以上且100%以下] 本發明之沃斯田鐵系不鏽鋼箔具有良好鼓膨成形性(塑性變形能力)是必要的。具體而言，輥軋後之組織受到加工，會蓄積諸如差排等晶格缺陷，故結晶粒即使是微細也有高差排密度，而呈硬化。因此，必須按照材料而適當地控制熱處理條件，使得組織再結晶，且使差排密度低。即，為了再結晶組織形成有作為驅動力之差排密度，利用使得再結晶粒内之差排密度減小，並抑制再結晶組織之粗大化，藉此可以確保良好的鼓膨成形性(塑性變形能力)。
又，差排密度測定方法中例示有蝕刻斑(etch pit)法等，但是因為受到測定條件等之影響，定量的測定係困難的。藉由顯微鏡觀察，雖可直接測定差排密度，但是因觀察視野而引起的偏差係較大。在此，本發明者等係發現藉由測定反映差排密度之特性值的再結晶率，而能夠把握是否已進行適當的熱處理。
再結晶率係能夠藉由(已再結晶的結晶之面積)/(觀察面積)來算出。「已再結晶的結晶之面積」，係能夠藉由在光學顯微鏡下觀察沃斯田鐵系不鏽鋼箔的任意剖面來得到。或者，亦可求出前述鋼箔之X線繞射所得到(220)面之繞射峰的半峰寬而算出。半峰寬在0.20度以下的話，再結晶率可視為90%以上；0.15度以下的話，再結晶率可視為95%以上；0.10度以下的話，再結晶率100%。
本發明之沃斯田鐵系不鏽鋼箔之再結晶率，在90%以上即可。再結晶率若在90%以上，差排密度十分低，可確保成形性。較佳是再結晶率為95%以上。後述之集合組織只要符合本發明之規定，再結晶率亦可100%。即，本發明之沃斯田鐵系不鏽鋼箔全體亦可再結晶。
[集合組織] 本發明之沃斯田鐵系不鏽鋼箔藉由再結晶率在上述的範圍，並且控制再結晶過程，而具有特徴性的集合組織。具體而言，本發明之沃斯田鐵系不鏽鋼箔在測定視野内具有下述面積率合計在20%以下的集合組織：自{112}＜111＞方位起算方位差（偏差）在10°以内的結晶方位之面積率、自{110}＜112＞方位起算方位差在10°以内結晶方位之面積率，以及自{110}＜001＞方位起算方位差在10°以内結晶方位之面積率。又，在上述3個方位{112}、{110}、{110}面是顯示與輥軋面平行的面，＜111＞、＜112＞、＜001＞方向是顯示與輥軋方向平行的方向。再者，上述3個方位是以在結晶學上含有等價方位之方位群所構成者。
前述{112}＜111＞方位，即是為Copper方位之方位，前述{110}＜112＞方位即是被稱為Brass方位之方位，前述{110}＜001＞方位即是被稱Goss方位之方位。此等3個方位已知是能量優位之方位，在沃斯田鐵系不鏽鋼之再結晶集合組織中、優先的容易集積(易配向)之方位。
輥軋後之不鏽鋼箔中，自此3個方位計算方位差在10°以内之配向結晶粒的比例是少的，組織中結晶粒之方位儘管會變得比較地隨機，如前所述者，因差排密度高，故成形性差。在此，藉由退火處理進行組織之回復與再結晶，而使得差排密度低。此時，經過再結晶，結晶粒是朝向粗大化(晶粒成長)，集積在能量優位方位上之述3個方位的結晶粒比例就增加。
進行在此等特定方位上的結晶粒配向，結晶粒就會朝特定方位偏向排列。此時，若不鏽鋼箔受到鼓膨成形等壓制加工，雖變形上有利方位(容易生成滑動之方位)上亦顯示出良好的成形性，變形上不利方位(難以生成滑動之方位)上的成形性悪化。若如此，在如電池殼的角隅部上，若在輥軋面受到在任意方向被拉伸之鼓膨成形時，顯示出充分的延伸(變形)方位，另一方面，其亦會有以變形上不利方位作為起點發生有斷裂(塑性變形能惡化)，而無法得到所欲的成形深度。即，對於鼓膨成形之變形發生有異向性。
在此，於本發明中，為了減低結晶粒的配向度而造成之成形性異方性，進行退火處理並使其再結晶之後，可使結晶粒方位為隨機的。在沃斯田鐵系不鏽鋼中，如上述所欲者，由於容易集積在{112}＜111＞方位、{110}＜112＞方位、{110}＜001＞方位之3個方位上，可判斷為在各方位上集積之結晶粒(由各方位計算方位差在10°以内之配向結晶粒)所占之面積合計的比例是設在20%以下。藉此，消解在沃斯田鐵系不鏽鋼箔之集合組織中結晶粒方位的偏向，減低成形性異方性，在輥軋面内縱或受到被任意之方向拉伸加工時，亦可以得到充分的成形深度。再者，自前述3個方位起算方位差10°以内之集積領域的方位是比前述3個方位更難以集積之結晶方位，不會在特定方位上集積。亦即，有關自前述3個方位起算方位差超過10°的任意結晶方位X，自X起算之方位差在10°以内之結晶方位的面積率是在20%以下。
本發明中，在測定視野内，自{112}＜111＞方位起算在方位差在10°以内的結晶方位、自{110}＜112＞方位起算方位差在10°以内結晶方位，以及自{110}＜001＞方位起算方位差在10°以内結晶方位所占的面積率合計是以在１5%以下為宜，7%以下為佳。
自上述各方位起算方位差在10°以内之結晶方位所占的面積率在本發明中是使用電子線背散射繞射(EBSD：Electron Back Scatter Diffraction)法藉由決定各測定點之結晶方位來算出。該EBSD法是將EBSD檢出器連接到SEM(掃描式電子顯微鏡)，使試料傾斜70°左右，分析對傾斜之試料表面之預定測定視野照射了收歛式電子光束時所發生之繞射圖案(EBSD圖案)，測定結晶方位的方法。
具體而言，在各測定點中自繞射圖案推定出位幾個方位，並決定以確度最高方位作為測定點中的結晶方位。如此進行所獲得之各測定點之方位因應在反極點圖上之位置而以色分圖示顯示，因而得到IPF(反極點圖，Inverse Pole Figure)地圖。由此IPF地圖，與上述各方位之角度差是在許容角度(Tolerance Angle)(本發明中為10°)以下之結晶粒是在測定視野面積中占有的比例作為面積率加以算出。又，本發明中，測定視野是以100×100μm左右以上之領域為宜。
[在板厚方向之結晶粒為3個以上] 本發明之沃斯田鐵系不鏽鋼箔，在板厚方向上結晶粒係存在3個以上為較佳。板厚度方向的結晶數，能夠在板厚方向上的任何斷面上依據JIS G 0551而測定結晶粒徑且算出平均結晶粒徑，而且以平均結晶粒徑除以板厚，基於其商而設作板厚方向的結晶粒數。又，結晶粒為等軸晶粒時，亦可在與板厚方向正交的面測定結晶粒且算出平均結晶粒徑。
或是在任意的剖面內之板厚方向，描繪任意直線3根以上且計算該等直線橫切之結晶粒的個數，將該等進行算術平均而求取。此時，結晶粒與表面接觸時，係設作0.5個而統計。又，直線係沿著結晶晶界時，亦能夠統計構成結晶晶界之複數個結晶。但是，不鏽鋼箔的寬度方向之兩端部，因為容易受到退火的影響，所以不適合測定結晶粒數。因此，以將不鏽鋼箔的寬度方向之兩端部除外，在板厚方向描繪任意直線且測定結晶粒數為佳。例如，能夠藉由在不鏽鋼箔的寬度方向之中央(從一端起算1/2寬度之位置)及兩端與中央之中間(從一端起算1/4寬度及3/4寬度之2個位置)的3處計算結晶粒的個數，且將該等進行算術平均，來進行該不鏽鋼箔的板厚方向之結晶粒數。
若如此作求的結晶粒數是在3個以上，由於提高塑性變形能力，鼓膨成形性亦良好，而為較佳的。亦即，為了各自的結晶粒係塑性變形成為任意的形狀，必須滿足米塞斯(von Mises)的條件且複數個滑動系統必須產生多層滑動。但是，板厚方向的結晶粒數較少時，對變形方向為不滿足米塞斯(von Mises)條件的方位之結晶粒(變形能力差之結晶粒)在厚度方向排列之概率係變高。那樣時，因為壓製加工時該等結晶粒係無法追隨箔整體的變形，所以成為斷裂的起點。另一方面，若是板厚度方向上結晶粒存在有3個以上時，因為即便存在變形能力差之結晶粒，周圍的結晶粒變形成為任意的形狀而能夠維持箔整體的變形，其結果，塑性變形能力提升。
再者，若按照板厚而決定板厚方向的結晶粒數時，能夠進一步確保塑性變形能力。板厚愈厚則變形抗性就愈大，因此，板厚愈厚，可使則結晶粒數要多。具體而言，板厚為15μm以上時，板厚方向的結晶粒數係以5個以上為佳，特別是板厚為40μm以上時，板厚方向的結晶粒數係以10個以上為更佳。藉此，能夠使塑性變形能力進一步提升。又，板厚小於15μm之沃斯田鐵系不鏽鋼箔時，板厚對板厚方向的結晶粒數之影響係成為能夠忽視之程度。
結晶粒數的上限係沒有特別限定。因為依照沃斯田鐵系不鏽鋼箔的板厚，板厚方向的結晶粒數係產生變化。只要結晶粒數為3個以上，結晶粒的大小(依據JIS G 0051之結晶粒徑(以下，在本說明書係只要未特別告知，就稱為「結晶粒徑」))沒有特別限定。因為上述的多層滑動，不是決取於結晶粒的大小，而是取決於厚度方向的結晶粒之數目。
[表層的氮濃度] 如上所示，氮化不鏽鋼箔之表面時，若特別使板厚變薄，則會顯現出因氮化而有表層硬化所造成的種種問題點。因而，不鏽鋼箔的表層係以不氮化為佳。「表層不氮化」係指表層之氮原子濃度在1.0質量%以下。在此，所謂表層，係在藉由歐傑電子能譜術之測定，氧濃度為尖峰値的一半之厚度，氮濃度為在表層之平均的濃度。
再次重複說明，不鏽鋼箔的表層氮化時，因為經壓製加工時，表層係因氮化變硬且成為斷裂的起點，所以壓製成形性低下。板厚為60μm以下的較薄本發明不鏽鋼箔中，表面的影響係相對地變大，故此問題變得顯著。藉由將氮濃度設為上述的範圍，因為能夠變形且不產生表層斷裂(龜裂)，就能夠得到良好的壓製成形性。因此，不要使得不鏽鋼箔表層氮原子濃化，如上所示，表層之氮為濃度以1.0質量%以下為佳。表層的氮濃度之下限係沒有必要特別限定。下限係與在不鏽鋼箔整體進行評價之氮含量同等。亦即，通常的SUS304等不含有氮的鋼種時，作為不可避免的不純物之氮含量水準係成為下限。
不鏽鋼箔的表層之氮濃度，係能夠藉由將退火環境中的氮濃度控制在0.1體積%以下，而可控制在1質量%以下。
[層疊] 本發明之沃斯田鐵系不鏽鋼箔，係與通常的層疊不鏽鋼箔同樣地，亦可在其表面層積(層疊)樹脂薄膜而成為層疊沃斯田鐵系不鏽鋼箔。藉由層積樹脂薄膜，能夠使在電解液中的耐蝕性提升且能夠進一步提高在以鋰離子電池為首之電池殼體的適用性。
樹脂薄膜層積係可在不鏽鋼箔的兩表面施行，亦可在任一表面施行。
針對不鏽鋼箔與樹脂的剝離強度，係藉由在不鏽鋼箔的表面設置適當厚度的鉻酸鹽處理層而能夠得到必要的性能。例如，在專利文獻5係揭示在不鏽鋼箔的至少一面設置厚度2~200nm的鉻酸鹽處理層，且在其表面層積含有具有極性的官能基之聚烯烴系樹脂之技術。
又，針對壓製加工後的樹脂之白化，係藉由將樹脂的設計最佳化而能夠防止。具體而言，係使熱層疊後的樹脂成為非晶質即可，因此，將熱層疊時的冷卻速度加速即可。例如將在120℃~80℃的範圍的冷卻速度設為20℃/s以上即可。
(2.沃斯田鐵系不鏽鋼箔之製造方法) 其次，說明本發明之沃斯田鐵系不鏽鋼箔的製造方法。
本發明之沃斯田鐵系不鏽鋼箔的製造步驟係與通常的不鏽鋼箔之製造步驟大致相同。亦即，將不鏽鋼帶進行箔輥軋，隨後表面洗淨，最後進行退火且按照必要進行調質輥軋(拉力整平器(tension leveler))而成為沃斯田鐵系不鏽鋼箔。又，按照提供箔輥軋之素材的不鏽鋼帶之板厚而將箔輥軋步驟分次複數次(多段輥軋)，亦可在各箔輥軋步驟之間進行中間退火。但是，為了得到本發明之沃斯田鐵系不鏽鋼箔，係如前述，在最後箔輥軋的軋縮率及在最後退火溫度控制係重要的。
[軋縮率] 在箔輥軋，藉由進行強軋縮輥軋，係能夠在不鏽鋼中導入成為再結晶的核生成位置之位錯。軋縮率越高，被導入的差排就越增加。差排密度是利用軋縮率與輥軋後施予退火處理一起控制的。因而，進行2次以上的箔輥軋時，係在最後的箔輥軋，亦即最後退火之前之箔輥軋以強軋縮進行即可。
具體而言，將最後退火前的箔輥軋之軋縮率設為30%以上即可。從確保差排密度的觀點而言，較佳是設為40%以上，更佳是設為45%以上即可。
又，軋縮率係使用以下的式定義。 軋縮率=(輥軋前板厚-輥軋後板厚)/(輥軋前板厚)
在箔輥軋，減少板厚係自不待言，亦是為了導入差排之目的，故而未特別限定軋縮率的上限。但是，因為理論上係無法得到軋縮率100%，所以實際上的軋縮率之上限係95%左右。
軋縮率之下限亦是依沃斯田鐵系不鏽鋼箔之最終板厚而不同，以盡可能設為40%以上為佳，以45%以上為較佳。
分成複數次而進行箔輥軋時，在中間進行的箔輥軋及其後緊接著進行的中間退火亦可控制材料的構造。此時，與最後箔輥軋相同進行同様地進行即可。亦即，將在各箔輥軋的軋縮率設為30%以上即可。但是如上述，因為最後退火之前的箔輥軋係重要的，所以相較於其他箔輥軋軋縮率，將最後箔輥軋的軋縮率設定為較高為佳。
[退火溫度] 箔輥軋後的退火(最後退火)，係擔當用以減少差排密度且進行再結晶之重要的分派任務。有關本發明之沃斯田鐵系不鏽鋼箔，係如前述，是以使差排密度減少、維續進行再結晶，抑制晶粒成長，而抑制特定方位的集積為其目的。
若是本發明之沃斯田鐵系不鏽鋼，將退火溫度設為950℃以上且1050℃以下。950℃以下由於差排密度不減少，再結晶率就會變低。另一方面，若超過1050℃，結晶則粗大化，同時會進行朝在上述三個的任一個方位上的配向，因而無法得到良好成形性。因為退火溫度的下限係比950℃更高若干為佳者，所以較佳是設為960℃，更佳是設為970℃為佳。
從抑制結晶方位的集積的觀點而言，退火溫度的上限亦是設為比1050℃更低若干，以設為1040℃為佳，更佳是設1030℃為佳。
[退火保持時間] 將不鏽鋼箔保持在上述的退火溫度之保持時間設為3秒以上且30秒以下。少於3秒時，熱處理係變為不充分且再結晶未充分地進展，而無法得到再結晶率。另一方面，若超過30秒，結晶則粗大化，同時會進行朝上述三個方向中任一個方位配向，因而無法得到良好成形性。
[退火環境] 退火環境係設為氫或氬等的稀有氣體環境，而使不鏽鋼箔的表面不會氮化。又，雖然在退火環境中係以完全不含有氮為佳，但是從大氣中以不可避免的方式混入之氮仍能夠容許某種程度。為了使得表層的氮濃度為1.0質量%以下，退火環境中之氮濃度若在0.1體積%以下即可。
[中間退火] 設作複數次的箔輥軋步驟時，針對中間退火的條件下係沒有特別規定，但以950℃以上1050℃以下為佳。因為結晶晶界亦成為再結晶的核心，故宜在箔輥軋前大量導入，所以較佳是藉由設為上述的溫度範圍來抑制再結晶粒的粗大化。
實施例 作為本發明之沃斯田鐵系不鏽鋼箔的實施例，具有市售的SUS304使用箔輥軋機且基於表1記載的輥軋條件進行輥軋，來製造具有在表1所記載的厚度之沃斯田鐵系不鏽鋼箔。
在此，軋縮率係表示在即將最後退火之前的箔輥軋步驟之軋縮率；精加工退火溫度係表示在輥軋步驟完成後所施行的最後退火步驟之溫度；保持時間係表示在精加工退火溫度保持不鏽鋼箔之時間。
退火環境係0.1體積%氮－99.9體積%氫混合氣體。
再結晶率係以輥軋方向剖面作為觀察面且進行鏡面研磨、蝕刻而進行觀察，求取整個板厚×在500μm寬度的範圍已再結晶之結晶粒的面積且計算(已再結晶之結晶的面積)/(觀察面積)而得到。
精加工退火後之不鏽鋼箔集合組織是將該箔之表面利用科學上的蝕刻法或者CP(斷面拋光，Cross-section Polishing)法研磨而得者利用EBSD法測定。測定100Μm角之測定視野中、與copper 方位{112}＜111＞、brass方位{110}＜112＞、Goss方位{110}＜001＞之方位差在10°以内之結晶方位的集積度(面積%)。
表層的氮濃度係藉由傑電子能譜術(Auger electron spectroscopy；AES)來測定。測定從不鏽鋼箔表面起算至30nm的深度為止，且將至氧濃度成為尖峰値一半的濃度之深度為止的平均氮濃度設作表層的氮濃度。
板厚方向的結晶粒數係在板厚方向將試片切取且進行剖面研磨後，施行蝕刻之後，使用顯微鏡觀察之後，依據JIS G 0551而測定結晶粒徑且算出平均結晶粒徑，並且設為將板厚除以平均結晶粒徑所得到的商。
又，使用精加工退火(最後退火)後的不鏽鋼箔，在其一面設置10nm的鉻酸鹽處理層之後，在其上層疊聚丙烯薄膜，在另一面係層疊聚酯薄膜或耐綸薄膜，來製造約100mm四方的試樣。在該等試樣之中央，使用縱40mm×橫30mm的衝頭且在間隙0.3mm的條件下進行壓製成形，來評價不產生皺紋和龜裂之最大的深度。由於板厚愈大最大成形深度就愈大，板厚未達30μm時，成形深度在4.0mm以上為佳，板厚30μm以上，成形深度在4.5mm以上為佳。將評價結果顯示在表1。
[表1]
Figure TWI609973BD00001
如表1所示者，本發明之沃斯田鐵系不鏽鋼箔之實施例是在各方位集積結晶粒面積比例低，其結果為、板厚未達30μm時，成形深度為4.0mm以上，板厚30μm以上，成形深度為4.5mm以上。
板厚未達30μm之比較例1則由於精加工退火温度低，無法充分進行再結晶化，而使得再結晶率低。其結果是成形深度是比4.0mm小。
另一方面，板厚未達30μm之比較例2與比較例3則由於精加工退火温度高，會充分進行再結晶，且進一步晶粒成長，同時再結晶得到之結晶粒集積在各方位。此結果是對鼓膨成形形成有變形之異向性，成形深度則變得比4.0mm還小。
板厚是小於30μm之比較例4與6則由於精加工退火温度低，無法充分進行再結晶化，而使得再結晶率低。其結果是成形深度會變得比4.5mm還小。
又，板厚是30μm以上之比較例5則由於精加工退火温度高，會充分進行再結晶，且進一步晶粒成長，同時再結晶得到之結晶粒集積在各個方位。此結果是對鼓膨成形之形成有變形異向性，成形深度會變得比4.5mm還小。
藉由以上的結果，比較板厚相同之實施例4與比較例2，可確認出成形深度有0.3mm以上之差。此一差異如下所示，是非常顯著的差異。即，不鏽鋼箔適用到，例如，手機等小型且輕量之電子機器中搭載的電池殼時，電池殼的厚度被要求是數mm程度。就此種狀況，成形深度若變大0.3mm以上，就相當於電池殼之厚度的10%以上，大大有助於電池容量的增加。因此，本發明之效果非常大。
產業上之可利用性 本發明之沃斯田鐵系不鏽鋼箔能夠應用在小型電子機器用的鋰離子電池等的電池殼體等。
無

Claims (5)

  1. 一種沃斯田鐵系不鏽鋼箔，其特徵在於：其板厚在5μm以上且60μm以下，並且前述不鏽鋼箔的再結晶率為90%以上且100%以下，前述不鏽鋼箔在測定視野內具有下述面積率合計在20%以下的集合組織：自{112}<111>方位起算方位差在10°以內的結晶方位之面積率、自{110}<112>方位起算方位差在10°以內結晶方位之面積率，以及自{110}<001>方位起算方位差在10°以內結晶方位之面積率。
  2. 如請求項1之沃斯田鐵系不鏽鋼箔，其中前述板厚為5μm以上且25μm以下。
  3. 如請求項1或2之沃斯田鐵系不鏽鋼箔，其中在板厚方向具有結晶粒3個以上。
  4. 如請求項1或2之沃斯田鐵系不鏽鋼箔，其中表層的氮濃度在1.0質量%以下。
  5. 如請求項1或2之沃斯田鐵系不鏽鋼箔，其中前述沃斯田鐵系不鏽鋼箔的至少一表面層積有樹脂薄膜。
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