CN106537643B - 隔膜卷及非水系二次电池 - Google Patents
隔膜卷及非水系二次电池 Download PDFInfo
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- CN106537643B CN106537643B CN201580037576.8A CN201580037576A CN106537643B CN 106537643 B CN106537643 B CN 106537643B CN 201580037576 A CN201580037576 A CN 201580037576A CN 106537643 B CN106537643 B CN 106537643B
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Abstract
本发明涉及一种隔膜卷,所述隔膜卷是将隔膜卷绕于卷芯而得到的,所述隔膜具有多孔基材和多孔层,所述多孔层是将下述涂布层固化而形成的,所述涂布层是将含有树脂和无机粒子中的至少任一者的涂布液涂布于所述多孔基材的一面或两面而形成的,利用下述方法求出的所述隔膜的机械方向的收缩率为1.0%以下。所述方法为:自隔膜卷的外端起去除5倍周长量的隔膜,然后,自其端部起在机械方向上切取200mm的隔膜作为试样。将该试样在25℃下、在无张力状态下放置24小时,测定放置前后的机械方向的长度,算出机械方向的收缩率。
Description
技术领域
本发明涉及隔膜卷(separator roll)及非水系二次电池。
背景技术
关于非水电解质电池用隔膜,在聚烯烃微多孔膜等多孔基材的表面上设置功能层从而赋予耐热性、与电极的粘接性等功能的技术是已知的(例如,专利文献1及2)。作为上述功能层的制作方法,已知有下述涂布法:将涂布液涂布于多孔基材而形成涂布层,通过干燥而除去涂布层中的溶剂,从而制作功能层的方法;将涂布液涂布于多孔基材而形成涂布层,浸渍于凝固液中而使涂布层中的树脂固化,经水洗和干燥而制作功能层的方法;等等(例如,专利文献1及2)。而且,隔膜通常是以卷绕于卷芯而成的卷的形式制造的(例如,专利文献3及4)。
但是,在制造方型电池、聚合物电池这样的扁平型的电池时,用卷绕装置将隔膜与电极一同卷绕而制作电池元件时,有时发生电池元件的卷绕错位,或者引起电池元件的变形(例如膨胀)而发生电池的外观不良。作为与电池元件的卷绕错位、变形有关的因素,包括卷绕装置的规格、电极的种类等多种因素,对于隔膜的相关性,迄今为止并未充分研究。
现有技术文献
专利文献
专利文献1:日本特开2003-171495号公报
专利文献2:日本专利第5431581号公报
专利文献3:日本特开2013-216868号公报
专利文献4:日本特开2014-12391号公报
发明内容
发明所要解决的课题
本发明的实施方式是基于上述情况而完成的。
本发明的实施方式的目的在于提供用于供给不易引起电池元件的卷绕错位及变形的非水电解质电池用隔膜的隔膜卷、以及制造成品率高的非水系二次电池。
用于解决课题的手段
用于解决上述课题的具体的手段包括以下的方式。
[1]隔膜卷,所述隔膜卷是将非水电解质电池用隔膜卷绕于卷芯而得到的,所述非水电解质电池用隔膜具有:
多孔基材;和
多孔层,所述多孔层是将下述涂布层固化而形成的,所述涂布层是将含有树脂和无机粒子中的至少任一者的涂布液涂布于上述多孔基材的一面或两面而形成的,
利用下述的方法(1)求出的上述非水电解质电池用隔膜的机械方向的收缩率为1.0%以下。
方法(1):自隔膜卷的外端起去除5倍周长量的非水电解质电池用隔膜,然后,自其端部起在机械方向上切取200mm的非水电解质电池用隔膜作为试样。将该试样在25℃下、在无张力状态下放置24小时,测定该放置前后的机械方向的长度,利用下式算出机械方向的收缩率。
机械方向的收缩率(%)=(放置前的机械方向的长度-放置后的机械方向的长度)÷放置前的机械方向的长度×100
[2][1]所述的隔膜卷,其中,上述多孔基材含有熔点低于200℃的热塑性树脂。
[3][1]或[2]所述的隔膜卷,其中,上述隔膜卷是一次卷或二次卷,所述一次卷是在制造上述非水电解质电池用隔膜后将所述非水电解质电池用隔膜直接卷绕于卷芯而成的,所述二次卷是从上述一次卷将上述非水电解质电池用隔膜卷绕于卷芯而成的,上述一次卷是以下述卷绕速度将上述非水电解质电池用隔膜卷绕于卷芯而成的隔膜卷,所述卷绕速度相对于上述多孔基材的送出速度的速度比为100%以上103%以下。
[4][1]~[3]中任一项所述的隔膜卷,其中,上述隔膜卷是一次卷或二次卷,所述一次卷是在制造上述非水电解质电池用隔膜后将所述非水电解质电池用隔膜直接卷绕于卷芯而成的,所述二次卷是从上述一次卷将上述非水电解质电池用隔膜卷绕于卷芯而成的,上述一次卷是被实施了下述操作的隔膜卷,所述操作为:在40℃以上110℃以下的气氛中放置12小时以上。
[5][1]~[4]中任一项所述的隔膜卷,其中,利用下述的方法(2)求出的上述非水电解质电池用隔膜的宽度方向的扩大率为0%以上0.6%以下。
方法(2):自隔膜卷的外端起去除5倍周长量的非水电解质电池用隔膜,然后,自其端部起在机械方向上切取200mm的非水电解质电池用隔膜作为试样。将该试样在25℃下、在无张力状态下放置24小时,测定该放置前后的宽度方向的长度,利用下式算出宽度方向的扩大率。
宽度方向的扩大率(%)=(放置后的宽度方向的长度-放置前的宽度方向的长度)÷放置前的宽度方向的长度×100
[6][1]~[5]中任一项所述的隔膜卷,其中,利用下述的方法(3)求出的上述非水电解质电池用隔膜的机械方向的热收缩率为3%以上40%以下。
方法(3):从隔膜卷切出非水电解质电池用隔膜,得到机械方向的长度为190mm的试样。针对该试样进行在135℃下、在无张力状态下放置30分钟的热处理,测定该热处理前后的机械方向的长度,利用下式算出机械方向的热收缩率。
机械方向的热收缩率(%)=(热处理前的机械方向的长度-热处理后的机械方向的长度)÷热处理前的机械方向的长度×100
[7][1]~[6]中任一项所述的隔膜卷,其中,利用上述方法(1)求出的上述非水电解质电池用隔膜的机械方向的收缩率为0.5%以下。
[8][1]~[7]中任一项所述的隔膜卷,其中,上述涂布液含有粘接性树脂。
[9]非水系二次电池,其具有:
正极;
负极;和
非水电解质电池用隔膜,所述非水电解质电池用隔膜被配置于上述正极和上述负极之间,是从[1]~[8]中任一项所述的隔膜卷供给的,
所述非水系二次电池通过锂的掺杂·脱掺杂而获得电动势。
发明的效果
通过本发明的实施方式,可提供用于供给不易引起电池元件的卷绕错位及变形的非水电解质电池用隔膜的隔膜卷、以及制造成品率高的非水系二次电池。
附图说明
[图1]为用于说明实施例中进行的测定方法的概略图。
具体实施方式
以下,对本发明的实施方式进行说明。需要说明的是,这些说明及实施例是为了对本发明进行示例,不限制本发明的范围。
本说明书中,使用“~”表示的数值范围表示,将“~”的前后所记载的数值分别作为最小值及最大值包含在内的范围。
本说明书中,“机械方向”是指长条状的多孔基材及隔膜中的长尺寸方向,“宽度方向”是指与“机械方向”正交的方向。本说明书中,将“机械方向”亦称为“MD方向”,将“宽度方向”亦称为“TD方向”。
本说明书中,术语“工序”并不仅仅是独立的工序,即使在不能与其他工序明确区别的情况下,如果能实现该工序所期待的作用,则也包含在本术语中。
<隔膜卷>
本公开文本的隔膜卷是将沿机械方向连续地制造的非水电解质电池用隔膜(以下,也简称为“隔膜”。)卷绕于卷芯而成的隔膜卷。本公开文本的隔膜卷中,隔膜是具有多孔基材、和被设置于该多孔基材的一面或两面的多孔层的隔膜,上述多孔层是将下述涂布层固化而形成的多孔层,所述涂布层是涂布含有树脂和无机粒子中的至少任一者的涂布液而形成的。
对于本公开文本的隔膜卷而言,利用下述的方法(1)求出的隔膜的MD方向的收缩率为1.0%以下。
方法(1):自隔膜卷的外端起去除5倍周长量的隔膜,然后,自其端部起在机械方向上切取200mm的隔膜作为试样。将该试样在25℃下、在无张力状态下放置24小时,测定该放置前后的MD方向的长度,利用下式算出MD方向的收缩率。
MD方向的收缩率(%)=(放置前的MD方向的长度-放置后的MD方向的长度)÷放置前的MD方向的长度×100
本公开文本中,将利用方法(1)测得的隔膜的MD方向的收缩率称为“25℃下MD方向收缩率”。
从本公开文本的隔膜卷供给的隔膜在制造电池元件时不易引起电池元件的卷绕错位。另外,从本公开文本的隔膜卷供给的隔膜不易引起电池元件的变形。
经本申请的发明人研究发现,具有利用涂布法而被设置在多孔基材上的多孔层的隔膜于室温下在MD方向上收缩是与电池元件的卷绕错位、变形的发生有关的。在利用涂布法在多孔基材上设置多孔层时,为了将涂布液均匀地涂布于多孔基材的表面,需要向多孔基材施加张力。而且,为了在不产生褶皱的情况下输送多孔基材,需要对多孔基材施加一定程度上较强的张力。由于在将涂布液涂布于多孔基材上时向多孔基材施加强张力,结果将导致多孔基材在MD方向上被拉长,制作的隔膜具有即使不暴露于高温也会在MD方向上收缩的性质。
本公开文本的隔膜卷中,隔膜的25℃下MD方向收缩率为1.0%以下,因此,在利用从本公开文本的隔膜卷供给的隔膜制作电池元件时,可抑制电池元件的卷绕错位及变形的发生。对于本公开文本的隔膜卷而言,从上述的观点考虑,隔膜的25℃下MD方向收缩率更优选为0.5%以下,越低越优选。另一方面,从隔膜具有一定程度的柔软性时可良好地制造电池元件这样的观点考虑,作为25℃下MD方向收缩率的下限值,优选为0.1%以上,更优选为0.15%以上。
以往,将多孔基材固定并加热而除去多孔基材的残留应力的技术、通过增加多孔层的无机填料的含量来抑制高温下(例如150℃左右)的隔膜收缩的技术是已知的,但均不是抑制在室温下发生的隔膜收缩的技术。迄今为止,并未获知抑制在室温下发生的隔膜收缩的技术。经本申请的发明人研究发现,隔膜的25℃下MD方向收缩率可通过隔膜的制造工序中的改进来控制。
具有利用涂布法而被设置在多孔基材上的多孔层的隔膜还具有在室温下伴随着在MD方向上的收缩而在TD方向上伸长的性质。隔膜的TD方向的伸长从抑制电池短路的观点考虑是优选的。但是,TD方向的伸长与MD方向的收缩存在权衡(trade-off)关系,因此,优选隔膜在室温下在TD方向上不过度伸长。因此,对于本公开文本的隔膜卷而言,利用下述的方法(2)求出的隔膜的TD方向的扩大率优选为0%以上0.6%以下,更优选大于0%且为0.6%以下。
方法(2):自隔膜卷的外端起去除5倍周长量的隔膜,然后,自其端部起在机械方向上切取200mm的隔膜作为试样。将该试样在25℃下、在无张力状态下放置24小时,测定该放置前后的TD方向的长度,利用下式算出TD方向的扩大率。
TD方向的扩大率(%)=(放置后的TD方向的长度-放置前的TD方向的长度)÷放置前的TD方向的长度×100
本公开文本中,将利用方法(2)测得的隔膜的TD方向的扩大率称为“25℃下TD方向扩大率”。
本公开文本中,详细而言,25℃下MD方向收缩率(%)利用下述方法求出。也可同时求出25℃下TD方向扩大率(%),因而一并进行说明。
自隔膜卷的外端起去除5倍周长量的隔膜后,自其端部起在MD方向上切取200mm的隔膜,将切出的长度为200mm的隔膜作为试样。用夹具把持试样的一端,在温度为25℃、相对湿度为50±10%的恒温槽中,以MD方向成为重力方向的方式悬吊试样,在无张力状态下放置24小时。在进行24小时放置之前和之后,针对MD方向及TD方向,测定试样的长度,利用上述2个式子算出MD方向的收缩率(%)和TD方向的扩大率(%)。在测定时,使得从开始自隔膜卷的外端取出隔膜起、直至将试样悬吊于恒温槽为止(即,直至开始进行24小时放置为止)的时间为10分钟以内,从恒温槽中取出试样后,立即进行24小时放置后的长度测定。在从隔膜卷制备试样时,注意不向隔膜施加张力。详细的测定方法如实施例中所记载。
此外,卷绕在本公开文本的隔膜卷中的隔膜的利用下述的方法(3)求出的MD方向的热收缩率优选为3%~40%。
方法(3):从隔膜卷切出隔膜,得到MD方向的长度为190mm的试样。用夹具把持试样的一端,在将库内温度保持为135℃的烘箱中,以MD方向成为重力方向的方式悬吊试样,进行在无张力状态下放置30分钟的热处理。在该热处理之前和之后,针对MD方向,测定试样的长度,利用下式算出MD方向的热收缩率(%)。方法(3)的详细内容如实施例中所记载。
MD方向的热收缩率(%)=(热处理前的MD方向的长度-热处理后的MD方向的长度)÷热处理前的MD方向的长度×100
本公开文本中,将利用方法(3)测得的隔膜的MD方向的热收缩率称为“135℃下MD方向热收缩率”。
135℃下MD方向热收缩率为3%以上反映出多孔基材具有伸缩性。多孔基材具有伸缩性时,在制造隔膜的各工序(尤其是,一边向多孔基材施加张力一边涂布涂布液的工序、及赋予热而将溶剂或水除去的干燥工序)中,多孔基材及复合膜(在多孔基材的一面或两面上具有多孔层的片材)柔软地伸缩,因此,不易在隔膜的卷中产生褶皱、筋条,结果,不易引起电池元件及电池的外观不良。另一方面,从与电池的安全性有关的隔膜的热尺寸稳定性的观点考虑,135℃下MD方向热收缩率优选为40%以下。
从上述的观点考虑,135℃下MD方向热收缩率的下限优选为3%以上,更优选为5%以上,进一步优选为10%以上,135℃下MD方向热收缩率的上限优选为40%以下,更优选为30%以下,进一步优选为25%以下。
以下,对卷绕在本公开文本的隔膜卷中的隔膜所具有的多孔基材及多孔层进行详细说明。
[多孔基材]
本公开文本中,多孔基材是指在内部具有孔隙或空隙的基材。作为这样的基材,可举出微多孔膜;由纤维状物形成的无纺布、纸等多孔性片材;在微多孔膜或多孔性片材上层叠1层以上多孔性的层而成的复合多孔片材;等等。作为多孔基材,从隔膜的薄膜化及强度的观点考虑,优选为微多孔膜。微多孔膜是指下述膜,所述膜形成为在内部具有大量的微细孔、并且这些微细孔被连结的结构,气体或液体可从一侧的面向另一侧的面通过。
多孔基材包含具有电绝缘性的有机材料及/或无机材料。
从向多孔基材赋予关闭功能的观点考虑,多孔基材优选包含热塑性树脂。关闭功能是指下述功能:在电池温度升高时,材料熔化,将多孔基材的孔闭塞,由此阻断离子的移动,防止电池的热失控。
多孔基材中包含的热塑性树脂的一例是熔点低于200℃的热塑性树脂。包含熔点低于200℃的热塑性树脂的多孔基材与不含该树脂的多孔基材相比,容易在张力作用下在MD方向上被拉伸。因此,以往,使用包含熔点低于200℃的热塑性树脂的多孔基材制作的隔膜在室温下容易在MD方向上收缩。通过本公开文本的技术,即使在使用包含熔点低于200℃的热塑性树脂的多孔基材的情况下,也可提供不易引起电池元件的卷绕错位及变形的隔膜及隔膜卷。
本公开文本中,作为多孔基材中包含的熔点低于200℃的热塑性树脂,优选为聚烯烃。
作为多孔基材,优选为包含聚烯烃的微多孔膜(称为“聚烯烃微多孔膜”。)。作为聚烯烃微多孔膜,可举出应用于以往的电池隔膜的聚烯烃微多孔膜,优选从其中选择具有充分的力学特性和离子透过性的聚烯烃微多孔膜。
从呈现关闭功能的观点考虑,聚烯烃微多孔膜优选包含聚乙烯,作为聚乙烯的含量,优选为95质量%以上。
从赋予在暴露于高温时不会容易地破膜的程度的耐热性这样的观点考虑,聚烯烃微多孔膜优选为包含聚乙烯和聚丙烯的聚烯烃微多孔膜。作为这样的聚烯烃微多孔膜,可举出聚乙烯和聚丙烯在1个层中混合存在的微多孔膜。该微多孔膜中,从同时实现关闭功能和耐热性这样的观点考虑,优选包含95质量%以上的聚乙烯和5质量%以下的聚丙烯。另外,从同时实现关闭功能和耐热性的观点考虑,下述聚烯烃微多孔膜也是优选的,所述聚烯烃微多孔膜具有2层以上的层叠结构,且至少1层包含聚乙烯,至少1层包含聚丙烯。
作为聚烯烃微多孔膜中包含的聚烯烃,优选重均分子量为10万~500万的聚烯烃。重均分子量为10万以上时,可确保充分的力学特性。另一方面,重均分子量为500万以下时,关闭特性良好,容易进行膜的成型。
聚烯烃微多孔膜例如可利用以下的方法制造。即,将熔融后的聚烯烃树脂从T-模挤出而制成片材,对其进行结晶化处理后,进行拉伸,然后,进行热处理而制成微多孔膜的方法。或者,将与液体石蜡等增塑剂一同熔融后的聚烯烃树脂从T-模挤出,将其冷却而制成片材,进行拉伸后,提取增塑剂,进行热处理而制成微多孔膜的方法。
作为由纤维状物形成的多孔性片材,可举出由各种树脂(例如,聚对苯二甲酸乙二醇酯等聚酯;聚乙烯、聚丙烯等聚烯烃;芳香族聚酰胺、聚酰亚胺、聚醚砜、聚砜、聚醚酮、聚醚酰亚胺等耐热性树脂)的纤维状物形成的无纺布、纸等。耐热性树脂是指,熔点为200℃以上的树脂、或不具有熔点且分解温度为200℃以上的树脂。
作为复合多孔片材,可举出在微多孔膜或由纤维状物形成的多孔性片材上层叠功能层而成的片材。这样的复合多孔片材可通过功能层而进一步附加功能,从这方面考虑是优选的。作为功能层,例如从赋予耐热性这样的观点考虑,优选包含耐热性树脂的多孔性的层、包含耐热性树脂及无机填料的多孔性的层。作为耐热性树脂,可举出选自芳香族聚酰胺、聚酰亚胺、聚醚砜、聚砜、聚醚酮及聚醚酰亚胺中的1种或2种以上的树脂。作为无机填料,可举出氧化铝等金属氧化物、氢氧化镁等金属氢氧化物等。作为复合多孔片材的制造方法,可举出在微多孔膜或多孔性片材上涂布功能层的方法、用粘接剂将微多孔膜或多孔性片材与功能层接合的方法、将微多孔膜或多孔性片材与功能层热压接的方法等。
从得到良好的力学特性和内电阻的观点考虑,多孔基材的厚度优选为5μm~30μm。
从防止电池短路和得到离子透过性的观点考虑,多孔基材的Gurley值(JIS P8117(2009))优选为50秒/100cc~800秒/100cc。
从得到适当的薄膜电阻、关闭功能的观点考虑,多孔基材的孔隙率优选为20%~60%。
从提高制造成品率的观点考虑,多孔基材的戳穿强度优选为300g以上。
[多孔层]
本公开文本中,多孔层是下述层,所述层形成为在内部具有大量的微细孔、并且这些微细孔被连结的结构,气体或液体可从一侧的面向另一侧的面通过。本公开文本中,多孔层被设置于多孔基材的一面或两面上作为隔膜的最外层。
多孔层优选为可与电极粘接的粘接性多孔层。从电池的循环特性优异的观点考虑,与仅在多孔基材的一面上存在粘接性多孔层的情况相比,更优选在多孔基材的两面上存在粘接性多孔层。这是因为,在多孔基材的两面上存在粘接性多孔层时,隔膜的两面介由粘接性多孔层与两电极良好地粘接。
从离子透过性和力学强度的观点考虑,多孔层的孔隙率优选为30%~80%,更优选为50%~80%。
对于多孔层的涂布量而言,从与电极的粘接性及离子透过性的观点考虑,在多孔基材的一面上优选为0.5g/m2~3.0g/m2。在多孔基材的两面上设置有多孔层时,对于多孔层的涂布量而言,作为两面的合计,优选为1.0g/m2~6.0g/m2。
对于多孔层的平均厚度而言,从确保与电极的粘接性和高能量密度的观点考虑,在多孔基材的一面上优选为0.5μm~5μm。
多孔层是将下述涂布层固化而形成的层,所述涂布层是将含有树脂和无机粒子中的至少任一者的涂布液涂布于多孔基材上而形成的。因此,多孔层含有树脂及无机粒子的至少任一者。以下,详细说明涂布液及多孔层中含有的树脂及无机粒子。
[树脂]
对于多孔层中包含的树脂而言,优选的是,相对于电解液稳定,且电化学稳定,具有连结无机粒子的功能,可与电极粘接。多孔层可仅包含1种树脂,也可包含2种以上的树脂。
从与电极的粘接性的观点考虑,多孔层中包含的树脂优选为粘接性树脂。由于隔膜与电极介由含有粘接性树脂的多孔层而密合,因此,电池元件的卷绕错位及变形变得更不易发生。
作为粘接性树脂,例如,可举出聚偏二氟乙烯、聚偏二氟乙烯共聚物、苯乙烯-丁二烯共聚物、丙烯腈、甲基丙烯腈等乙烯基腈的均聚物或共聚物、聚环氧乙烷、聚环氧丙烷等聚醚。其中,特别优选聚偏二氟乙烯及聚偏二氟乙烯共聚物(将它们称为“聚偏二氟乙烯系树脂”。)。
作为聚偏二氟乙烯系树脂,可举出偏二氟乙烯的均聚物(即聚偏二氟乙烯);偏二氟乙烯与其他可共聚的单体的共聚物(聚偏二氟乙烯共聚物);它们的混合物。
作为可与偏二氟乙烯共聚的单体,例如,可举出四氟乙烯、六氟丙烯、三氟乙烯、三氯乙烯、氟乙烯等,可使用1种或2种以上。
聚偏二氟乙烯系树脂可利用乳液聚合或悬浮聚合来制造。
从耐热性的观点考虑,多孔层中包含的树脂优选为耐热性树脂(熔点为200℃以上的树脂、或不具有熔点且分解温度为200℃以上的树脂)。作为耐热性树脂,例如,可举出聚酰胺、全芳香族聚酰胺、聚酰亚胺、聚酰胺酰亚胺、聚砜、聚酮、聚醚酮、聚醚砜、聚醚酰亚胺、纤维素、及它们的混合物。其中,从多孔结构的形成容易性、与无机粒子的粘结性、耐氧化性等观点考虑,优选全芳香族聚酰胺。全芳香族聚酰胺中,从多孔层的成型容易进行这样的观点考虑,优选为间位型全芳香族聚酰胺,特别优选为聚间苯二甲酰间苯二胺。
[无机粒子]
对于无机粒子而言,优选的是,相对于电解液稳定,并且,电化学稳定。无机粒子可单独使用1种,也可组合2种以上而使用。
作为无机粒子,例如,可举出氢氧化铝、氢氧化镁、氢氧化钙、氢氧化铬、氢氧化锆、氢氧化铈、氢氧化镍、氢氧化硼等金属氢氧化物;二氧化硅、氧化铝、氧化锆、氧化镁等金属氧化物;碳酸钙、碳酸镁等碳酸盐;硫酸钡、硫酸钙等硫酸盐;硅酸钙、滑石等粘土矿物;等等。其中,从赋予阻燃性、除静电效果的观点考虑,优选金属氢氧化物及金属氧化物。无机粒子可以是利用硅烷偶联剂等进行了表面改性的无机粒子。
无机粒子的粒子形状是任意的,可以是球形、椭圆形、板状、棒状、不定形中的任何形状。从防止电池短路的观点考虑,优选板状的粒子、未凝集的一次粒子。对于无机粒子而言,从与电极的良好的粘接性、离子透过性、滑动性、及多孔层的成型性的观点考虑,一次粒子的体积平均粒径优选为0.01μm~10μm,更优选为0.1μm~10μm。
从与电极的粘接性的观点考虑,多孔层优选至少含有树脂,从耐热性的观点考虑,多孔层优选还含有无机粒子。多孔层含有树脂及无机粒子时,无机粒子在树脂与无机粒子的总量中所占的比例例如为30体积%~90体积%。
多孔层也可含有有机填料、其他成分。作为有机填料,例如,可举出由交联聚(甲基)丙烯酸、交联聚(甲基)丙烯酸酯、交联聚硅氧烷、交联聚苯乙烯、交联聚二乙烯基苯、苯乙烯-二乙烯基苯共聚物交联物、聚酰亚胺、三聚氰胺树脂、酚醛树脂、苯并胍胺-甲醛缩合物等交联高分子形成的粒子;由聚砜、聚丙烯腈、芳族聚酰胺、聚缩醛、热塑性聚酰亚胺等耐热性树脂形成的粒子;等等。
[隔膜的各种物性]
本公开文本中,从机械强度与薄膜电阻的均衡性良好的方面考虑,隔膜的Gurley值(JIS P8117(2009))优选为50秒/100cc~800秒/100cc。
本公开文本中,对于隔膜而言,从离子透过性的观点考虑,从在多孔基材上设置有多孔层的隔膜的Gurley值减去多孔基材的Gurley值而得到的值优选为300秒/100cc以下,更优选为150秒/100cc以下,进一步优选为100秒/100cc以下。
本公开文本中,从机械强度及制成电池时的能量密度的观点考虑,隔膜的膜厚优选为5μm~40μm,更优选为5μm~35μm,进一步优选为10μm~20μm。
[隔膜卷的制造方法]
本公开文本的隔膜卷包括:在制造隔膜后将隔膜直接卷绕于卷芯而成的一次卷、及从一次卷将隔膜卷绕于卷芯而成的二次卷。二次卷包括:从一次卷将隔膜直接进行卷绕而成的卷、及一边将从一次卷送出的隔膜分切成所期望的宽度一边进行卷绕而成的卷。
一次卷的卷芯与二次卷的卷芯可以相同也可以不同。作为两卷芯,没有特别限制,可举出卷绕长条状片材的已知的卷芯。
作为卷芯的材质,可举出树脂、纸、金属等。作为卷芯的一个实施方式,可举出在外周面上具有槽及/或狭缝(slit)的卷芯。作为卷芯的一个实施方式,可举出在外周面上具有用于抑制卷绕的片材的损伤的弹性层(例如橡胶层)的卷芯。
卷芯的轴向的长度只要为卷绕的片材的宽度以上即可,没有特别限制,相对于卷绕的片材的宽度,优选为+0cm~+50cm的长度。卷芯的外径优选为7cm~30cm。
本公开文本中,隔膜是在多孔基材的一面或两面上设置有多孔层的隔膜。多孔层是将下述涂布层固化而形成的层,所述涂布层是将涂布液涂布于多孔基材的一面或两面上而形成的。涂布液含有树脂及无机粒子中的至少任一者。
作为在多孔基材上设置多孔层的方法,可举出下述方法:将涂布液涂布于多孔基材而形成涂布层,然后,通过干燥而使涂布层固化,从而设置多孔层的干式制法;将涂布液涂布于多孔基材而形成涂布层,然后,使涂布层与凝固液接触而使涂布层固化,从而设置多孔层的湿式制法;等等。干式制法与湿式制法相比,多孔层容易变得致密,因此,从可得到良好的多孔结构的方面考虑,湿式制法是优选的。
湿式制法优选具有下述工序:涂布液制备工序,制备含有树脂的涂布液;涂布工序,将涂布液涂布于多孔基材的一面或两面上而形成涂布层;凝固工序,使涂布层与凝固液接触,使涂布层中包含的树脂凝固,得到复合膜(在多孔基材的一面或两面上具有多孔层的片材);水洗工序,对复合膜进行水洗;以及,干燥工序,对复合膜进行干燥。也可以在涂布液中进一步分散无机粒子。
干式制法优选具有下述工序:涂布液制备工序,制备含有树脂的涂布液;涂布工序,将涂布液涂布于多孔基材的一面或两面上而形成涂布层;凝固工序,将涂布层中包含的溶剂除去,使涂布层中包含的树脂凝固,得到复合膜(在多孔基材的一面或两面上具有多孔层的片材)。也可以在涂布液中进一步分散无机粒子。
湿式制法及干式制法的各工序的详细内容如下所述。
-涂布液制备工序-
涂布液制备工序是制备含有树脂的涂布液的工序。涂布液例如通过将树脂溶解于溶剂中、根据需要进一步分散无机粒子而制备。
作为涂布液的制备中使用的溶解树脂的溶剂(以下,也称为“良溶剂”。),可合适地使用N-甲基吡咯烷酮、二甲基乙酰胺、二甲基甲酰胺、二甲基甲酰胺等极性酰胺溶剂。
从形成具有良好的多孔结构的多孔层的观点考虑,优选将诱发相分离的相分离剂混合在良溶剂中。作为相分离剂,可举出水、甲醇、乙醇、丙醇、丁醇、丁二醇、乙二醇、丙二醇、三丙二醇等。优选的是,将相分离剂以可确保适合于涂布的粘度的范围的量与良溶剂混合。
作为涂布液的制备中使用的溶剂,从形成良好的多孔结构的观点考虑,优选包含60质量%以上的良溶剂、10质量%~40质量%的相分离剂的混合溶剂。
对于涂布液而言,从形成良好的多孔结构的观点考虑,优选以相对于涂布液的总质量为3质量%~10质量%的浓度含有树脂。
-涂布工序-
涂布工序是在多孔基材的一面或两面上涂布含有树脂的涂布液而形成涂布层的工序。作为向多孔基材上涂布涂布液的手段,可举出迈耶棒、模涂机、逆转辊涂布机、凹版涂布机等。在多孔基材的两面上形成多孔层时,从生产率的观点考虑,优选在两面同时将涂布液涂布于基材。
-凝固工序-
在湿式制法的情况下,凝固工序是使涂布层与凝固液接触而使涂布层中包含的树脂凝固从而得到复合膜的工序。作为使涂布层与凝固液接触的方法,优选使具有涂布层的多孔基材浸渍于凝固液中,具体而言,优选使具有涂布层的多孔基材通过装有凝固液的槽(凝固槽)。
凝固液通常含有涂布液的制备中使用的良溶剂及相分离剂、和水。在生产上,优选良溶剂和相分离剂的混合比与涂布液的制备中使用的混合溶剂的混合比一致。从多孔结构的形成及生产率的观点考虑,优选凝固液中的水的含量为40质量%~80质量%。凝固液的温度例如为20℃~50℃。
在干式制法的情况下,凝固工序是通过干燥而除去涂布层中包含的溶剂、使涂布层中包含的树脂凝固从而得到复合膜的工序。干式制法中,从复合膜中除去溶剂的方法不受限制,例如,可举出下述方法:使复合膜与发热构件接触的方法;将复合膜输送到调节了温度及湿度的室(chamber)内的方法;等等。
-水洗工序-
水洗工序是在湿式制法中出于除去复合膜中包含的溶剂(涂布液中包含的溶剂、及凝固液中包含的溶剂)的目的而对复合膜进行水洗的工序。具体而言,水洗工序优选通过将复合膜输送到装有水的槽(水洗槽)中而进行。水洗用的水的温度例如为20℃~50℃。
-干燥工序-
干燥工序是在水洗工序后、出于从水洗后的复合膜中除去水的目的而进行的工序。干燥方法不受限制,例如,可举出下述方法:使复合膜与发热构件接触的方法;将复合膜输送至调节了温度及湿度的室内的方法;向复合膜吹热风的方法;等等。在向复合膜赋予热时,其温度例如为50℃~80℃。
一次卷可通过将依次进行上述各工序而制造的隔膜直接卷绕于卷芯来制造。二次卷可通过从一次卷将隔膜进一步进行卷绕来制造。在制造一次卷时,隔膜的卷绕速度例如为10m/min~100m/min,基于对生产率的考虑,更优选为40m/min~100m/min。另一方面,在制造二次卷时,隔膜的卷绕速度例如为10m/min~200m/min,基于对生产率的考虑,更优选为50m/min~200m/min。
在湿式制法或干式制法的各工序中,从在将25℃下MD方向收缩率控制为1.0%以下的同时制造褶皱少的外观良好的隔膜的观点考虑,优选应用以下的(a)~(g)。
(a)在隔膜的制造中,使用内部应力小的多孔基材。因此,本公开文本中,优选充分实施了热固定的多孔基材。
(b)尽可能降低在多孔基材上涂布涂布液时的拉伸比(涂布结束时的输送速度相对于涂布开始时的输送速度的比)。
(c)在通过凝固槽及水洗槽时,作用于输送物的输送阻力大,因此,多孔基材容易被拉伸,结果,有时在隔膜上产生褶皱。为了抑制上述情况,尽可能地降低凝固液及水洗槽的水的温度。凝固液及水洗槽的水的温度优选为40℃以下,更优选为35℃以下,进一步优选为25℃左右。
(d)在干燥工序中向复合膜赋予热的情况下,为了抑制因热收缩而导致的复合膜的尺寸变化,还设置使复合膜与辊构件等接触的松弛工序。
(e)各工序的拉伸比(工序结束时的输送速度相对于该工序开始时的输送速度的比)的降低与输送物中的褶皱的产生存在权衡关系,因此,单纯降低各工序的拉伸比时,容易在多孔基材及隔膜中产生褶皱。作为输送上的对策,实施下述对策:使输送辊全部为驱动辊;缩短输送辊之间的距离;设置展平褶皱的扩展器(expander)、夹送辊;等等。由于在向多孔基材上涂布涂布液时对多孔基材施加的张力也最强,因此,特别地,在即将涂布之前设置夹送辊。
(f)尽可能降低隔膜的卷绕速度相对于多孔基材的送出速度的速度比(%)(隔膜的卷绕速度÷多孔基材的送出速度×100)(本公开文本中,称为“总体拉伸比”。)。总体拉伸比优选为103%以下,更优选为102%以下,但优选为100%以上。
(g)尽可能降低将隔膜卷绕于卷芯时向隔膜施加的张力。但是,过度降低该张力时,在隔膜中产生褶皱,因此,优选采用与(e)同样的输送上的对策。
此外,在将隔膜卷绕于卷芯后,可通过以下的(h)~(k),将25℃下MD方向收缩率控制为1.0%以下。
(h)针对一次卷,实施在热环境中放置的热处理(退火)。退火温度(热环境的温度)优选为40℃~110℃,更优选为50℃~90℃。但是,退火温度超过90℃时,需要注意多孔基材中包含的树脂部分熔融、或者发生隔膜彼此粘接的粘连现象。处理时间(热环境下的放置时间)越长越优选,例如为12小时以上。
(i)一边将从一次卷送出的隔膜分切一边将其卷绕于卷芯而制造二次卷时,尽可能降低从一次卷送出隔膜时向隔膜施加的张力、及将隔膜卷绕于卷芯时向隔膜施加的张力。但是,为了得到分切端的外观良好的隔膜,两种张力需要以一定程度施加。
(j)在制造二次卷时,为了不在隔膜中产生褶皱地将隔膜卷绕于卷芯,优选在即将卷绕之前用辊构件(即,接触辊)向隔膜施加接触压力,该情况下,尽可能降低辊构件的接触压力。
(k)针对二次卷,实施在热环境中放置的热处理(退火)。但是,热处理有时引起隔膜的宽度方向两端的松弛,因此,需要注意热处理的温度及处理时间。温度优选为40℃~70℃,更优选为40℃~60℃。处理时间例如为1小时~48小时。
作为制造本公开文本的隔膜卷的制造方法,可举出下述的实施方式作为优选例。
隔膜卷的制造方法的一个实施方式是利用湿式制法在多孔基材的一面或两面上设置多孔层的制造方法,凝固液的温度为40℃以下(优选为35℃以下,更优选为25℃左右)。
隔膜卷的制造方法的一个实施方式包括以下述卷绕速度将隔膜卷绕于卷芯的步骤,所述卷绕速度相对于多孔基材的送出速度的速度比为103%以下(优选为100%~103%,更优选为100%~102%)。根据该实施方式,容易制作褶皱少、卷绕形态良好的一次卷,也容易将加工成2次卷后的收缩率抑制为低值。
隔膜卷的制造方法的一个实施方式包括下述步骤:将在制造隔膜后将隔膜直接卷绕于卷芯而成的卷在40℃~110℃的气氛中放置12小时以上(例如24小时)。通过该实施方式,可抑制多孔性基材及涂布层的多孔结构的闭塞。尤其是,在涂布层为包含粘接性树脂的涂布层时,可抑制粘连现象(隔膜卷中相互叠合的隔膜彼此粘接的现象)、及涂布层的多孔结构的闭塞。隔膜卷的制造方法的一个实施方式更优选将上述卷在50℃~80℃的气氛中放置12小时以上(例如24小时)。
作为本公开文本的隔膜卷,可举出下述的实施方式作为优选例。
隔膜卷的一个实施方式中,隔膜所具有的多孔层是利用湿式制法在多孔基材的一面或两面上设置的多孔层,是通过与温度为40℃以下(优选为35℃以下,更优选为25℃左右)的凝固液接触从而使涂布层中的树脂固化而形成的多孔层。
隔膜卷的一个实施方式是在制造隔膜后将隔膜直接卷绕于卷芯而成的一次卷、或从一次卷将隔膜卷绕于卷芯而成的二次卷,一次卷是以103%以下(优选为100%~103%,更优选为100%~102%)的总体拉伸比将隔膜卷绕于卷芯而成的卷。通过该实施方式,可抑制多孔性基材及涂布层的多孔结构的闭塞。尤其是,在涂布层为包含粘接性树脂的涂布层时,可抑制粘连现象及涂布层的多孔结构的闭塞。
隔膜卷的一个实施方式为在制造隔膜后将隔膜直接卷绕于卷芯而成的一次卷、或从一次卷将隔膜卷绕于卷芯而成的二次卷,一次卷是被实施了下述操作的卷,所述操作为:在40℃~110℃(优选为50℃~80℃)的气氛中放置12小时以上(例如24小时)。通过该实施方式,可抑制多孔性基材及涂布层的多孔结构的闭塞。尤其是,在涂布层为包含粘接性树脂的涂布层时,可抑制粘连现象及涂布层的多孔结构的闭塞。
一次卷的一个实施方式例如为卷绕至少100m以上、至多3000m以下的宽度为200mm~2000mm的隔膜而成的卷。
二次卷的一个实施方式例如为卷绕至少100m以上、至多2500m以下的宽度为15mm~500mm的隔膜而成的卷。
隔膜卷的一个实施方式中,隔膜卷的直径例如为15cm~30cm。
本公开文本的隔膜卷可用于制造一次电池及二次电池。以下,对将本公开文本的隔膜卷中卷绕的隔膜应用于二次电池的实施方式例进行说明。
<非水系二次电池>
本公开文本的非水系二次电池是通过锂的掺杂·脱掺杂而获得电动势的非水系二次电池,具有正极、负极、和从本公开文本的隔膜卷供给的隔膜。非水系二次电池具有电池元件被封入到外部封装材料内而成的结构,所述电池元件是在负极和正极隔着隔膜对置而成的结构体中含浸电解液而得到的。掺杂是指吸藏、担载、吸附、或嵌入,是指锂离子进入到正极等电极的活性物质中的现象。
本公开文本的非水系二次电池适合于非水电解质二次电池,特别适合于锂离子二次电池。
本公开文本的非水系二次电池使用从本公开文本的隔膜卷供给的隔膜进行制造,由此,在制造电池元件时,不易引起卷绕错位。另外,本公开文本的非水系二次电池具有从本公开文本的隔膜卷供给的隔膜,由此,电池元件不易发生变形。因此,对于本公开文本的非水系二次电池而言,电池的制造成品率高。
作为本公开文本的非水系二次电池中正极的实施方式例,可举出包含正极活性物质及粘结剂树脂的活性物质层被成型在集电体上而成的结构。活性物质层还可包含导电助剂。作为正极活性物质,例如,可举出含锂的过渡金属氧化物等,具体而言,可举出LiCoO2、LiNiO2、LiMn1/2Ni1/2O2、LiCo1/3Mn1/3Ni1/3O2、LiMn2O4、LiFePO4、LiCo1/2Ni1/2O2、LiAl1/4Ni3/4O2等。作为粘结剂树脂,例如,可举出聚偏二氟乙烯系树脂等。作为导电助剂,例如,可举出乙炔黑、科琴黑、石墨粉末等碳材料。作为集电体,例如,可举出厚度为5μm~20μm的铝箔、钛箔、不锈钢箔等。
作为本公开文本的非水系二次电池中负极的实施方式例,可举出包含负极活性物质及粘结剂树脂的活性物质层被成型在集电体上而成的结构。活性物质层还可包含导电助剂。作为负极活性物质,可举出能电化学地吸藏锂的材料,具体而言,例如,可举出碳材料;硅、锡、铝等与锂的合金;等等。作为粘结剂树脂,例如,可举出聚偏二氟乙烯系树脂、苯乙烯-丁二烯橡胶等。作为导电助剂,例如,可举出乙炔黑、科琴黑、石墨粉末等碳材料。作为集电体,例如,可举出厚度为5μm~20μm的铜箔、镍箔、不锈钢箔等。代替上述的负极,也可使用金属锂箔作为负极。
本公开文本的非水系二次电池中的电解液例如是将锂盐溶解于非水系溶剂而得到的溶液。作为锂盐,例如,可举出LiPF6、LiBF4、LiClO4等。作为非水系溶剂,例如,可举出碳酸亚乙酯、碳酸1,2-亚丙酯、氟代碳酸亚乙酯、二氟代碳酸亚乙酯等环状碳酸酯;碳酸二甲酯、碳酸二乙酯、碳酸甲乙酯、及其氟取代物等链状碳酸酯;γ-丁内酯、γ-戊内酯等环状酯;等等,它们可单独使用,也可混合使用。作为电解液,将环状碳酸酯和链状碳酸酯以20∶80~40∶60的质量比(环状碳酸酯∶链状碳酸酯)混合、并溶解0.5M~1.5M锂盐而得到的电解液是优选的。
作为本公开文本的非水系二次电池的外部封装材料,可举出金属外壳、铝层压膜制包装等。本公开文本的非水系二次电池的形状可以是方型、扁平型、圆筒型、纽扣型等中的任何形状。本公开文本中的隔膜适合于上述任意形状。
本公开文本的非水系二次电池的制造方法没有特别限制。本公开文本的非水系二次电池的电池元件例如可利用将正极、隔膜、负极、隔膜依次重叠、并沿长度方向卷绕的方式制造。
作为本公开文本的非水系二次电池的实施方式例,可举出使用了具有含有粘接性树脂的多孔层的隔膜的电池。该非水系二次电池中,隔膜与电极介由含有粘接性树脂的多孔层而密合,因此,电池元件的卷绕错位及变形变得更不易发生,结果,电池的制造成品率变得更高。
实施例
以下举出实施例,进一步具体说明本公开文本的隔膜卷及非水系二次电池。但是,本公开文本的隔膜卷及非水系二次电池不限于以下的实施例。本例中的膜厚及Gurley值的测定方法如下所述。
[膜厚]
多孔基材及复合膜的膜厚(μm)通过以下方式求出:使用接触式的厚度计(Mitutoyo Corporation制LITEMATIC),测定10cm×30cm内的任意的20个点,求出其平均值。使用直径为5mm的圆柱状的测定端子,在负荷为7g的条件下进行测定。
[Gurley值]
按照JIS P8117(2009),使用Gurley式透气度测定仪(东洋精机公司制G-B2C)测定多孔基材的Gurley值(秒/100cc)。
<实施例1>
将作为聚偏二氟乙烯系树脂(PVDF系树脂)的将KUREHA CORPORATION制的KF聚合物#9300和ARKEMA公司制的KYNAR2801以50∶50的质量比混合而成的树脂溶解于溶剂(二甲基乙酰胺∶三丙二醇=70∶30(质量比))中,制作PVDF系树脂的浓度为5质量%的涂布液。将该涂布液等量涂布于多孔基材(聚乙烯微多孔膜,SK公司制TN0901,膜厚为9μm,Gurley值为150秒/100cc)的两面,在多孔基材的两面上形成涂布层。将形成涂布层后的多孔基材浸渍于凝固液(水∶二甲基乙酰胺∶三丙二醇=62.5∶30∶7.5(质量比),温度为35℃)中,使涂布层固化,得到在聚乙烯微多孔膜的两面上具有多孔层的复合膜。接下来,对复合膜进行水洗并干燥,在卷芯(纸制,内径为15cm,外径为18cm)上卷绕500m,对该卷实施在75℃的气氛中放置24小时的热处理,得到一次卷。使制造一次卷时的总体拉伸比为102.0%。
接下来,将一次卷在室温下放置而进行冷却,然后,一边将从一次卷送出的隔膜分切成100mm宽,一边将其在卷芯(合成树脂制,内径为7.6cm,外径为20cm)上卷绕400m,得到卷为100mm×400m的二次卷。
<实施例2>
将对一次卷实施的热处理的条件变更为50℃且为24小时,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<实施例3>
将对一次卷实施的热处理的条件变更为50℃且为24小时,将制造一次卷时的总体拉伸比变更为103.0%,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<实施例4>
将聚间苯二甲酰间苯二胺(PMIA)(Teijin Techno Products公司制Conex)溶解于溶剂(二甲基乙酰胺∶三丙二醇=70∶30(质量比))中,制作PMIA浓度为5质量%的溶液。在该溶液中分散作为无机粒子的α-氧化铝(岩谷化学工业公司制SA-1,平均粒径为0.8μm),使得α-氧化铝∶PMIA=50∶50(质量比),制作涂布液。使用该涂布液,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<实施例5>
将制造一次卷时的总体拉伸比变更为103.0%,除此之外,与实施例4同样地操作,得到一次卷及二次卷。
<实施例6>
按照日本特开2013-139652号公报中公开的芳族聚酰胺纤维无纺布的制造方法,制作膜厚为30μm的芳族聚酰胺纤维无纺布。使用该无纺布作为多孔基材,将总体拉伸比变更为100.2%,除此之外,与实施例4同样地操作,得到一次卷及二次卷。
<实施例7>
作为多孔基材,使用膜厚为30μm的聚对苯二甲酸乙二醇酯(PET)纤维无纺布。作为聚偏二氟乙烯系树脂(PVDF系树脂),使用将KUREHA CORPORATION制的KF聚合物#9300和ARKEMA公司制的KYNAR2801以50∶50的质量比混合而成的树脂。将该PVDF系树脂溶解于溶剂(二甲基乙酰胺∶三丙二醇=70∶30(质量比))中,制作树脂浓度为5质量%的溶液。在该溶液中分散作为无机粒子的α-氧化铝(岩谷化学工业公司制SA-1,平均粒径为0.8μm),使得α-氧化铝∶PVDF系树脂=50∶50(质量比),制作涂布液。使用该多孔基材和该涂布液,将总体拉伸比变更为100.2%,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<比较例1>
将对一次卷实施的热处理的条件变更为35℃且为24小时,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<比较例2>
将用于使涂布层固化的凝固液的温度变更为50℃,使总体拉伸比为103.5%,不对一次卷实施热处理,除此之外,与实施例1同样地操作,得到一次卷及二次卷。
<评价>
针对实施例1~7及比较例1~2,如下所述地进行隔膜卷的评价。将结果示于表1。
[一次卷的外观]
目视观察一次卷,判定有无褶皱。在观察时,由于照射光时容易观察到褶皱,因此照射光而进行观察。
-评价基准-
A:未确认到褶皱。
B:存在褶皱,但为不妨碍实用的程度。
C:存在大量褶皱。
[隔膜的25℃下MD方向收缩率及25℃下TD方向扩大率]
为了去除一次卷或二次卷的最表层,从一次卷或二次卷的外端取出5倍周长量的隔膜并将其切除。从该切除端切取长度为200mm的隔膜,将其作为试验片(MD方向200mm×TD方向100mm)。
在试验片的一面上,在图1所示的位置A1、A2、B1、B2、C1、C2、C3、D1、D2及D3上标注标记。用夹具把持试验片的一端,将试验片以MD方向成为重力方向的方式悬吊于温度为25℃、相对湿度为50±10%的恒温槽中,在无张力状态下放置24小时。
在进行24小时放置之前和之后,测定A1B1间、A2B2间、C1D1间、C2D2间及C3D3间的长度,利用下式算出MD方向的收缩率(%)和TD方向的扩大率(%)。
25℃下MD方向收缩率(%)={[(放置前的A1B1间的长度-放置后的A1B1间的长度)÷放置前的A1B1间的长度]+[(放置前的A2B2间的长度-放置后的A2B2间的长度)÷放置前的A2B2间的长度]}÷2×100
即,将A1B1间的收缩率与A2B2间的收缩率的平均值作为25℃下MD方向收缩率。
25℃下TD方向扩大率(%)={[(放置后的C1D1间的长度-放置前的C1D1间的长度)÷放置前的C1D1间的长度]+[(放置后的C2D2间的长度-放置前的C2D2间的长度)÷放置前的C2D2间的长度]+[(放置后的C3D3间的长度-放置前的C3D3间的长度)÷放置前的C3D3间的长度]}÷3×100
即,将C1D1间的扩大率、C2D2间的扩大率和C3D3间的扩大率的平均值作为25℃下TD方向扩大率。
虽然在本例中使试验片的TD方向长度为100mm,但对于求出25℃下MD方向收缩率及25℃下TD方向扩大率而言,TD方向长度不限于此。
在本例中,使得从开始自一次卷或二次卷的外端取出隔膜起、直至将试验片悬吊于恒温槽为止(即,直至开始进行24小时放置为止)的时间为10分钟以内,从恒温槽中取出试验片后,立即进行24小时放置后的长度测定。试验片的长度、A1等标记的位置、及A1B1间等的长度使用大山光学制玻璃刻度尺进行测定,用50倍的放大镜,读取至0.00mm刻度。
[135℃下的隔膜的热收缩率]
从一次卷或二次卷中切出MD方向190mm×TD方向60mm的隔膜,将其作为试验片。在位于将TD方向2等分的线上、并且距MD方向的一方的端部20mm及170mm的2点(称为点A及点B。)处标注标记。用夹具把持距点A最近的端部与点A之间,将试验片以MD方向成为重力方向的方式悬吊在135℃的烘箱中,在无张力状态下进行30分钟热处理。测定热处理前后的AB间的长度,利用下式算出热收缩率(%)。
MD方向的热收缩率(%)=(热处理前的AB间的长度-热处理后的AB间的长度)÷热处理前的AB间的长度×100
虽然在本例中使试验片的TD方向长度为60mm,但对于求出135℃热收缩率而言,TD方向长度不限于此。
[电池元件的卷绕错位]
从二次卷供给隔膜,将正极、隔膜、负极、隔膜依次重叠,使用卷绕装置沿长度方向卷绕,制作电池元件。在卷绕时,向正极、负极分别施加了300g的张力,向隔膜施加了100g的张力。在制作电池元件之后,测定2片隔膜的卷绕错位(mm)。将隔膜的卷绕错位为0.2mm以上的情况判定为“有卷绕错位产生”,将小于0.2mm的情况判定为“无卷绕错位产生”。按照以下方式制作本试验中使用的负极及正极。
-负极的制作-
利用双臂式混合机,对300质量份作为负极活性物质的人造石墨、7.5质量份作为粘结剂的含有40质量%苯乙烯-丁二烯共聚物的改性物的水溶性分散液、3质量份作为增稠剂的羧甲基纤维素、及适量的水进行搅拌,制作负极用浆料。将该负极用浆料涂布于作为负极集电体的厚度为10μm的铜箔的两面,干燥后进行加压,得到具有负极活性物质层的负极。
-正极的制作-
将89.5质量份作为正极活性物质的钴酸锂粉末、4.5质量份作为导电助剂的乙炔黑、及6质量份作为粘结剂的聚偏二氟乙烯溶解于N-甲基-2-吡咯烷酮中,使得聚偏二氟乙烯的浓度成为6质量%,利用双臂式混合机进行搅拌,制作正极用浆料。将该正极用浆料涂布于作为正极集电体的厚度为20μm的铝箔的两面,干燥后进行加压,得到具有正极活性物质层的正极。
[电池元件的外观]
在温度为25±3℃、相对湿度为50±10%的气氛中,利用与上述相同的工序制作电池元件,在相同气氛中将电池元件放置1小时。在进行1小时放置之前和之后,测定电池元件的最大直径(mm),利用下式算出膨胀率(%)。膨胀率越大,表示电池元件膨胀程度越大,表示电池元件的外观越不良。
膨胀率(%)=(放置后的最大直径-放置前的最大直径)÷放置前的最大直径×100
-评价基准-
A:膨胀率小于5%。
B:膨胀率为5%以上且小于10%。
C:膨胀率为10%以上。
[电池元件的合格率]
在温度为25±3℃、相对湿度为50±10%的气氛中,利用与上述相同的工序制作20个电池元件,对各电池元件实施热压(压力为1MPa,温度为95℃)。将热压后的各电池元件拆开,观察电极及隔膜,将在电极上无裂纹并且在隔膜上未观察到褶皱、折断的情况判断为合格品,算出20个的合格率(合格品的个数÷20×100)。
将于2014年7月11日提出申请的日本申请号第2014-143662号的全部公开内容通过参照并入本说明书中。
本说明书中记载的所有文献、专利申请、及技术标准通过参照被并入本说明书中,各文献、专利申请、及技术标准通过参照被并入的程度与具体且分别地记载的情况的程度相同。
Claims (8)
1.隔膜卷,所述隔膜卷是将非水电解质电池用隔膜卷绕于卷芯而得到的,所述非水电解质电池用隔膜具有:
多孔基材;和
多孔层,所述多孔层是将下述涂布层固化而形成的,所述涂布层是将含有树脂和无机粒子中的至少任一者的涂布液涂布于所述多孔基材的一面或两面而形成的,
所述隔膜卷是一次卷或二次卷,所述一次卷是在制造所述非水电解质电池用隔膜后将所述非水电解质电池用隔膜直接卷绕于卷芯而成的,所述二次卷是从所述一次卷将所述非水电解质电池用隔膜卷绕于卷芯而成的,
所述一次卷的、卷绕于所述卷芯时的所述非水电解质电池用隔膜的卷绕速度相对于所述多孔基材的送出速度的速度比为100%以上103%以下,
利用下述的方法(1)求出的所述非水电解质电池用隔膜的机械方向的收缩率为1.0%以下,
方法(1):自隔膜卷的外端起去除5倍周长量的非水电解质电池用隔膜,然后,自其端部起在机械方向上切取200mm的非水电解质电池用隔膜作为试样,将所述试样在25℃下、在无张力状态下放置24小时,测定所述放置前后的机械方向的长度,利用下式算出机械方向的收缩率,
机械方向的收缩率(%)=(放置前的机械方向的长度-放置后的机械方向的长度)÷放置前的机械方向的长度×100。
2.如权利要求1所述的隔膜卷,其中,所述多孔基材含有熔点低于200℃的热塑性树脂。
3.如权利要求1或2所述的隔膜卷,其中,所述一次卷是被实施了下述操作的隔膜卷,所述操作为:在40℃以上110℃以下的气氛中放置12小时以上。
4.如权利要求1或2所述的隔膜卷,其中,利用下述的方法(2)求出的所述非水电解质电池用隔膜的宽度方向的扩大率为0%以上0.6%以下,
方法(2):自隔膜卷的外端起去除5倍周长量的非水电解质电池用隔膜,然后,自其端部起在机械方向上切取200mm的非水电解质电池用隔膜作为试样,将所述试样在25℃下、在无张力状态下放置24小时,测定所述放置前后的宽度方向的长度,利用下式算出宽度方向的扩大率,
宽度方向的扩大率(%)=(放置后的宽度方向的长度-放置前的宽度方向的长度)÷放置前的宽度方向的长度×100。
5.如权利要求1或2所述的隔膜卷,其中,利用下述的方法(3)求出的所述非水电解质电池用隔膜的机械方向的热收缩率为3%以上40%以下,
方法(3):从隔膜卷切出非水电解质电池用隔膜,得到机械方向的长度为190mm的试样,针对所述试样进行在135℃下、在无张力状态下放置30分钟的热处理,测定所述热处理前后的机械方向的长度,利用下式算出机械方向的热收缩率,
机械方向的热收缩率(%)=(热处理前的机械方向的长度-热处理后的机械方向的长度)÷热处理前的机械方向的长度×100。
6.如权利要求1或2所述的隔膜卷,其中,利用所述方法(1)求出的所述非水电解质电池用隔膜的机械方向的收缩率为0.5%以下。
7.如权利要求1或2所述的隔膜卷,其中,所述涂布液含有粘接性树脂。
8.非水系二次电池,其具有:
正极;
负极;和
非水电解质电池用隔膜,所述非水电解质电池用隔膜被配置于所述正极和所述负极之间,是从权利要求1~7中任一项所述的隔膜卷供给的,
所述非水系二次电池通过锂的掺杂·脱掺杂而获得电动势。
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2015
- 2015-06-24 KR KR1020227045404A patent/KR20230007535A/ko not_active IP Right Cessation
- 2015-06-24 CN CN201580037576.8A patent/CN106537643B/zh active Active
- 2015-06-24 US US15/324,415 patent/US20180183028A1/en not_active Abandoned
- 2015-06-24 JP JP2015551300A patent/JP5918455B1/ja active Active
- 2015-06-24 WO PCT/JP2015/068234 patent/WO2016006453A1/ja active Application Filing
- 2015-06-24 KR KR1020177000473A patent/KR20170029494A/ko not_active Application Discontinuation
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Publication number | Publication date |
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CN106537643A (zh) | 2017-03-22 |
WO2016006453A1 (ja) | 2016-01-14 |
KR20230007535A (ko) | 2023-01-12 |
KR20170029494A (ko) | 2017-03-15 |
JP5918455B1 (ja) | 2016-05-18 |
US20180183028A1 (en) | 2018-06-28 |
JPWO2016006453A1 (ja) | 2017-04-27 |
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Application publication date: 20170322 Assignee: SHANGHAI ENJIE NEW MATERIAL TECHNOLOGY Co.,Ltd. Assignor: TEIJIN Ltd. Contract record no.: X2022990000978 Denomination of invention: Diaphragm roll and non-aqueous secondary battery Granted publication date: 20191025 License type: Common License Record date: 20221210 |