CN106553403B - 一种具有优异耐酸腐蚀性能的铝塑复合膜及其制备方法 - Google Patents
一种具有优异耐酸腐蚀性能的铝塑复合膜及其制备方法 Download PDFInfo
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Abstract
一种具有优异耐酸腐蚀性能的铝塑复合膜,其特征在于自内至外依次包括流延聚丙烯层、第一胶黏层、第一硬脂酸膜层、铝箔层、第二硬脂酸膜层、第二胶黏层和外保护层,所述外保护层为双向拉伸聚对苯二甲酸乙二醇酯层或双向拉伸聚酰胺层。本发明还提供上述具有优异耐酸腐蚀性能的铝塑复合膜的一种制备方法。本发明的铝塑复合膜可作为锂离子电池的外壳用包装材料,具有优异的耐酸腐蚀性能,能够为锂离子电池提供可靠的保护,确保其使用寿命。本发明的铝塑复合膜在90±5%相对湿度、85±2℃环境中浸泡电解液14天后,超疏水铝层与流延聚丙烯层不分层,无损坏,且剥离力维持在8‑10N/15mm。
Description
技术领域
本发明涉及电池外壳用包装材料,具体涉及一种具有优异耐酸腐蚀性能的铝塑复合膜及其制备方法。
背景技术
锂离子二次电池被广泛用于笔记本电脑、摄像机、便携电话、电动汽车等的电源。作为该锂离子二次电池,利用外壳保卫电池本体周围的结构,称为外壳用包装材料。锂离子软包电池需要用铝塑复合膜对其进行热封包装,包装对其来说是一个不可或缺的重要组成部分,锂电池不能脱离包装而独立存在,包装的使用寿命与锂电池的使用寿命具有相同的寿命周期。
钢壳或铝壳等硬盒封装的锂电池在化成(指对新生产的电池初次充电过程,是对电池材料激活活性)和后续使用过程中均会释放气体,如未能及时排气将会影响电池的电化学性能,当内部气压增大到一定值会导致电池***。目前已有将由拉伸聚酰胺层、铝箔层、热塑性树脂层按顺序粘合一体化而成的包装材料,俗称铝塑复合膜。采用铝塑复合膜作为封装材料的软包装锂电池,可以利用铝塑复合膜这种柔性材料膨胀释放压力,从而防止电池***,增加使用安全性。
锂电池内含有作为离子传输载体的电解液,一般是由碳酸酯类有机溶剂和六氟磷酸锂盐组成。六氟磷酸锂易吸潮,产生氢氟酸,腐蚀电池包装材料,致使锂电池胀气鼓包,最终失效。为满足电池使用质量的稳定性要求,要求作为包装材料的铝塑复合膜具有足够强的耐酸腐蚀性能。
为了增强铝塑复合膜的耐酸腐蚀性能,目前采用的方法有:采用六价铬盐、酸、氟化物的混合溶液对铝箔进行单面或双面的化学处理,以提高铝箔材料的抗酸腐蚀性能;或者在铝塑复合膜的内层热塑性树脂层上再涂覆功能性涂层(如油酸酰胺、芥酸酰胺、液体石蜡等),以避免电解液直接接触热塑性树脂层。然而上述包装材料尚存在下述缺陷:(1)使用六价铬离子,对环境和人体有重大危害,且处理后的铝箔层与其内侧的热塑性树脂层及其外侧的拉伸聚酰胺层粘结性能降低;(2)虽然改善了材料与模具的机械性能适应性,但牺牲了自身部分的密封性能;(3)仅靠热塑性树脂层及其功能性涂层无法保证达到耐电解液腐蚀的目的。
发明内容
本发明所要解决的技术问题是提供一种铝塑复合膜以及这种铝塑复合膜的制备方法,这种铝塑复合膜可作为锂离子电池的外壳用包装材料,具有优异的耐酸腐蚀性能。采用的技术方案如下:
一种具有优异耐酸腐蚀性能的铝塑复合膜,其特征在于自内至外依次包括流延聚丙烯层、第一胶黏层、第一硬脂酸膜层、铝箔层、第二硬脂酸膜层、第二胶黏层和外保护层,所述外保护层为双向拉伸聚对苯二甲酸乙二醇酯层(双向拉伸PET层)或双向拉伸聚酰胺层(双向拉伸PA层)。
优选方案中,在铝箔层的内侧表面、外侧表面上形成第一硬脂酸膜层、第二硬脂酸膜层的方法依次包括下述步骤:
(1)将铝箔浸入温度为20-30℃的盐酸-草酸混合溶液中,浸泡0.5-2min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸5-20克,浓盐酸(氯化氢含量为37wt%)5-100克,余量为水;
(2)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为20-30℃的高锰酸钾溶液中,浸泡1-2min;
每升高锰酸钾溶液含有:高锰酸钾5-32克,余量为水;
(3)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥(优选在70-80℃下烘干);
(4)将铝箔浸入质量百分比浓度为0.1-1%的硬脂酸乙醇溶液中,浸泡1-10分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥(优选用50-70℃热风干燥),在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层。
优选步骤(1)中,所用铝箔是厚度为30-50μm的铝合金箔。
上述步骤(1)中,盐酸-草酸混合溶液对铝箔浸渍酸刻蚀,在铝箔表面形成微米级多孔结构。盐酸-草酸混合液对铝箔表面作用:将铝箔浸入盐酸-草酸混合溶液中,铝箔表面的氧化膜首先被溶解;接着铝箔表面的高能量点区在遇到盐酸时,会优先腐蚀(点状腐蚀),随后在氢气以及酸的作用下使腐蚀孔内部金属发生溶解,由于金属内部晶格缺陷的不均匀性,使金属刻蚀速度不一致,也就导致表面腐蚀程度不一样,出现了许多尺寸不一的凹凸微细结构,从而在铝箔表面形成微米级的无规则多孔结构。草酸属于弱酸,对铝及氧化膜溶解性小,起到酸性缓蚀剂的作用。
步骤(2)中,高锰酸钾溶液对铝箔浸渍,高锰酸钾作为一种强氧化剂、钝化剂,可以在微米级多孔结构的铝表面上再形成一层更细小的(纳米级)、更致密的氧化层,从而在铝箔表面形成微、纳米相间的多孔结构的颗粒层(该多孔结构颗粒层的孔深约1-5μm,孔径约1-2μm,孔间距约5-20μm),使铝箔层表面粗糙化。
上述步骤(4)中,将经表面粗糙化的铝箔浸泡在硬脂酸乙醇溶液中时,硬脂酸乙醇溶液可渗入到铝箔表面的孔隙中,并包裹住多孔结构的颗粒层,这样,形成的第一硬脂酸膜层、第二硬脂酸膜层将颗粒层包裹住,并与铝箔层表面紧密结合。硬脂酸为低表面能物质,与微米多孔结构颗粒层相互交织,形成致密的覆膜层(即第一硬脂酸膜层、第二硬脂酸膜层),具有超疏水特性,优良的耐酸腐蚀性;同时,硬脂酸是一种饱和的脂肪酸,分子长链中均以亚甲基单键相连,内部的碳原子键合着两个氢原子,硬脂酸分子可通过离子键与铝箔表面的多孔结构层结合而使覆膜层粘附性强,表面性能稳定,因而第一硬脂酸膜层、第二硬脂酸膜层与铝箔表面结合力大,可进一步与第一胶黏层和第二胶黏层形成良好的粘结,易于与塑性树脂层和外保护层粘结。
上述第一硬脂酸膜层、第二硬脂酸膜层为稳定的超疏水层。通常,上述第一硬脂酸膜层、第二硬脂酸膜层与水的接触角均大于150°,水滴滚动角均小于10°。优选上述第一硬脂酸膜层、第二硬脂酸膜层与水的接触角均大于160°,水滴滚动角均小于7°。优选上述第一硬脂酸膜层、第二硬脂酸膜层的厚度均为3-10μm。
所形成的超疏水铝箔(由第一硬脂酸膜层、铝箔层和第二硬脂酸膜层组成)在普通空气环境和弱酸性水溶液环境中都具有良好的超疏水稳定性。
上述第一硬脂酸膜层、第二硬脂酸膜层与水的接触角可通过视屏光学接触角测量仪测定,采用液滴测试法测量,测量时所用的水滴为7μl-9μl。水滴滚动角可采用下述方法测试:将需测试的超疏水铝箔样品固定于带量角器的样品台上,然后从0°开始小心地倾斜样台,再用微量注射器将5μl-9μl水滴滴在样品台上,水滴滚落铝箔样品表面时样品台倾斜角就为该超疏水铝箔表面的水滴滚动角。
上述流延聚丙烯层(也称无拉伸聚丙烯膜层)作为热封层。
聚酰胺(PA)俗称尼龙,优选其中的尼龙6或尼龙66作为双向拉伸聚酰胺层的材料。
优选方案中,上述外保护层的厚度为10-30μm,流延聚丙烯层的厚度为30-100μm。
本发明还提供上述具有优异耐酸腐蚀性能的铝塑复合膜的一种制备方法,其特征在于包括下述步骤:
(1’)将铝箔浸入温度为20-30℃的盐酸-草酸混合溶液中,浸泡0.5-2min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸5-20克,浓盐酸5-100克,余量为水;
(2’)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为20-30℃的高锰酸钾溶液中,浸泡1-2min;
每升高锰酸钾溶液含有:高锰酸钾5-32克,余量为水;
(3’)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥(优选在70-80℃下烘干);
(4’)将铝箔浸入质量百分比浓度为0.1-1%的硬脂酸乙醇溶液中,浸泡1-10分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥(优选用50-70℃热风干燥),在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层;
(5’)在第二硬脂酸膜层的外侧面上形成第二胶黏层并粘结上双轴拉伸聚对苯二甲酸乙二醇酯薄膜或双向拉伸聚酰胺薄膜,形成外保护层;并在第一硬脂酸膜层的内侧面上形成第一胶黏层并粘结上流延聚丙烯薄膜,形成流延聚丙烯层,得到铝塑复合膜。
优选步骤(1’)中,所用铝箔是厚度为30-50μm的铝合金箔。
本发明的铝塑复合膜可作为锂离子电池的外壳用包装材料,具有优异的耐酸腐蚀性能,能够为锂离子电池提供可靠的保护,确保其使用寿命。本发明的铝塑复合膜在90±5%相对湿度、85±2℃环境中浸泡电解液14天后,超疏水铝层与流延聚丙烯层不分层,无损坏,且剥离力维持在8-10N/15mm(通过万能电子拉力机,依照GB/T8808要求测试)。
此外,对铝箔进行超疏水处理所用的盐酸、草酸、硬脂酸等原料价格低廉,对环境和人体较友好;处理方法操作工艺简单,适合工业化规模应用。
附图说明
图1是本发明各优选实施例铝塑复合膜的结构示意图。
具体实施方式
实施例1
本实施例中,铝塑复合膜的制备方法包括下述步骤:
(1’)将铝箔(所用铝箔是厚度为40μm的铝合金箔)浸入温度为25℃的盐酸-草酸混合溶液中,浸泡1min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸7.2克,浓盐酸5克,余量为水;
(2’)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为25℃的高锰酸钾溶液中,浸泡1min;
每升高锰酸钾溶液含有:高锰酸钾15.8克,余量为水;
(3’)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥(在75℃下烘干);
在铝箔表面形成微、纳米相间的多孔结构的颗粒层,该多孔结构颗粒层的孔深约1-2μm,孔径约1μm,孔间距约15-20μm;
(4’)将铝箔浸入质量百分比浓度为0.5%的硬脂酸乙醇溶液中,浸泡5分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥(用60℃热风干燥),在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层;
第一硬脂酸膜层、铝箔层和第二硬脂酸膜层组成超疏水铝箔。经测试,第一硬脂酸膜层、第二硬脂酸膜层与水的接触角均为153±1.8°,水滴滚动角均为9°;第一硬脂酸膜层、第二硬脂酸膜层的厚度均约为5μm;
(5’)在第二硬脂酸膜层的外侧面上形成第二胶黏层并粘结上双轴拉伸聚对苯二甲酸乙二醇酯薄膜(其厚度为20μm),形成外保护层;并在第一硬脂酸膜层的内侧面上形成第一胶黏层并粘结上流延聚丙烯薄膜(采用厚度为60μm的流延聚丙烯薄膜),形成流延聚丙烯层,得到铝塑复合膜。
参考图1,得到的铝塑复合膜自内至外依次包括流延聚丙烯层1、第一胶黏层4、第一硬脂酸膜层6、铝箔层2、第二硬脂酸膜层7、第二胶黏层5和外保护层3。外保护层3为双向拉伸聚对苯二甲酸乙二醇酯层。
实施例2
本实施例中,铝塑复合膜的制备方法包括下述步骤:
(1’)将铝箔(所用铝箔是厚度为30μm的铝合金箔)浸入温度为20℃的盐酸-草酸混合溶液中,浸泡0.8min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸7.2克,浓盐酸20克,余量为水;
(2’)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为20℃的高锰酸钾溶液中,浸泡1.5min;
每升高锰酸钾溶液含有:高锰酸钾31.6克,余量为水;
(3’)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥(在70℃下烘干);
在铝箔表面形成微、纳米相间的多孔结构的颗粒层,该多孔结构颗粒层的孔深约2-5μm,孔径约2μm,孔间距约5-10μm;
(4’)将铝箔浸入质量百分比浓度为1%的硬脂酸乙醇溶液中,浸泡5分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥(用50℃热风干燥),在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层;
第一硬脂酸膜层、铝箔层和第二硬脂酸膜层组成超疏水铝箔。经测试,第一硬脂酸膜层、第二硬脂酸膜层与水的接触角均为166±1.8°,水滴滚动角均为7°;第一硬脂酸膜层、第二硬脂酸膜层的厚度均约为8μm;
(5’)在第二硬脂酸膜层的外侧面上形成第二胶黏层并粘结上双向拉伸聚酰胺薄膜(其厚度为30μm),形成外保护层;并在第一硬脂酸膜层的内侧面上形成第一胶黏层并粘结上流延聚丙烯薄膜(采用厚度为40μm的流延聚丙烯薄膜),形成流延聚丙烯层,得到铝塑复合膜。
参考图1,得到的铝塑复合膜自内至外依次包括流延聚丙烯层1、第一胶黏层4、第一硬脂酸膜层6、铝箔层2、第二硬脂酸膜层7、第二胶黏层5和外保护层3。外保护层3为双向拉伸聚酰胺层。
实施例3
本实施例中,铝塑复合膜的制备方法包括下述步骤:
(1’)将铝箔(所用铝箔是厚度为50μm的铝合金箔)浸入温度为30℃的盐酸-草酸混合溶液中,浸泡0.5min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸20克,浓盐酸100克,余量为水;
(2’)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为30℃的高锰酸钾溶液中,浸泡2min;
每升高锰酸钾溶液含有:高锰酸钾7.9克,余量为水;
(3’)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥(在80℃下烘干);
在铝箔表面形成微、纳米相间的多孔结构的颗粒层(该多孔结构颗粒层的孔深约4-5μm,孔径约1-2μm,孔间距约15-20μm);
(4’)将铝箔浸入质量百分比浓度为0.1%的硬脂酸乙醇溶液中,浸泡10分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥(用70℃热风干燥),在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层;
第一硬脂酸膜层、铝箔层和第二硬脂酸膜层组成超疏水铝箔。经测试,第一硬脂酸膜层、第二硬脂酸膜层与水的接触角均为160±1.8°,水滴滚动角均为8°;第一硬脂酸膜层、第二硬脂酸膜层的厚度均约为7μm;
(5’)在第二硬脂酸膜层的外侧面上形成第二胶黏层并粘结上双轴拉伸聚对苯二甲酸乙二醇酯薄膜(其厚度为10μm),形成外保护层;并在第一硬脂酸膜层的内侧面上形成第一胶黏层并粘结上流延聚丙烯薄膜(采用厚度为100μm的流延聚丙烯薄膜),形成流延聚丙烯层,得到铝塑复合膜。
参考图1,得到的铝塑复合膜自内至外依次包括流延聚丙烯层1、第一胶黏层4、第一硬脂酸膜层6、铝箔层2、第二硬脂酸膜层7、第二胶黏层5和外保护层3。外保护层3为双向拉伸聚对苯二甲酸乙二醇酯层。
对实施例1-3的铝塑复合膜性能进行测试,测试结果如下表1所示。表1:实施例1-3铝塑复合膜性能的测试结果
Claims (5)
1.一种具有优异耐酸腐蚀性能的铝塑复合膜,其特征在于自内至外依次包括流延聚丙烯层、第一胶黏层、第一硬脂酸膜层、铝箔层、第二硬脂酸膜层、第二胶黏层和外保护层,所述外保护层为双向拉伸聚对苯二甲酸乙二醇酯层或双向拉伸聚酰胺层;
在铝箔层的内侧表面、外侧表面上形成第一硬脂酸膜层、第二硬脂酸膜层的方法依次包括下述步骤:
(1)将铝箔浸入温度为20-30℃的盐酸-草酸混合溶液中,浸泡0.5-2min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸5-20克,浓盐酸5-100克,余量为水;
(2)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为20-30℃的高锰酸钾溶液中,浸泡1-2min;
每升高锰酸钾溶液含有:高锰酸钾5-32克,余量为水;
(3)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥;
(4)将铝箔浸入质量百分比浓度为0.1-1%的硬脂酸乙醇溶液中,浸泡1-10分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥,在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层。
2.根据权利要求1所述的铝塑复合膜,其特征在于:步骤(1)中,所用铝箔是厚度为30-50μm的铝合金箔。
3.根据权利要求1或2所述的铝塑复合膜,其特征在于:所述外保护层的厚度为10-30μm,流延聚丙烯层的厚度为30-100μm。
4.权利要求1所述的铝塑复合膜的制备方法,其特征在于包括下述步骤:
(1’)将铝箔浸入温度为20-30℃的盐酸-草酸混合溶液中,浸泡0.5-2min;
每升盐酸-草酸混合溶液由下述比例的原料配制而成:草酸5-20克,浓盐酸5-100克,余量为水;
(2’)将铝箔从盐酸-草酸混合溶液中取出并浸入温度为20-30℃的高锰酸钾溶液中,浸泡1-2min;
每升高锰酸钾溶液含有:高锰酸钾5-32克,余量为水;
(3’)将铝箔从高锰酸钾溶液中取出,用水将铝箔洗净后,再将铝箔干燥;
(4’)将铝箔浸入质量百分比浓度为0.1-1%的硬脂酸乙醇溶液中,浸泡1-10分钟;然后将铝箔从硬脂酸乙醇溶液中取出并干燥,在铝箔的内侧表面、外侧表面上分别形成第一硬脂酸膜层、第二硬脂酸膜层,所述铝箔构成铝塑复合膜的铝箔层;
(5’)在第二硬脂酸膜层的外侧面上形成第二胶黏层并粘结上双轴拉伸聚对苯二甲酸乙二醇酯薄膜或双向拉伸聚酰胺薄膜,形成外保护层;并在第一硬脂酸膜层的内侧面上形成第一胶黏层并粘结上流延聚丙烯薄膜,形成流延聚丙烯层,得到铝塑复合膜。
5.根据权利要求4所述的铝塑复合膜的制备方法,其特征在于:步骤(1’)中,所用铝箔是厚度为30-50μm的铝合金箔。
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