CN115071025B - 干膜的制造方法、辊压装置、干膜以及电化学存储元件 - Google Patents
干膜的制造方法、辊压装置、干膜以及电化学存储元件 Download PDFInfo
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- CN115071025B CN115071025B CN202210381330.4A CN202210381330A CN115071025B CN 115071025 B CN115071025 B CN 115071025B CN 202210381330 A CN202210381330 A CN 202210381330A CN 115071025 B CN115071025 B CN 115071025B
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Abstract
本发明涉及干膜的制造方法、辊压装置、干膜以及电化学存储元件。用于制造干膜(3)的方法中,通过包含第一辊(2a)和第二辊(2b)的辊压装置将干粉混合物加工成所述干膜(3)。所述第一辊(2a)的圆周旋转速度大于所述第二辊(2b)的圆周旋转速度,并且所述干膜(3)被置于所述第一辊(2a)上。
Description
本申请是申请日为2018年5月14日、发明名称为“干膜的制造方法、辊压装置、干膜以及覆有干膜的基板”的申请号为201880032871.8的专利申请的分案申请。
技术领域
本发明涉及基板的制造方法、辊压装置、干膜和覆有干膜的基板。
背景技术
在电池电极的生产中,必须以高卷绕速度将50μm至100μm厚的层施加至金属集电器上。这通常是由活性物质在水性或有机溶剂中的悬浮液通过湿法化学“卷对卷(roll-to-roll)”工序而实现的。为此,对于活性物质的分散以及层的干燥而言,都需要高能量输入。人们越来越致力于实现以无溶剂的(即,因此是干燥的)的方式实现涂覆。为此,必须将活性材料、导电剂和合适的粘合剂(binder)的干粉混合物转换成机械承载层。
现有技术中的一些方法是已知的,其中,如专利文献US 7352558 B2中所公开的那样,实现了自支撑膜(free-standing film)的压制。为此,通常进行如下三阶段工序,其中,通过气流粉碎机(air jet mill)将干粉混合物原纤维化,将粉末输送到压延机辊隙(calender nip)中并且在压延机辊隙中被压制成自支撑膜,并且将自支撑膜施加到集电器上。尽管该方法能够进行连续处理,但是难以处理的自支撑膜的多阶段性质以及(最重要的是)中间步骤是有问题的。
在专利文献DE 10 2010 044 552 B4中公开的另一种方法中,借助于静电充电和用于机械稳定的下游热处理,通过热塑性粘合剂将干粉混合物施加到目标基板上。这种方法的缺点是,在施加粉末之后必须进行密封处理或通过压延进行机械稳定化,因此需要额外的处理步骤。而且,针对该方法,必须使用平面的目标基板。
从专利文献DE 10 2014 208 145 B3中已知一种具有涂覆的电极的电池单元及其制造方法。
一种具有基于干颗粒的可回收电极的电池。
发明内容
因此,本发明的目的是提出一种避免上述缺点的方法,通过该方法能够以有效且机械稳定的方式将干膜施加至基板。
在用于制造干膜的方法中,通过具有第一辊和第二辊的辊压装置将干粉混合物加工成干膜。在这种情况下,第一辊具有比第二辊更高的旋转圆周速度,并且获得的干膜被安置在第一辊上。
通过以两个辊的不同旋转圆周速度操作的辊压装置,实现了机械稳定性和在第一辊上的膜形成,所述第一辊旋转得比第二辊快。因此,避免了自支撑膜的形成,并且能够对支撑在第一辊上的干膜进行进一步的处理。
通常,在两个棍的加工之后,干膜被施加至基板上,优选地,被层压至基板上;然而,可替代地或额外地,这可以在生成干膜的同时完成。如果基板具有足够的粗糙度(例如被设计为金属丝网或碳纤维毡),则由于有效的相互连结,干膜也能够被压至基板上。但是,也可以设置成例如通过刮刀从第一辊分离干膜。由于不同的辊速度(其影响干膜中形成的结构的间距)和压力(其影响这些结构的结构高度),制造的干膜通常具有粗糙度Ra为10μm或更小的原纤维结构。
可以规定,第一辊的旋转圆周速度与第二辊的旋转圆周速度之比在10:9至10:11之间。优选地,保持10:7至10:3的比例,特别优选地保持2:1的比例。结果,在两个辊之间的间隙中的粉末被施加剪切力,这导致沿行进方向产生原纤维化。因此,干膜能够被形成为具有波纹结构,其中,由于不同的辊速度,可以看到结构的周期性。
第一辊的周长通常对应于第二辊的周长,从而获得具有两个相同直径的辊的简单构造。但是也可以例如考虑到相应的圆周来实现限定的转速,因而设计具有不同直径(并且因此具有不同的辊圆周)的第一辊和第二辊。
辊压装置能够被构造为压延辊装置。通过可加热的辊,能够实现干膜的进一步压实。借助于多个可加热的辊或至少一个可加热的辊,能够促进原纤维结构的形成。在聚四氟乙烯(PTFE)粘合剂的情况下,至少一个可加热辊的温度应在80℃至120℃之间。
优选地,具有比第一辊低的旋转圆周速度的第二辊在其表面上具有改性(modification),优选是改性涂层,该改性涂层对形成的干膜具有排斥性和/或降低的粘附性,使得干膜能够更容易地被去除。该涂层可以包含聚四氟乙烯(PTFE)、硅树脂和/或类金刚石碳,或者由它们构成。可替代地或额外地,第一辊可以具有对应的改性,该改性对成形的干膜具有增强粘附性的效果。该改性也可以通过粗糙化的表面来实现,例如,第一辊的表面具有比第二辊更大的粗糙度。特别地,第二辊的表面可以被抛光成光滑的。
通常将干膜施加至(优选地,层压至)基材上,并以与第一辊的旋转圆周速度相对应的速度移动以进行施加或层压。由于相互匹配的速度,这使得能够实现干膜从第一辊到基板的流畅输送。
优选地,在干膜形成在基板上的同时,基板在第一辊上移动。结果,促进了与基板的移动同时发生的干燥层的直接形成。如果基板与涂底剂箔一起被直接馈送经过第一辊,则可以将粘附性增强层施加至基板上。
可以规定,由第一辊和第二辊形成干膜,其中,在辊隙中在第一辊和第二辊之间作用的线性力为100N/cm至10kN/cm,优选为400N/cm,从而实现干膜的充分的机械压实(mechanical compaction)。
通常,基板由金属材料形成或包含该金属材料,以便能够用作用于能量存储单元的电极。
在将干膜层压在为施加或层压而提供的相应的表面上之前,可以为基板提供涂底剂和/或粘合剂。因此,实现了改进的连接。优选地,为此目的使用热塑性涂底剂和/或热塑性粘合剂。可替代地或额外地,也可以使用反应性涂底剂或者黏合剂(adhesive)。涂底剂层可以包含导电炭黑和/或热塑性组分,优选聚乙烯吡咯烷酮(PVP)。优选地,由网眼金属(expanded metal)、金属丝网、无纺布、具有允许机械互锁的结构化表面的基板或金属箔(优选地,铜箔或铝箔)形成基板。特别优选地,使用涂覆有碳涂底剂的铜箔或铝箔。
干膜通常形成为小于500μm,优选小于300μm,特别优选小于150μm的厚度,以获得尽可能薄且机械稳定的干膜。
通常,使用包含或含有聚四氟乙烯、导电剂、多孔碳(例如碳纳米管)、过渡金属氧化物和/或硫的干粉混合物。对于碳/硫阴极,干粉混合物可包括多孔碳(例如,多孔炭黑或碳纳米管)、硫、聚四氟乙烯和可选的其它导电剂。对于锂离子电极,除了聚四氟乙烯和额外的导电剂之外,还可以使用活性材料,优选磷酸铁锂(LFP)、锰酸锂(LMO)、镍锰钴(NMC)、富镍锂镍锰钴氧化物(NMC 622或NMC 811)、锂镍钴铝氧化物(NCA)、锂钴氧化物(LCO)、锂锰镍氧化物(LMNO)和/或钛酸锂(LTO)。说明的方法对于锂离子电池中的阴极材料特别有利,因为它们很少经过水性处理。
在用于实施该方法的辊压装置中,将来自粉末输送机的干粉混合物供给至第一压延辊和第二压延辊之间的辊隙中。第一压延辊和第二压延辊被构造为或被驱动为使得第一压延辊具有比第二压延辊更高的旋转圆周速度,并且第一压延辊和第二压延辊各自具有相反的旋转方向。
除了干粉混合物之外,基板,特别是箔或网也可以被供给通过辊隙。
在一些情况下,例如对于电池应用,可能需要进行所谓的间歇涂覆。这允许以横切于涂覆方向的条带形式的涂覆。为此,以规则的且精确同步的间隔使涂覆暂停,从而形成未涂层的条带。这种同步化和可生产的形状的精确度以及边缘的精度受到限制。因此,与连续涂层相比,干膜以及基板上的涂层的间歇形成的处理速度可能降低一半(~30m/min而不是~60m/min)。
利用根据本发明的方法,可以通过在相应的基板表面上使用粘附性增强涂底剂层来实现这种结构化。为此,必须预先以期望的几何形状用粘附性增强涂底剂层涂覆要在其上形成干膜的基板表面。由于只有(处于干燥状态)约1μm厚的层,因此构建涂底剂层比构建实际的电极层(各种印刷或喷涂处理)更容易。任何几何形状(矩形,也可以是圆形或其它)都是可能的。在这样的方法中(例如,图2),干膜层将被连续地完全形成在更快旋转的第一压延辊上。但是,只有在基板表面设置有涂底剂层的那些位置处干膜才会成层。多余的(未被转送到基板表面的)干膜被从第一压延辊上去除,进行重新处理并重新使用。因此,可以在不降低处理速度的情况下以高精度实现任何几何形状。
也可以将包含第一压延辊和第二压延辊的两对压延辊以镜像对称的方式并排布置,从而在两个第一压延辊之间形成辊隙,通过辊隙将干膜施加至基板的两侧,所述基板也被馈送通过该辊隙,并且两个第一压延辊具有相反的旋转方向。
在另一个实施例中,可以存在绕旋转轴线旋转的另一第一压延辊,在第一压延辊和第二压延辊之间形成的干膜在离开辊隙之后可以被卷绕在所述另一第一压延辊上。两个第一压延辊应具有相同的旋转圆周速度。在该实施例中,可以引导衬底,基板(优选地,箔)通过第一压延辊和第二压延辊之间的辊隙能够被供给有干膜,并缠绕到另一第一压延辊上。
干膜具有各向异性地形成的原纤维。通过辊隙中的剪切,这些原纤维优选在第一辊和第二辊的运行方向上各向异性地形成。原纤维的长度在0.1μm和1000μm之间的范围内。可替代地或额外地,具有原纤维的干膜能够具有小于10μm的粗糙度Ra。通常干膜被布置在基板上。
优选地,电化学存储器或电化学转化器包括具有所述性质的干膜或设置有所述干膜并具有所述性质的基板。
干膜和具有干膜的基板优选根据所述方法制造,因此所述方法用于形成干膜和具有干膜的基材。
为了制备,可以使用不能流动的粉末混合物。这里,可以在根据德国标准EN ISO6186:1998(从1998年8月开始)的测试条件下确定这种不可流动性。
附图说明
附图中示出了本发明的说明性的实施例并且下文中将参考图1至图3对这些实施例进行说明,其中:
图1示出了辊压装置的示意性侧视图;
图2示出了双辊压装置的与图1对应的示图;以及
图3示出了具有基板进给的辊压装置的与图1对应的示图。
具体实施方式
图1图示了辊压装置的示意性侧视图,其中,从粉末输送机1起,存储在粉末输送机1中的干粉混合物在两个相同尺寸的镀铬压延辊2a和2b上通过,并且通过压延辊施加压力和剪切力而转变成稳定的状态。这里,第一压延辊2a以高于第二压延辊2b的旋转速度运作,使得形成的干膜3在挤压和剪切结合操作之后保留在第一压延辊2a上。
在图示的代表性实施例中,使用的干粉处于预混合状态并且包含90重量%的科琴黑/硫(1:2m/m)、3重量%的聚四氟乙烯(PTFE)和7重量%的多壁碳纳米管(MWCNT)。对于锂离子电极,通常使用95重量%的锂锰氧化物,3重量%的导电剂(在此情况下为多壁碳纳米管,MWCNT)和2重量%的PTFE。在位于第一辊2a和第二辊2b之间的压延机辊隙中,干粉混合物发生原纤维化,由此产生封闭的干膜3。
第一辊2a和第二辊2b的旋转速度在10:9至10:4之间的范围内,在所示的说明性实施例中为大约2:1,即10mm/s:5mm/s或20mm/s:10mm/s。然而,在其它的说明性实施例中,取决于参数窗口和粉末条件,也可以将80mm/s:40mm/s用作转速。因此,更高的旋转速度导致具有更不明显的波纹结构或更不明显的原纤维的更薄的干膜,从而具有更低的表面粗糙度Ra。在所示的说明性实施例中,原纤维的平均长度为10μm,并且在辊2a和2b的行进方向上各向异性地形成。由于旋转速度,剪切力被施加至辊隙中的粉末上并沿上述行进方向产生原纤维化,在图示的示例性实施例中的辊隙的宽度为50μm,但其宽度也可以在10μm至300μm之间。这导致机械稳定并且在以更高的速度旋转的第一辊2a上形成膜,并且避免了自支撑膜的形成(但是,在必要时,可以通过机械地(例如借助刮刀)从辊2a上去除而实现)。相反,获得了被支撑在较快的辊2a上的干膜3,由于有限的机械稳定性,这是有利的,特别是对于厚度小于200μm的干膜而言。
在所示的说明性实施例中,第一辊2a和第二辊2b可分别被加热到100℃的温度。此外,第一辊2a能够设置有干膜3粘附于其上的粘附性增强表面,而第二辊2b具有对于干膜的粘附性减小表面。在所示的说明性实施例中,第一辊2a和第二辊2b之间的作用线性力总计为400N。
通过随后层压至设置有热塑性涂底剂或粘合剂的集电器上,能够将干膜3从第一辊2a上移除,因此,例如,能够产生以无溶剂方式生产的电极。
在图2中,在对应于图1的视图中示出了说明性实施例,其中存在由两个图1所示的辊压装置组成的对称结构。此图中的重复特征具有相同的附图标记,在后面的图中也是如此。
在所示的说明性实施例中,基板4被馈送穿过两个辊压装置之间,这两个辊压装置彼此镜像对称地布置。两个第一辊2a彼此相对并且两个干辊3分别在两个第一辊2a上运行,使得基板4的两侧都能够设置有干膜3,这是因为两个表面分别面向一个辊2a。为此,基板4以精确地与两个第一辊2a的旋转圆周速度对应的速度移动。在所示的示意性实施例中,除了镜面对称布置之外,两个辊压装置的构造相同,因此特别地具有相等的尺寸,并且以相同的旋转速度或旋转圆周速度进行操作。虽然在图2所示的说明性实施例中干膜3是相同的,但是在其它的说明性实施例中,也可以将成分彼此不同的干膜3施加至基板4。
此外,所描述的方法还允许制造具有替代的集电器的电极作为基板4,例如具有低基重的穿孔基材,诸如穿孔金属箔或导电织物。在图2所示的说明性实施例中,基板4是具有碳涂底剂作为双面涂层的铝箔。
因此,使得用于一次和二次电池的电池电极的连续薄膜生产成为可能,例如锂离子电池、锂硫电池、钠硫电池、固态电池、超级电容器电极、燃料电池用电极、电解电池用电极、其它电化学元件用电极,以及通过使用多孔颗粒的滤膜或吸附涂层、装饰层、用于吸收的光学层和/或对水分敏感的材料的层或对溶剂敏感的材料的层。
图3示出了本发明的另一说明性实施例的与图1对应的示意性侧视图,其中基板4以箔的形式缠绕在基板辊5上并且以箔的形式被引导至辊隙中,使得形成的干膜3在辊隙中被直接层叠在基板4上。在该说明性实施例中,干膜3不再直接支撑在第一辊2a上,即,不再与第一辊2a直接接触,而是仅间接地在第一辊2a上被引导并被缠绕在另一辊2a上。
因此,说明的方法允许直接从预混合的干膜粉末制备电极,而无需额外的用于原纤维化的步骤,因此无需形成自支撑膜。该方法可以用于预原纤维化,其中,能够增强干膜的机械稳定性。而且,可以通过与承载辊的分离来实现自支撑膜。通过第一辊2a和第二辊2b的圆周速度或旋转圆周速度以及在压延机辊隙或者辊之间的辊隙的方向上作用的挤压力,能够设定载荷和密度。干膜形成是通过自定量方式实现的,获得的层厚度源于两个辊2a和2b的所用的挤压力。通过特定的(根据工艺参数调整的)粉末量的连续输入,例如通过粉末输送机1或进料基板,实现预配料(pre-dosing)。以这种方式,也可以影响层厚度。
干膜3的机械稳定性通过使用的挤压力和旋转速度(剪切率)来调节。与由于辊2a和2b的相同的旋转速度而仅在辊隙中的被挤压的自支撑膜相比,通过本文所提出的方法生产的干膜3具有显著提高的机械稳定性。
仅在说明性实施例中被公开的各个实施例的那些特征可以相互组合并且单独地要求保护。
Claims (28)
1.一种干膜(3)的制造方法,其中,
通过具有第一辊(2a)和第二辊(2b)的辊压装置将干粉混合物加工成所述干膜(3),其中
所述第一辊(2a)具有比所述第二辊(2b)更高的旋转圆周速度,并且所述干膜(3)被安置在所述第一辊(2a)上,
其中,保持所述第一辊(2a)的旋转圆周速度与所述第二辊(2b)的旋转圆周速度的比为10:5至10:1,并且
形成具有各向异性地形成的原纤维的干膜(3)。
2.根据权利要求1所述的方法,其特征在于,保持所述第一辊(2a)的旋转圆周速度与所述第二辊(2b)的旋转圆周速度的比为10:5至10:3。
3.根据权利要求1或2所述的方法,其特征在于,所述辊压装置是压延辊装置。
4.根据权利要求1或2所述的方法,其特征在于,将不能流动的粉末混合物用于干膜制造。
5.根据权利要求1或2所述的方法,其特征在于,所述第一辊(2a)具有粘附性增强改性,并且/或者所述第二辊(2b)具有粘附性减小改性。
6.根据权利要求1或2所述的方法,其特征在于,将所述干膜(3)施加至基板(4)。
7.根据权利要求6所述的方法,其特征在于,为了所述施加,以与所述第一辊(2a)的旋转圆周速度相对应的速度移动所述基板(4)。
8.根据权利要求6所述的方法,其特征在于,在将所述干膜(3)形成在所述基板(4)上的同时使所述基板(4)在所述第一辊(2a)上移动。
9.根据权利要求1或2所述的方法,其特征在于,由所述第一辊(2a)和所述第二辊(2b)通过作用在所述第一辊(2a)和所述第二辊(2b)之间的辊隙中的100N/cm至10kN/cm的线性力形成所述干膜(3)。
10.根据权利要求9所述的方法,其特征在于,由所述第一辊(2a)和所述第二辊(2b)通过作用在所述第一辊(2a)和所述第二辊(2b)之间的辊隙中的400N/cm的线性力形成所述干膜(3)。
11.根据权利要求6所述的方法,其特征在于,使用包含金属材料的所述基板(4)。
12.根据权利要求6所述的方法,其特征在于,在将所述干膜(3)层压在相应的表面上之前,所述基板(4)具有涂底剂以及/或者粘合剂。
13.根据权利要求12所述的方法,其特征在于,所述涂底剂是热塑性的涂底剂以及/或者所述粘合剂是热塑性的粘合剂。
14.根据权利要求6所述的方法,其特征在于,使用包含施加有碳涂底剂的网眼金属、金属丝网、无纺布、铜箔或者铝箔的所述基板(4)。
15.根据权利要求1或2所述的方法,其特征在于,所述干膜(3)的厚度被形成为小于500μm。
16.根据权利要求15所述的方法,其特征在于,所述干膜(3)的厚度被形成为小于300μm。
17.根据权利要求15所述的方法,其特征在于,所述干膜(3)的厚度被形成为小于150μm。
18.根据权利要求1或2所述的方法,其特征在于,使用包含聚四氟乙烯、导电剂、多孔碳、过渡金属氧化物和/或硫的干粉混合物。
19.根据权利要求1或2所述的方法,其特征在于,借助于在相应的基板表面区域上的粘附性增强涂底剂层,实现所述干膜(3)的结构的形成。
20.根据权利要求19所述的方法,其特征在于,所述结构为条纹的形式或矩形形状。
21.根据权利要求20所述的方法,其特征在于,条纹的形式或矩形形状的所述结构在涂覆方向上。
22.用于实施如前述权利要求中任一项所述的方法的辊压装置,其特征在于,干粉混合物被导入至第一压延辊(2a)与第二压延辊(2b)之间的辊隙中,并且所述第一压延辊和所述第二压延辊(2a和2b)被构造为或被驱动为使得所述第一压延辊(2a)具有比所述第二压延辊(2b)更高的旋转圆周速度,并且所述第一压延辊和所述第二压延辊(2a和2b)分别具有相反的旋转方向,
其中,所述辊压装置被构造成
保持所述第一辊(2a)的旋转圆周速度与所述第二辊(2b)的旋转圆周速度的比为10:5至10:1,并且
形成具有各向异性地形成的原纤维的干膜(3)。
23.根据权利要求22所述的辊压装置,其特征在于,除了所述干粉混合物之外,基板(4)也被馈送经过所述辊隙。
24.根据权利要求22所述的辊压装置,其特征在于,均包含所述第一压延辊和所述第二压延辊(2a和2b)的两对压延辊以镜像对称的方式并排布置,从而在两个第一压延辊(2a)之间形成辊隙,通过该辊隙将干膜(3)施加在基板(4)的两侧,所述基板(4)也被馈送通过该辊隙,并且所述两个第一压延辊(2a)具有相反的旋转方向。
25.根据权利要求22所述的辊压装置,其特征在于,存在绕旋转轴线旋转的另一第一压延辊(2a),在所述第一压延辊(2a)和所述第二压延辊(2b)之间形成的干膜在离开所述辊隙之后能够被卷绕在所述另一第一压延辊上,并且所述第一压延辊(2a)和所述另一第一压延辊(2a)具有相同的旋转圆周速度。
26.采用如权利要求1至21中任一项所述的方法制造的干膜,其特征在于,所述干膜的原纤维的长度为0.1μm至1000μm。
27.根据权利要求26所述的干膜,其特征在于,所述干膜(3)被施加至基板(4)。
28.具有如权利要求26或27所述的干膜的电化学存储元件或电化学转化器。
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EP4119323A1 (de) | 2023-01-18 |
ES2963957T3 (es) | 2024-04-03 |
US11990599B2 (en) | 2024-05-21 |
CN110869179A (zh) | 2020-03-06 |
KR20200020702A (ko) | 2020-02-26 |
JP7248835B2 (ja) | 2023-03-29 |
JP2022062188A (ja) | 2022-04-19 |
EP3625018C0 (de) | 2023-08-30 |
RS64947B1 (sr) | 2024-01-31 |
EP3625018B1 (de) | 2023-08-30 |
CN110869179B (zh) | 2022-04-29 |
JP2023103999A (ja) | 2023-07-27 |
KR102597499B1 (ko) | 2023-11-06 |
DE102017208220A1 (de) | 2018-11-22 |
HUE064505T2 (hu) | 2024-03-28 |
CN115071025A (zh) | 2022-09-20 |
JP2020522090A (ja) | 2020-07-27 |
WO2018210723A1 (de) | 2018-11-22 |
EP3625018A1 (de) | 2020-03-25 |
PL3625018T3 (pl) | 2024-02-26 |
KR20220098052A (ko) | 2022-07-08 |
KR102416449B1 (ko) | 2022-07-04 |
US20210320288A1 (en) | 2021-10-14 |
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