CN102834955A - 用于电化学储存的复合材料 - Google Patents
用于电化学储存的复合材料 Download PDFInfo
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Abstract
提供了复合材料和形成复合材料的方法。本文描述的复合材料能用作电池的电极材料。在某些实施方案中,复合材料包含大于0%重量比且小于约90%重量比的硅颗粒,以及大于0%重量比且小于约90%重量比的一种或多种类型的碳相。一种或多种类型的碳相中的至少一种能为基本上连续的相。形成复合材料的方法包括提供包含前体和硅颗粒的混合物,并热解前体以将前体转化为一种或多种类型的碳相从而形成复合材料。
Description
相关申请的交叉引用
本申请要求2010年1月18日提交的第61/295,993号美国临时申请和2010年3月19日提交的第61/315,845号美国临时申请的权益,通过引用方式将其整体内容并入本文。
背景
发明领域
本发明涉及包含硅和碳的复合材料。具体地,本发明涉及用于电池电极的复合材料。
相关技术描述
锂离子电池通常包含隔板和/或位于阳极和阴极之间的电解质。在一种类型的电池中,将隔板、阴极和阳极材料单独地形成片或膜。随后,将阴极片、隔板片和阳极片与分隔阴极和阳极(例如,电极)的隔板相继地堆叠或轧制以形成电池。对于待轧制的阴极、隔板和阳极,各个片必须足够可变形或有弹性以被轧制而不损坏,例如裂纹、破碎、机械损坏等。典型的电极包括导电金属(例如,铝和铜)上的电化学活性材料层。膜能被轧制或切割为片,然后将这些片分层堆积为堆。所述堆具有与在它们之间的隔板交替的电化学活性材料。
发明概述
在某些实施方案中,提供了复合材料。复合材料能包含大于0%重量比且小于约90%重量比的硅颗粒和大于0%重量比且小于约90%重量比的一种或多种类型的碳相(carbon phase)。此外,一种或多种类型的碳相中的至少一种为基本上连续的相。
硅颗粒可具有小于约1μm的平均最大尺寸。在一些实施方案中,硅颗粒包含复合材料的约20%重量比至约80%重量比。
为基本上连续的相的一种或多种类型的碳相中的至少一种能为电化学活性的和导电性的。在一些实施方案中,为基本上连续的相的一种或多种类型的碳相中的至少一种包含硬碳。
复合材料还可包含其它颗粒。例如,一种或多种类型的碳相能包含石墨颗粒。复合材料可包含导电颗粒、金属颗粒等。
复合材料能基本上为电化学活性的。此外,复合材料可为自支撑的。在某些实施方案中,提供了包含本文描述的复合材料的电池电极。
在某些实施方案中,提供了使用本文描述的复合材料的方法。所述方法包括仅在重量容量小于所述复合材料的约70%的最大重量容量下使用所述复合材料。
在某些实施方案中,提供了形成复合材料的方法。所述方法包括提供包含前体和硅颗粒的混合物,并热解所述前体以将所述前体转化为一种或多种类型的碳相从而形成该复合材料。
在热解所述前体后,混合物可形成自支撑的复合结构。一种或多种类型的碳相中的至少一种能为基本上连续的相。为基本上连续的相的一种或多种类型的碳相中的至少一种包含硬碳。在一些实施方案中,硅颗粒包含复合材料的约20%重量比至约80%重量比。在其它实施方案中,在所述混合物中硅颗粒包括大于0%重量比且小于约80%重量比,并且在所述混合物中所述前体包括约5%重量比且小于约80%重量比。
混合物还可包括溶剂。所述前体能包括烃化合物、聚酰亚胺、酚醛树脂等。所述方法还能包括在基板上浇铸所述混合物,干燥所述混合物以形成膜,从基板上除去所述膜,以及在热压机中固化所述膜。所述方法还可包括由所述复合材料形成电池电极。
附图简述
图1例示了形成复合材料的方法的实施方案,其包括形成包含前体的混合物,浇铸所述混合物,干燥所述混合物,固化所述混合物以及热解所述前体;
图2是平均速率为C/2.6的放电容量图;
图3是平均速率为C/3的放电容量图;
图4是平均速率为C/3.3的放电容量图;
图5是平均速率为C/5的放电容量图;
图6是平均速率为C/9的放电容量图;
图7是放电容量图;
图8是平均速率为C/9的放电容量图;
图9A和9B是对于20wt.%Si的固定百分比,作为来自2611c的PI衍生的碳和石墨颗粒的各个重量百分比的函数的可逆容量和不可逆容量的绘图;
图10是作为碳的重量百分比的函数的第一循环放电容量的绘图;
图11是作为热解温度的函数的可逆(放电)和不可逆容量的绘图;
图12是4.3cm×4.3cm的不含金属箔支撑层的复合阳极膜的照片;
图13是进行循环之前的复合阳极膜的扫描电子显微镜(SEM)显微照片(焦点未对准的部分是阳极的底部部分以及焦点对准的部分是复合膜的裂开的边缘);
图14是进行循环之前的复合阳极膜的另一SEM显微照片;
图15是被循环10次循环后的复合阳极膜的SEM显微照片;
图16是被循环10次循环后的复合阳极膜的另一SEM显微照片;
图17是被循环300次循环后的复合阳极膜的SEM显微照片;以及
图18包括复合阳极膜横截面的SEM显微照片。
详细描述
典型的碳阳极电极包括集电器,例如铜片。将碳连同惰性粘合材料一起沉积在集电器上。常使用碳,因为其具有优异的电化学性质并且还是导电的。如果除去集电器层(例如,铜层),则碳不能自我机械支撑。因此,常规电极需要诸如集电器等支撑结构以能够用作电极。本申请描述的电极(例如,阳极或阴极)组合物能产生自支撑的电极。消除或最小化对金属箔集电器的需要,因为导电的碳化聚合物用于阳极结构中的电流收集以及用于机械支撑。与一类常规的锂离子电池电极中悬浮于非导电性粘合剂的微粒碳相反,碳化聚合物能在整个电极中形成基本上连续的导电碳相。使用碳化聚合物的碳复合混合物的优点包括例如,1)较高的容量,2)增强的过充电/放电保护,3)归因于消除(或最小化)金属箔集电器的较低的不可逆容量,以及4)归因于制造简单的潜在成本节约。
目前用于可再充电锂离子电池的阳极电极通常具有约200毫安小时每克的比容量(包括金属箔集电器、导电添加剂和粘合材料)。石墨,即用于大多数锂离子电池阳极的活性材料,具有372毫安小时每克(mAh/g)的理论能量密度。相比之下,硅具有4200mAh/g的高理论容量。然而,锂插入时,硅膨胀超过300%。由于该膨胀,包含硅的阳极应能因为硅而膨胀以保持与硅的电接触。
本申请还描述了使用碳化聚合物制造单片的、自支撑阳极的新方法。由于将聚合物转化为导电的电化学活性基质,因此产生的电极为足够导电的而能省略或最小化金属箔或网状集电器。转化的聚合物还充当循环过程中硅颗粒的膨胀缓冲以使得能实现高的循环寿命。在某些实施方案中,所产生的电极为基本上由活性材料组成的电极。在其它实施方案中,所产生的电极基本上为活性材料。电极能具有约500mAh/g至约1200mAh/g的高能量密度,其可能原因在于例如,1)使用硅,2)消除或显著减少金属集电器以及3)完全(或几乎完全)由活性材料组成。
本文描述的复合材料能用作大多数常规锂离子电池中的阳极;它们还能在一些电化学电偶(electrochemical couples)中与其它添加剂一起用作阴极。复合材料还能用于二次电池(例如,可再充电的)或原电池(例如,不可再充电的)。在某些实施方案中,复合材料为自支撑的结构。在其它实施方案中,复合材料为自支撑的单片结构。例如,在由复合材料组成的电极中可能不包含集电器。在某些实施方案中,复合材料能用于形成第12/838,368号美国专利申请中讨论的碳结构,发明名称为“Carbon Electrode Structures for Batteries(电池的碳电极结构)”,其整体内容通过引用方式并入本文。此外,本文描述的复合材料能为例如,硅复合材料、碳复合材料和/或硅-碳复合材料。
图1例示了形成复合材料100的方法的一个实施方案。例如,形成复合材料的方法包括形成包含前体的混合物,模块101。所述方法还能包括热解所述前体以将所述前体转化为碳相。所述前体混合物可包含碳添加剂,例如石墨活性材料、短切的或磨碎的碳纤维、碳纳米纤维、碳纳米管和/或其它碳。在将所述前体热解后,所产生的碳材料能为自支撑的单片结构。在某些实施方案中,将一种或多种材料加入至混合物以形成复合材料。例如,能将硅颗粒加入至混合物。碳化的前体产生使复合材料保持在一起的电化学活性结构。例如,碳化的前体能为基本上连续的相。硅颗粒可遍及复合材料中分布。有利地,碳化的前体为结构材料以及电化学活性和导电性材料。在某些实施方案中,加入至混合物的材料颗粒遍及复合材料中均匀分布以形成均匀的复合物。
混合物能包含多种不同的组分。混合物能包含一种或多种前体。在某些实施方案中,所述前体为烃化合物。例如,所述前体能包括聚酰胺酸、聚酰亚胺等。其它前体包括酚醛树脂、环氧树脂和其它聚合物。混合物还能包含溶剂。例如,溶剂能为N-甲基-吡咯烷酮(NMP)。其它可能的溶剂包括丙酮、乙醚、γ-丁内酯、异丙醇、碳酸二甲酯、碳酸乙酯、二甲氧基乙烷等。前体和溶剂溶液的实例包括PI-2611(HDMicrosystems)、PI-5878G(HD Microsystems)和VTEC PI-1388(RBI,Inc.)。PI-2611由>60%的n-甲基-2-吡咯烷酮和10%-30%的s-联苯二酐/对苯二胺组成。PI-5878G由>60%的n-甲基吡咯烷酮、10%-30%的均苯四甲酸二酐/二氨基二苯醚的聚酰胺酸、包含5%-10%的1,2,4-三甲苯的10%-30%的芳香烃(石油馏分)组成。在某些实施方案中,溶剂中前体的量为约10wt.%至约30wt.%。混合物中还能包含附加材料。例如,如前面所述,能将硅颗粒或包括石墨活性材料、短切的或磨碎的碳纤维、碳纳米纤维、碳纳米管和其它导电碳在内的碳颗粒加入至混合物。此外,能将混合物混合以使混合物均匀。
在某些实施方案中,将混合物浇铸在基板上,图1中的模块102。在一些实施方案中,浇铸包括使用间隙挤出(gap extrusion)或刮片浇铸技术。所述刮片浇铸技术能包括通过使用被控制在基板上方一定距离的平面(例如,刮片)将涂层涂覆于基板。能将液体或浆液涂覆于基板,并使刮片在液体上通过以将该液体在基板上面铺展开。通过刮片和基板之间的间隙控制涂层的厚度,因为液体经过该间隙。当液体经过所述间隙时,还能刮除过量的液体。例如,能在聚合物片、聚合物卷或者由玻璃或金属制成的箔或卷上浇铸混合物。然后,将混合物干燥以去除溶剂,模块103。例如,在约110℃下将聚酰胺酸和NMP溶液干燥约2小时以去除NMP溶液。然后从基板上去除干燥的混合物。例如,能使用HCl蚀刻掉铝基板。或者,通过剥离从基板上去除干燥的混合物或从基板上机械地去除干燥的混合物。在某些实施方案中,干燥的混合物为膜或片。在一些实施方案中,将干燥的混合物固化,模块104。能使用热压机以固化并使干燥的混合物保持平整。例如,能在约200℃下将源自聚酰胺酸和NMP溶液的干燥的混合物热压约8小时至16小时。或者,使用标准的膜处理设备以卷对卷制程的形式实施包括浇铸和干燥在内的整个过程。能将干燥的混合物漂洗以去除任何溶剂或可能残留的蚀刻剂。例如,能使用去离子(DI)水漂洗干燥的混合物。在某些实施方案中,能将流延浇铸技术用于浇铸。在其它实施方案中,没有用于浇铸的基板并且不需要从任何基板上去除阳极膜。可将干燥的混合物切割或机械切片为较小的片。
混合物还经历热解以将所述前体转化为碳,模块105。在某些实施方案中,在还原气氛中将混合物热解。例如,能使用惰性气氛、真空和/或流动的氩气、氮气或氦气。在一些实施方案中,将混合物加热至约900℃至约1350℃。例如,在约1175℃下将由聚酰胺酸形成的聚酰亚胺碳化约1小时。在某些实施方案中,混合物的加热速率和/或冷却速率为约10℃/min。可使用支撑物以使混合物保持特定的几何形状。支撑物能为石墨、金属等。在某些实施方案中,将混合物保持平整。在将混合物热解后,能将标签(tabs)与热解的材料连接以形成电接触。例如,镍、铜或其合金能用于所述标签(tabs)。
在某些实施方案中,一种或多种本文描述的方法为连续过程。例如,能以连续过程的形式进行浇铸、干燥、固化和热解;例如,能将混合物涂覆在玻璃或金属圆柱体上。干燥混合物同时旋转圆柱体产生膜。能以卷的形式将膜转移或将其剥离并送入至另一个机器进行进一步加工。在热解步骤之前还能使用工业上已知的挤出和其它膜制造技术。
所述前体的热解产生碳材料(例如,至少一种碳相)。在某些实施方案中,碳材料为硬碳。在一些实施方案中,所述前体为能被热解以形成硬碳的任何材料。除碳化前体以外,当混合物还包含的一种或多种另外的材料或相时,能产生复合材料。特别地,混合物能包含产生硅-碳复合材料(例如,至少一种第一相包含硅和至少一种第二相包含碳)或硅-碳-碳复合材料(例如,至少一种第一相包含硅、至少一种第二相包含碳,和至少一种第三相包含碳)的硅颗粒。硅颗粒能增加复合材料的具体的锂嵌入容量。当硅吸收锂离子时,其经历大约300+体积百分比的大体积增加,这能导致电极结构完整性问题。除体积膨胀相关的问题之外,硅还不是固有导电的,但当将其与锂形成合金时(例如,锂化)则变为导电的。当硅脱锂时,硅的表面失去导电性。此外,当硅脱锂时,体积减小,这导致硅颗粒可能失去与基质的接触。体积的显著变化还导致硅颗粒结构的机械破坏,进而,导致其粉碎。粉碎和失去电接触使得在锂离子电池中使用硅作为活性材料成为挑战。降低硅颗粒的初始大小能阻止硅粉末的进一步粉碎以及最小化表面导电性的损失。此外,将能随硅颗粒的体积变化而弹性变形的材料加入至复合物中,能确保不损失与硅表面的电接触。例如,复合材料能包含诸如石墨的碳,石墨有助于复合材料吸收膨胀的能力并且还能够插入增加电极的储存容量(例如,化学活性)的锂离子。因此,复合材料可包含一种或多种类型的碳相。
硅颗粒最大尺寸的实施方案包括小于约40μm、小于约1μm、约10nm至40μm、约10nm至1μm、小于约500nm、小于约100nm和约100nm。全部、基本上全部或至少一部分的硅颗粒可包括上述最大尺寸。例如,硅颗粒的平均或中值的最大尺寸包括小于约40μm、小于约1μm、约10nm至40μm、约10nm至1μm、小于约500nm、小于约100nm和约100nm。以混合物和复合材料的重量计算,复合材料中硅的量能大于0百分比。在某些实施方案中,以混合物的重量计算,混合物中硅的量大于0%且小于约90%、或为约30%至约80%。复合材料中硅的量的实施方案包括大于0%重量比且小于约35%重量比、大于0%重量比且小于约25%重量比、约10%重量比至约35%重量比和约20%重量比。在其它某些实施方案中,混合物中硅的量为至少约30%重量比。复合材料中硅的量的另外实施方案包括大于约50%重量比、约30%重量比至约80%重量比、约50%重量比至约70%重量比和约60%重量比至约80%重量比。此外,硅颗粒可以是纯硅或可以不是纯硅。例如,硅颗粒可基本上是硅或可以是硅合金。在一个实施方案中,硅合金包含作为主要组分的硅以及一种或多种其它元素。
从所述前体中获得的碳的量能为来自聚酰胺酸的约50重量百分比。在某些实施方案中,复合材料中源自所述前体的碳的量为约10%重量比至25%重量比。源自所述前体的碳能为硬碳。硬碳为即使在超过2800摄氏度下加热仍不转化为石墨的碳。在热解过程中熔化或流动的前体随着足够的温度和/或压力转化为软碳和/或石墨。可选择硬碳,因为软碳前体可流动且软碳和石墨机械上比硬碳脆弱。其它可能的硬碳前体包括酚醛树脂、环氧树脂和具有非常高的熔点或是交联的其它聚合物。复合材料中硬碳的量的实施方案包括约10%重量比至约25%重量比、约20%重量比和大于约50%重量比。在某些实施方案中,硬碳相基本上为无定形的。在其它实施方案中,硬碳相基本上为结晶的。在其它实施方案中,硬碳相包括无定形碳和结晶碳。硬碳相能为复合材料中的基质相。还能将硬碳嵌入包含硅的添加剂的孔中。硬碳可与一些添加剂反应以在界面处产生一些材料。例如,在硅颗粒和硬碳之间可能有碳化硅层。
在某些实施方案中,将石墨颗粒加入至混合物。有利地,石墨为电池中的电化学活性材料以及是能响应硅颗粒体积变化的弹性可变形材料。对于目前市场上一些种类的锂离子电池而言,石墨是优选的活性阳极材料,因为其具有低的不可逆容量。此外,石墨比硬碳软并能更好地吸收硅添加剂的体积膨胀。在某些实施方案中,石墨颗粒的最大尺寸为约0.5微米至约20微米。全部,基本上全部或至少一部分的石墨颗粒可包括本文描述的最大尺寸。在其它实施方案中,石墨颗粒的平均的或中值的最大尺寸为约0.5微米至约20微米。在某些实施方案中,混合物包含大于0%重量比且小于约80%重量比的石墨颗粒。在其它实施方案中,复合材料包含约40%重量比至约75%重量比的石墨颗粒。
在某些实施方案中,将还可为电化学活性的导电颗粒加入至混合物。这种颗粒提供更导电的复合物以及能够吸收在锂化和脱锂过程中发生的大的体积变化的更机械可变形的复合物。在某些实施方案中,导电颗粒的最大尺寸为约10纳米至约7毫米。全部,基本上全部或至少一部分的导电颗粒可包括本文描述的最大尺寸。在其它实施方案中,导电颗粒的平均或中值的最大尺寸为约10nm至约7毫米。在某些实施方案中,混合物包含大于0至高达约80%重量比的导电颗粒。在其它实施方案中,复合材料包含约45%重量比至约80%重量比的导电颗粒。导电颗粒能为导电碳,其包括碳黑、碳纤维、碳纳米纤维、碳纳米管等。被看作非电化学活性的导电添加剂的许多碳一旦在聚合物基质中被热解就变为活性的。或者,导电颗粒能为金属或包括铜、镍或不锈钢在内的合金。
在某些实施方案中,电极能包含本文描述的复合材料。例如,复合材料能形成自支撑的单片电极。复合材料的热解的碳相(例如,硬碳相)能保持在一起并结构上支撑加入至混合物的颗粒。在某些实施方案中,自支撑的单片电极不包含单独的集电器层和/或其它支撑结构。在一些实施方案中,复合材料和/或电极不包含超过在热解所述前体后残留的痕量的聚合物。在其它实施方案中,复合材料和/或电极不包含非导电的粘合剂。复合材料还可包括孔隙率。例如,以体积孔隙度计,孔隙率能为约5%至约40%。
还能将复合材料制成粉末。例如,能将复合材料研磨成粉末。能将复合材料粉末用作电极的活性材料。例如,能以与工业上已知的制造常规电极结构相似的方式将复合材料粉末沉积在集电器上。
在某些实施方案中,电池或电化学电池中的电极能包含本文描述的复合材料。例如,复合材料能用于阳极和/或阴极。在某些实施方案中,电池为锂离子电池。在其它实施方案中,电池为二次电池,或者在其它实施方案中,电池为原电池。
此外,在使用电池的过程中,可能不使用复合材料的全容量以提高电池寿命(例如,在电池失效或电池的性能降低至低于可用性水平之前的充电和放电循环数量)。例如,具有约70%重量比的硅颗粒、约20%重量比的源自前体的碳和约10%重量比的石墨的复合材料可能具有约2000mAh/g的最大重量容量,然而复合材料可能仅被使用高达约550mAh/g至约850mAh/g的重量容量。尽管可能未使用复合材料的最大重量容量,但在较低容量下使用复合材料仍能达到比某些锂离子电池更高的容量。在某些实施方案中,在重量容量低于复合材料的约70%最大重量容量下使用复合材料或只在该范围下使用复合材料。例如,不在重量容量高于复合材料的约70%最大重量容量下使用复合材料。在其它实施方案中,在重量容量低于复合材料的约50%最大重量容量或低于复合材料的约30%最大重量容量下使用复合材料或只在上述范围下使用复合材料。
实施例
下列用于阳极制造的实施例方法通常包括将组分混合在一起,将那些组分浇铸在可除去的基板上,干燥、固化、除去基板,然后热解所产生的样品。通常,将N-甲基-2-吡咯烷酮(NMP)用作溶剂以改变任何混合物的粘度并使其可使用刮刀法(doctor blade approach)浇铸。
实施例1
在实施例1中,使用Spex 8000D机器,将重量比为200:55:5:20的聚酰亚胺液态前体(来自HD Microsystems corp.的PI 2611)、石墨颗粒(来自Timcal corp.的SLP30)、导电碳颗粒(来自Timcal corp.的SuperP)和硅颗粒(来自Alfa Aesar corp.)混合在一起,时间为5分钟。然后,将混合物浇铸在铝箔上并使其在90℃的烘箱中干燥以驱除溶剂,例如,NMP。这随后是在可忽略的压力下,在热压机中在200℃下的固化步骤,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气流下在1175℃下热解约1小时。以重量计,所述方法产生15.8%的PI 2611衍生的碳、57.9%的石墨颗粒、5.3%的来源于Super P的碳和21.1%的硅的组合物。
然后,相对锂NMC氧化物阴极,在袋装电池(pouch cell)配置中测试所产生的电极。典型循环图在图2中示出。
实施例2
在实施例2中,使用Turbula混合器将1:9重量比的硅颗粒(来自EVNANO Advanced Chemical Materials Co.,Ltd.)与NMP首先混合1小时。然后,以200:55:5:200的重量比将聚酰亚胺液态前体(来自HDMicrosystems corp.的PI 2611)、石墨颗粒(来自Timcal corp.的SLP30)和碳纳米纤维(来自Pyrograf corp.的CNF)加入至Si:NMP混合物中并涡旋约2分钟。然后,将混合物浇铸在覆盖有21μm厚的铜网的铝箔上。然后,使样品在90℃的烘箱中干燥以驱除溶剂,例如,NMP。这随后是在可忽略的压力下,在热压机中在200℃下的固化步骤,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气下在1000℃下热解约1小时。以重量计,所述方法产生15.8%的PI 2611衍生的碳、57.9%的石墨颗粒、5.3%的CNF和21.1%的硅的组合物。
然后,相对锂NMC氧化物阴极,在袋装电池配置中测试所产生的电极。典型循环图在图3中示出。
实施例3
在实施例3中,使用Turbula混合器将重量比为40:1的聚酰亚胺液态前体(来自HD Microsystems corp.的PI 2611)和325目的硅颗粒(来自Alfa Aesar corp.)混合在一起,时间为1小时。然后,将混合物浇铸在铝箔上并使其在90℃的烘箱中干燥以驱除溶剂,例如,NMP。这随后是在可忽略的压力下,在热压机中在200℃下的固化步骤,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气流下在1175℃下热解约1小时。以重量计,所述方法产生75%的PI 2611衍生的碳和25%的硅的组合物。
然后,相对锂NMC氧化物阴极,在袋装电池配置中测试所产生的电极。典型循环图在图4中示出。
实施例4
在实施例4中,使用涡旋仪,将重量比为20:200:30:8:4:2:1:15的硅微粒(来自Alfa Aesar corp.)、聚酰亚胺液态前体(来自HDMicrosystems corp.的PI 2611)、石墨颗粒(来自Timcal corp.的SLP30)、磨碎的碳纤维(来自Fibre Glast Developments corp.)、碳纳米纤维(来自Pyrograf corp.的CNF)、碳纳米管(来自CNANO Technology Limited)、导电碳颗粒(来自Timcal corp.的Super P)、导电石墨颗粒(来自Timcacorp.的KS6)混合5分钟。然后,将混合物浇铸在铝箔上。然后使样品在90℃的烘箱中干燥以驱除溶剂,例如,NMP。这随后是在可忽略的压力下,在热压机中在200℃下的固化步骤,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气下在1175℃下热解约1小时。所述方法产生与初始混合物相似的组合物但具有为7.5%的聚酰亚胺前体初始重量的PI 2611衍生的碳部分。
然后,相对锂NMC氧化物阴极,在袋装电池配置中测试所产生的电极。典型循环图在图5中示出。
实施例5
在实施例5中,使用Turbula混合器,将重量比为4:1的聚酰亚胺液态前体(来自HD Microsystems corp.的PI 2611)和硅微粒(来自AlfaAesar corp.)混合在一起,时间为1小时。然后,将混合物浇铸在覆盖有碳遮盖物(carbon veil)(来自Fibre Glast Developments Corporation)的铝箔上并使其在90℃的烘箱中干燥以驱除溶剂,例如,NMP。这随后是在可忽略的压力下,在热压机中在200℃下的固化步骤,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气流下在1175℃下热解约1小时。以重量计,所述方法产生约23%的PI 2611衍生的碳、76%的硅的组合物,并且遮盖物的重量为可忽略的。
然后,相对锂镍锰钴氧化物(NMC)阴极,在袋装电池配置中所测试产生的电极。典型循环图在图6中示出。
实施例6
在实施例6中,使用Spex 8000D机器将重量比为200:10:70的聚酰亚胺液态前体(来自HD Microsystems corp.的PI 2611)、石墨颗粒(来自Timcal corp.的SLP30)和硅微粒(来自Alfa Aesar corp.)混合在一起,时间为5分钟。然后,将混合物浇铸在铝箔上并使其在90℃的烘箱中干燥以驱除溶剂(例如,NMP)。在可忽略的压力下,在热压机中,在200℃下固化干燥的混合物,时间为至少12小时。然后,通过在12.5%的HCl溶液中蚀刻去除铝箔衬垫(backing)。然后,在DI水中漂洗剩余的膜、干燥,然后在氩气流下在1175℃下热解约1小时。以重量计,所述方法产生15.8%的PI 2611衍生的碳、10.5%的石墨颗粒、73.7%的硅的组合物。
然后,相对锂NMC氧化物阴极,在袋装电池配置中测试所产生的电极。各个循环中阳极被充电至600mAh/g并记录每一循环的放电容量。典型循环图在图7中示出。
实施例7
在实施例7中,将重量比为5:20:1:4:70:95的PVDF和硅颗粒(来自EVNANO Advanced Chemical Materials Co)、导电碳颗粒(来自Timcal corp.的Super P)、导电石墨颗粒(来自Timcal corp.的KS6)、石墨颗粒(来自Timcal corp.的SLP30)和NMP混合。然后,将混合物浇铸在铜基板上,然后放置于90℃的烘箱中以驱除溶剂,例如,NMP。然后,相对锂NMC氧化物阴极,在袋装电池配置中测试所产生的电极。典型循环图在图8中示出。
实施例8
进行多个实验以获得改变聚酰亚胺衍生的碳(例如,2611c)的百分比同时降低石墨颗粒(来自Timcal corp.的SLP30)的百分比并保持硅微粒(来自Alfa Aesar corp.)的百分比为20wt.%的影响。
如图9A和9B所示,结果显示通过提高比容量同时降低不可逆容量,较多的石墨和较少的2611c对电池性能有利。最小化2611c不利地影响所产生的阳极的强度,因此作为一个实施方案的折衷,接近20wt.%的值能为优选的。
实施例9
与实施例8相似,如果保持2611c为20wt.%并且以石墨颗粒为代价而增加Si百分比,则所产生的电极的第一循环放电容量增加。图10显示更高的硅含量能制造性能更好的阳极。
实施例10
根据实施例1中的步骤,热解并测试1密耳厚的聚酰亚胺片。以热解温度函数的形式绘制可逆容量和不可逆容量的图。图11表明在一个实施方案中,优选在约1175℃下热解聚酰亚胺片(UBE corp的Upilex)。
附加实施例
图12为4.3cm×4.3cm的不含金属箔支撑层的复合阳极膜的照片。复合阳极膜具有约30微米的厚度并具有以重量计约15.8%的PI2611衍生的碳、约10.5%的石墨颗粒和约73.7%的硅的组合物。
图13-18为复合阳极膜的扫描电子显微镜(SEM)显微照片。复合阳极膜的组合物为以重量计约15.8%的PI 2611衍生的碳、约10.5%的石墨颗粒和约73.7%的硅。图13和14显示在进行循环前(焦点未对准的部分为阳极的底部部分且焦点对准的部分为复合膜的裂开的边缘)。图15、16和17分别为在被循环10次循环、10次循环和300次循环后复合阳极膜的SEM显微照片。SEM显微照片显示硅没有任何显著的粉碎并且阳极在循环后不具有在其上部建立的固体电解质界面/相间(SEI)的过度层。图18为复合阳极膜横截面的SEM显微照片。
上文描述了各个实施方案。尽管参照这些具体的实施方案描述了本发明,但该描述仅意图为示例性的并且不意图为限制性的。在不违背所附加的权利要求中定义的本发明的真实实质和范围的前提下本领域技术人员可以想到各种修改和应用。
Claims (24)
1.复合材料,其包含:
大于0%重量比且小于约90%重量比的硅颗粒;
大于0%重量比且小于约90%重量比的一种或多种类型的碳相,其中所述一种或多种类型的碳相中的至少一种为基本上连续的相。
2.如权利要求1所述的复合材料,其中所述硅颗粒具有小于约1μm的平均最大尺寸。
3.如权利要求1或2所述的复合材料,其中所述硅颗粒包含所述复合材料的约20%重量比至约80%重量比。
4.如权利要求1-3中任一权利要求所述的复合材料,其中为基本上连续的相的所述一种或多种类型的碳相中的至少一种为电化学活性的和导电性的。
5.如权利要求1-4中任一权利要求所述的复合材料,其中为基本上连续的相的所述一种或多种类型的碳相中的至少一种包含硬碳。
6.如权利要求1-5中任一权利要求所述的复合材料,其中所述一种或多种类型的碳相包含石墨颗粒。
7.如权利要求1-6中任一权利要求所述的复合材料,其还包含导电颗粒。
8.如权利要求1-7中任一权利要求所述的复合材料,其还包含金属颗粒。
9.如权利要求1-8中任一权利要求所述的复合材料,其中所述复合材料基本上为电化学活性的。
10.如权利要求1-9中任一权利要求所述的复合材料,其中所述复合材料为自支撑的。
11.包含权利要求1-10中任一权利要求所述的复合材料的电池电极。
12.使用权利要求1-11中任一权利要求所述的复合材料的方法,其包括仅在重量容量小于所述复合材料的约70%的最大重量容量下使用所述复合材料。
13.形成复合材料的方法,其包括:
提供包含前体和硅颗粒的混合物;以及
热解所述前体以将所述前体转化为一种或多种类型的碳相从而形成所述复合材料。
14.如权利要求13所述的方法,其中在热解所述前体后,所述混合物形成自支撑的复合结构。
15.如权利要求13或14所述的方法,其中所述一种或多种类型的碳相中的至少一种为基本上连续的相。
16.如权利要求15所述的方法,其中为基本上连续的相的所述一种或多种类型的碳相中的至少一种包含硬碳。
17.如权利要求13-16中任一权利要求所述的方法,其中所述硅颗粒包含所述复合材料的约20%重量比至约80%重量比。
18.如权利要求13-17中任一权利要求所述的方法,其中所述混合物还包含溶剂。
19.如权利要求13-18中任一权利要求所述的方法,其中所述前体包含聚酰亚胺。
20.如权利要求13-19中任一权利要求所述的方法,其中所述前体包含酚醛树脂。
21.如权利要求13-20中任一权利要求所述的方法,其中所述前体包含烃化合物。
22.如权利要求13-21中任一权利要求所述的方法,其中在所述混合物中所述硅颗粒包含大于0%重量比且小于约80%重量比,以及在所述混合物中所述前体包含约5%重量比至约80%重量比。
23.如权利要求13-22中任一权利要求所述的方法,其还包括:
在基板上浇铸所述混合物;
干燥所述混合物以形成膜;
从所述基板上除去所述膜;以及
在热压机中固化所述膜。
24.如权利要求13-23中任一权利要求所述的方法,其还包括由所述复合材料形成电池电极。
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