CN101371381A - 制造由硅或者基于硅的材料组成的纤维的方法及其在锂充电电池中的应用 - Google Patents

制造由硅或者基于硅的材料组成的纤维的方法及其在锂充电电池中的应用 Download PDF

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CN101371381A
CN101371381A CNA2007800029760A CN200780002976A CN101371381A CN 101371381 A CN101371381 A CN 101371381A CN A2007800029760 A CNA2007800029760 A CN A2007800029760A CN 200780002976 A CN200780002976 A CN 200780002976A CN 101371381 A CN101371381 A CN 101371381A
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M·格林
F-M·刘
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Abstract

一种制造硅或者基于硅的材料的纤维的方法，包括蚀刻基底上的柱并使其分离的步骤。可通过使用该纤维作为复合阳极中的活性材料而形成电池阳极。

Description

制造由硅或者基于硅的材料组成的纤维的方法及其在锂充电电池中的应用
技术领域
本发明涉及一种制造由硅或者基于硅的材料组成的纤维的方法及其在可充电锂单体电池(battery cell)的活性阳极材料中的应用。
背景技术
熟知硅可被用作可充电锂离子电化学电池的活性阳极材料(例如参见Insertion Electrode Materials for Rechargeable Lithium Batteries，M.Winter，J.O.Besenhard，M.E.Spahr和P.Novak在Adv.Mater.1998，10，No.10)。图1中示出了常规锂离子可充电单体电池的基本组成，其包括将以基于硅的阳极代替的成份基于石墨的阳极。该单体电池包括单个单体但是还可包括多个单体。
单体电池通常包括合适地外部连接于负载或者再充电源的用于阳极10的铜集电器和用于阴极12的铝集电器。基于石墨的复合阳极层14覆盖集电器10，而基于含锂金属氧化物的复合阴极层16覆盖集电器12。在基于石墨的复合阳极层14和基于含锂金属氧化物的复合阴极层16之间设置多孔塑料隔板或者隔离体20，液态电解质材料分散在多孔塑料隔板或者隔离体20、复合阳极层14和复合阴极层16中。一些情况下，多孔塑料隔板或者隔离体20可被聚合物电解质材料替换，并且在这些情况下在复合阳极层14和复合阴极层16中都出现聚合物电解质材料。
当单体电池完全充电时，锂经电解质被从含锂金属氧化物传输至基于石墨的层，在那里其与石墨反应形成化合物LiC6。作为复合阳极层中电化学活性材料的石墨的最大容量为372mAh/g。注意，所使用的术语“阳极”和“阴极”是指电池被置于负载两端之间的情况。
通常认为，当用作锂离子可充电单体电池中的活性阳极材料时，硅的容量比常用的石墨大得多。当Si通过与电化学单体电池中的锂反应转换为化合物Li21Si5时，硅的容量为4,200mAb/g。
现有的在锂离子电化学电池中使用硅或者基于硅的活性阳极材料的方法未能提供所需数量充电/放电循环内的持续容量因此在商业上不可行。
一种方法采用粉末状的硅，在一些实例中其被形成为可选地具有电子添加剂的复合物并包含涂敷在铜集电器上的合适粘合剂，例如聚偏二氟乙烯。但是在充电/放电循环中该电极不能提供持续容量。认为该容量损失是由于和锂嵌入主体硅/从主体硅提取相关的体积膨胀/收缩引起的硅粉末质量的部分机械分离。这又造成粉末质量在电绝缘“小岛”中的集聚。
在由Ohara等人在Journal of Power Sources 136(2004)303-306中所描述的另一种方法中，硅被蒸镀至镍箔集电器上形成薄膜，并且然后利用该结构形成锂离子电池的阳极。但是，尽管该方法可产生良好的容量保持率，但是仅仅对于非常薄的膜才如此，因此这些结构不能产生单位面积上可用量的容量，而提高膜厚度以形成单位面积上可用量的容量又使得良好的容量保持率消除。
在US2004/0126659中所描述的另一种方法中，硅被蒸镀至然后用于形成锂电池阳极的镍纤维上。但是发现其形成了硅在镍纤维上的不均匀分布因此明显影响操作。
在US6,887,511中所描述的另一种方法中，硅被蒸镀至粗糙的基于铜的底上形成10μm的中间厚度膜。在初始嵌入锂离子过程中，硅膜破碎而形成硅柱。这些柱然后可逆地与锂离子反应并获得良好的容量保持率。但是，该过程对较厚的膜运行不好并且形成中间厚度膜是一种昂贵的过程。另外膜破碎所形成的柱状结构不具有内在的多孔性从而该组织可保持长期的容量保持率。
发明内容
在权利要求书中列出了本发明。因为阳极电极结构采用基于硅的材料或者硅的纤维，这些硅或者基于硅的纤维与锂的可逆反应问题被克服。特别是通过在复合结构中设置纤维，即聚合物粘合剂与电子添加剂的混合物，充电/放电过程变得可逆、可重复并且获得良好的容量保持率。此外，其中设置纤维的方式也具有优点。通过提供无序的无纺纤维垫，产生完全可逆以及可重复的充电容量而不会产生明显机械分离的风险。例如，该纤维可被沉积为毡或者毡状结构。对复合结构而言，其可具有其它元件，或者毡可以具有简单粘合剂或者在结构合适的地方松散。
另外，提供了一种制造纤维的简化方法，包括蚀刻基底以形成柱并分离柱，提供了一种可靠而产额高的方法。
附图说明
现在将通过实例参考附图描述本发明的实施例，其中:
图1是示出单体电池元件的示意图；
图2是根据本发明的电极的放大照片；以及
图3示出了硅纤维/PVDF/Super P复合电极的第一循环电压曲线。
具体实施方式
总之，本发明可形成硅或者基于硅的材料的纤维或者细丝，以及将这些纤维用于形成毡状电极结构和具有聚合物粘合剂、电子添加剂(如果需要)和金属箔集电器的复合阳极结构。特别是，认为构成复合物的硅元件结构克服了充电/放电容量损失问题。
例如通过随机或者无序或者真正有序地设置，而将纤维置于复合的或者毡或者毡状结构中，即交叉以提供多个交叉点的多条长细纤维，可缓解充电/放电容量损失问题。
通常，纤维的长度直径比大约为100:1，因此在阳极层例如复合阳极层中每条纤维将沿着其长度接触其它纤维多次，形成一种其中可忽略由断裂硅接触产生的机械分离的可能的结构。而且，尽管会造成体积膨胀和体积收缩，但是将锂嵌入纤维以及从纤维去除锂都不会造成纤维破坏，因此保持了纤维内部的电子传导性。
可通过将柱与基底分离制造纤维。此外，可通过简单可重复的化学工艺提供制造柱的方式。
可形成柱的一种方式为干法蚀，例如在美国申请10/049736中所描述的深反应离子蚀刻，该申请与本申请是共同拥有的，并在此引用作为参考。本领域技术人员熟知该过程从而在这里不需要详细描述。但是简单地，蚀刻并冲洗被涂敷天然氧化物的硅基底以形成亲水表面。氯化铯(CsCl)被蒸镀在表面上，并且在干燥条件下将涂敷的基底输送至水蒸气气压不变的腔内。CsCl薄膜显影成半球的小岛阵列，其尺寸特征取决于初始厚度、水蒸气气压和显影时间。小岛阵列提供了一种有效的掩模，在其后例如通过反应离子蚀刻进行蚀刻形成了对应半球小岛的柱阵列。CsCl抗蚀剂层高度溶于水并且容易被冲洗掉。
可选地，可通过湿法蚀刻/采用例如在我们的共同待审的申请GB0601318.9中所描述的化学电交换方法(chemical galvanic exchangemethod)形成柱，该申请具有共同的受让人、标题为“Method of etching asilicon-based material”，并且在此引用作为参考。在Peng K-Q，Yan，Y-J Gao，S-P，Zhu J.，Adv.Materials，14(2004)，1164-1167(“Peng”)；K.Peng等人，Angew.Chem.Int.Ed.，442737-2742；和K.Peng等人，Adv.Funct.Mater.，16(2006)，387-394中公开了也可使用的相关方法。
在优选实施例中，例如长度为100微米、直径为0.2微米的柱形成于硅基底上并从硅基底形成。更通常，长度处于20至300微米范围、直径或者最大横向尺寸处于0.08至0.5微米范围的柱可用于提供纤维。根据该工艺，硅基底可以为n-或者p-型，并且根据化学方法，其可在任何暴露的(100)或者(110)晶面上被蚀刻。因为蚀刻沿着晶面进行，所以所形成的纤维为单晶体。由于该结构特征，该纤维将非常容易地形成长度直径比为大约100:1，并且当处于复合阳极层中时，允许每条纤维沿着其长度多次接触其它纤维。还可在超大规模集成电路(VLSI)电子级晶片上或者其丢弃的样品(单晶晶片)上进行蚀刻工艺。作为更廉价的选择，还可采用如用于太阳能面板的光伏级多晶材料。
为将柱分离以获得纤维，附接有柱的基底被置于大口杯或者任何合适的容器中、被惰性液体例如乙醇覆盖并受到超声搅拌。发现在几分钟内可看到液体变混浊，并且可通过电子显微镜检验看到在该阶段柱被从其硅基底去除。
将认识到，用于“收集”柱的可选方法包括刮擦基底表面以将其分离或者将其化学分离。一种适合于n-型硅材料的化学方法包括在出现对硅晶片的背面照射时在HF溶液中蚀刻所述基底。
一旦硅柱被分离则其可被用作锂离子电化学电池的复合阳极中的活性材料。为制造复合阳极，从溶液中过滤所收集的硅，可将其与聚偏二氟乙烯混合，以及与浇铸溶剂例如n-甲基吡咯烷酮形成浆液。然后该浆液可例如利用刮刀物理地、或者以任何其它合适方式施加或者涂敷至金属板或者金属箔或者其它导电基底，以产生需要厚度的涂敷膜，然后利用可采用50℃至140℃的提高温度的合适干燥系统，将浇铸溶剂从该膜蒸发，以留下没有或基本没有浇铸溶剂的复合膜。所产生的垫或者复合膜具有多孔和/或毡状结构，其中硅纤维的质量通常占70％和95％。复合膜的孔体积百分比为10-30％，优选大约为20％。
图2示出了通过上面方法获得的复合电极结构的SEM。可选地，毡或毡状结构可形成为片材料(不一定在集电器上)并用作其本身的集电器。
其后可以例如根据图1所示出的总体结构但是以硅或者基于硅的活性阳极材料而非石墨活性阳极材料以合适方式制造锂离子单体电池。例如由多孔隔板18覆盖基于硅纤维的复合阳极层，添加到最终结构的电解质充满全部可进入的孔体积。在将电极置于合适的外壳中之后添加电解质，所述添加可包括真空填充阳极，以保证孔体积被填充液态电解质。
请参考下面的实例：
称量0.0140g的硅纤维放入2cm2的Eppendorf离心机管中，并添加0.0167g的Super P导电碳。然后将N-甲基吡咯烷酮(NMP)移入管中直到分散所有的材料(0.92g)。预先，7.8wt％的PVDF已经溶解于NMP中。将含有0.0074g PVDF的该溶液添加至管。混合成分如下Si:PVDF:Super P＝85.3:4.5:10.1wt％。
该管被置于超声槽中达一小时以使该混合物均匀，然后再搅拌一小时。然后采用刮刀间隙为0.8mm的刮刀将该浆液涂敷至14μm的铜箔上。然后在100℃下对该涂层干燥一小时以蒸发NMP溶剂。经过干燥之后，涂层的厚度为30-40μm。图2示出了没有Super P碳的相似混合物和涂层的SEM。
轻轻轧制涂层，然后电极盘被切削为直径为12mm。在充氩的手套箱将其组装至电化学电池中。反电极和基准电极都为锂金属。电解质为有机碳酸酯混合物中的LiPF6。在VMP3设备上测试该电池。经过三十分钟的浸泡之后，该电池被保持在-0.1mA达一小时，然后获得-0.2mA直到需要的锂化容量。然后在+0.2mA对电极脱锂化，直到1.0V vs.Li/Li+的电压。图3示出了该第一循环中的电池电压。
这里所描述方法的特别优点在于如果必要可制造、轧制大片的基于硅的阳极，然后和当前锂离子单体电池的基于石墨的阳极一样地随后切开或者冲压，这意味着这里所描述的方法可以以现有的制造能力进行改良。
这里所描述设置的另一个优点在于结构强度实际上随着每次充电操作提高。这是因为由于在形成无定形结构的纤维节点上的破裂晶体结构造成纤维相互“熔合”。这又降低了在多个循环上容量损失的风险，这是因为一旦纤维以上述方式连接则纤维机械分离的可能更低。
当然，将理解可采用任何合适的方法以实现上述方法和装置。例如，柱分离操作可包括摇动、刮擦、化学或者其它操作的任何一种，只要从基底去除柱以形成纤维。合适时，对基于硅的材料的参考包括硅。该纤维可具有任何合适的尺寸，并且例如可以为纯硅或者掺杂的硅或者其它基于硅的材料例如硅-锗混合物或者任何其它合适的混合物。形成柱的基底可以为n-或p-型，从100至0.001欧姆cm，或者其可以为合适的硅合金，例如SixGe1-x。纤维可用于任何合适的目的例如制造通常包括阴极的电极。该阴极材料可以为任何合适的材料，通常为基于锂的金属氧化物或者磷酸盐材料，例如LiCoO2、LiMnxNixCo1-2xO2或者LiFePO4。不同实施例的特征可以相互替换或者并列设置并且以任何合适的顺序进行该方法步骤。

Claims (35)

1.一种制造硅或者基于硅的材料的纤维的方法，包括如下步骤：蚀刻硅基底或者基于硅的基底以形成柱并将所述柱从所述基底分离。
2.根据权利要求1的方法，其中所述纤维的横向尺寸处于0.08至0.5微米的范围、优选为0.2微米，并且其长度处于20至300微米的范围、优选为100微米。
3.根据权利要求1的方法，其中所述纤维的纵横比为大约100:1。
4.根据权利要求1、2或3的方法，其中所述纤维具有基本上圆形的横截面。
5.根据权利要求1、2或3的方法，其中所述纤维具有基本上非圆形的横截面。
6.根据前述权利要求中任一项的方法，其中通过反应离子蚀刻形成所述柱。
7.根据前述权利要求中任一项的方法，其中通过化学反应蚀刻形成所述柱。
8.根据权利要求7的方法，其中通过电交换蚀刻形成所述柱。
9.根据前述权利要求中任一项的方法，其中通过刮擦、搅拌或者化学蚀刻的一种或多种使所述柱分离。
10.根据前述权利要求中任一项的方法，其中所述硅或者基于硅的材料包括未掺杂硅、掺杂硅或者硅锗混合物中的一种。
11.根据前述权利要求中任一项的方法，其中所述纤维为单晶硅，或者基于硅的材料包括单晶硅或者硅锗中的一种。
12.一种形成电池电极的方法，包括沉积含基于硅的纤维的浆液以形成基于硅的纤维的层。
13.根据权利要求12的方法，其中所述纤维为单晶纤维。
14.根据权利要求12或者13的方法，其中所述纤维被沉积在毡中。
15.根据权利要求12、13或者14的方法，其中所述纤维被沉积在复合物中。
16.根据权利要求12至15中任一项的方法，包括将所述纤维沉积在集电器上。
17.根据权利要求12至16中任一项的方法，其中通过根据权利要求1至11中任一项的方法制造所述纤维。
18.根据权利要求12至17中任一项的方法，其中所述电极为阳极。
19.根据权利要求12至15中任一项的方法，其中所述毡的孔体积百分比为大约10-30％。
20.一种制造锂可充电电池的方法，包括如下步骤：形成根据权利要求12至19中任一项的阳极并向阴极添加电解质。
21.根据权利要求20的方法，还包括在阴极和所述阳极之间添加隔离体。
22.根据权利要求20或21的方法，还包括在所述电池周围提供外壳。
23.一种复合电极，其包括采用前述权利要求中任一项制造的基于硅的纤维作为其活性材料的一种。
24.根据权利要求12的复合电极，其使用铜为集电器。
25.根据权利要求12的复合电极，其中所述电极为阳极。
26.一种电化学电池，包括如权利要求12至14中任一项所述的阳极。
27.根据权利要求15的电化学电池，其中所述阴极包括能够释放并重新吸收锂离子的含锂化合物作为其活性材料。
28.根据权利要求15的电化学电池，其中所述阴极包括作为其活性材料的基于锂的金属氧化物或者磷酸盐，优选为LiCoO2或者LiMnxNixCo1 -2xO2或者LiFePO4。
29.一种锂可充电电池阳极，包括基于硅的单晶纤维的层，其中所述纤维形成毡。
30.根据权利要求29的阳极，其中所述纤维为复合物的一部分。
31.根据权利要求29至30中任一项的阳极，包括位于所述纤维交叉点上的无定形硅部分。
32.一种电池，包括阴极和根据权利要求29至30中任一项的阳极。
33.根据权利要求32的电池，其中所述阴极包括基于锂的材料。
34.根据权利要求33的电池，其中所述阴极包括二氧化钴锂。
35.一种设备，由根据权利要求26至34中任一项的电池供电。
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