CN109562950A - 用于LIB阳极的阀金属基底上的纳米级/纳米结构Si涂层 - Google Patents

用于LIB阳极的阀金属基底上的纳米级/纳米结构Si涂层 Download PDF

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CN109562950A
CN109562950A CN201780050465.XA CN201780050465A CN109562950A CN 109562950 A CN109562950 A CN 109562950A CN 201780050465 A CN201780050465 A CN 201780050465A CN 109562950 A CN109562950 A CN 109562950A
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詹姆斯·翁
大卫·弗罗斯特
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Abstract

提供了纳米级和纳米结构的Si颗粒的改进结构，用作锂离子电池的阳极材料。将Si颗粒制备成涂有MgO的复合物，并冶金结合在导电耐火阀金属载体结构上。

Description

用于LIB阳极的阀金属基底上的纳米级/纳米结构Si涂层
技术领域
本发明涉及用于锂离子电池的阳极材料的改进，并且将结合这种用途进行描述，尽管可以考虑其它用途。
背景技术
硅是用于锂离子电池(LIB)中高容量阳极的有前途的材料。当与锂形成合金时，硅的比容量(mAh/g)比传统的石墨阳极材料高一个数量级。然而，硅在锂化(充电)和脱锂(放电)期间分别表现出大的体积变化(高达400％的膨胀和收缩)。对于体硅(bulk silicon)，这在硅内产生结构应力梯度并导致断裂和机械应力失效(粉碎)，从而降低硅阳极的有效电接触和寿命。
已经进行了相当大的努力来通过控制形态和将硅颗粒的尺寸限制到低于硅不太可能破裂的尺寸(约50nm)来克服该内在问题。
避免由硅的膨胀/收缩引起的物理损坏的各种尝试包括如薄膜、纳米线、纳米管、纳米颗粒、介孔材料、和纳米复合材料的形式的纳米级和纳米结构的硅。大多数这些方法都不能提供可行的，具有成本效益的解决方法。
发明内容
一种有希望的方法是利用Si-MgO复合材料，其根据以下反应，通过SiO2和镁的机械合金化/固相反应形成：
2Mg(s)+SiO2(s)→2MgO(s)+Si(s) (式1)
MgO基质已显示出缓冲体积变化的效果；然而，这些复合材料具有相对低的导电性，使得它们作为阳极材料效率很低。
分散在导电基底和载体上的亚微米级电化学活性颗粒长期以来一直用于包括燃料电池和蓄电池的电化学电池。该载体结构是电池效率和寿命方面的重要组成部分。特别是阀门(或耐火材料)金属，(特别是：钛、铌、钽及其合金)在化学处理和阴极保护的应用中已被用作电化学活性材料的基底70多年。这些应用利用在暴露的阀金属区域上形成钝化氧化膜，作为为活性材料产生导电和电化学稳定的载体结构的手段。
Mg长期以来被用作用于纯化耐火金属的镁热还原剂。这种工艺在生产用于电容器应用的高容量，高表面钽粉末中很常见，这些应用通过气相/固相反应发生：
5Mg(g)+Ta2O5(s)→5MgO(s)+2Ta(s)
(式II)
所得到的氧化镁在主体Ta颗粒上形成表面涂层，并使用无机酸除去。
在一个方面，本发明提供了与锂离子电池一起使用的电化学活性电极材料，该电化学活性材料电极材料包括阀金属基底材料，该阀金属基底材料由横截面不大于约10微米的阀金属的细丝或颗粒形成并涂有冶金结合的硅颗粒。
在优选的实施方式中，阀金属选自由钽、铌、钽合金、铌合金、铪、钛和铝组成的组。
在另一个优选的实施方式中，阀金属丝的厚度小于约5-10微米，优选厚度小于约1微米。
在一个方面，硅涂层由纳米级纳米颗粒组成。
在另一方面，硅颗粒涂覆到在稳定的MgO基质中的阀金属基底上。
在另一方面，如上所述的电活性电极材料形成阳极。
本发明还提供一种形成可用于形成锂离子电池的电极基底的方法，包括以下步骤：(a)提供由横截面不大于约10微米的阀金属的细丝或颗粒形成的阀金属基底材料；(b)用通过镁与二氧化硅和阀金属的镁热反应形成的冶金结合硅涂覆阀金属基底材料。
在该方法的一个方面，镁热反应在真空下或在惰性气体中在高温下进行，优选在选自由800-1200℃，900-1100℃和950-1050℃组成的组的高温下进行。
在该方法的另一个方面，镁热反应进行选自2-10小时，4-8小时和5-6小时的时间。
在该方法的另一个方面，包括在反应后通过酸蚀刻除去至少一些氧化镁的步骤。
在该方法的一个优选方面，阀金属选自由钽、铌、钽合金、铌合金、铪、钛和铝组成的组。
在该方法的另一个优选方面，细丝或纤维的厚度小于约5-10微米，优选厚度小于约1微米。
在该方法的另一个方面，电化学活性材料包含硅纳米颗粒。
本发明还提供一种锂离子电池，包括：壳体，其包含彼此分离的阳极和阴极；以及电解质，其中所述阳极由电活性电极材料形成，包括以下步骤：(a)提供由横截面不大于约10微米的阀金属的细丝或颗粒形成的阀金属基底材料；(b)用通过镁与硅和阀金属的镁热反应形成的冶金结合硅涂覆阀金属基底材料。
在电池的另一个方面，阀金属选自钽、铌、钽合金、铌合金、铪、钛和铝。
本发明提供耐火金属基底的Mg脱氧和基本上同时还原SiO2(二氧化硅)的组合反应(或共反应)，以在稳定的MgO涂层内部产生纳米结构Si的纳米级涂层，两者都冶金结合到阀金属基底上。
阀金属和SiO2中的氧化物杂质基本上同时反应以形成纯Si的纳米级纳米结构，其通过反应牢固地结合到阀金属基底，例如钽(Ta)：
9Mg(g)+2Ta2O5(s)+2SiO2→4Ta(s)+2Si(s)+9MgO(s)
(式III)
整个过程涉及将阀金属颗粒(例如钽)与在水基溶液或凝胶中的4至200微米尺寸，优选10至100微米尺寸，更优选20至50微米尺寸的SiO2纳米颗粒混合。在一种方法中，将SiO2颗粒浸渍到预先形成的钽纤维多孔垫中作为SiO2纳米颗粒的水凝胶。在另一种方法中，将松散的钽颗粒与SiO2颗粒混合。然后将所得混合物进行通过式III在真空或惰性气体下在900℃-1100℃的温度下进行2至10小时的镁热还原。镁还原了钽纤维中的二氧化硅和氧化物杂质，从而允许硅冶金结合到钽基底上。产生的氧化镁可以保留，或者例如通过酸蚀刻除去。所得到的结构是海绵状、高表面积、导电电化学稳定的耐火金属基底，在MgO涂层内涂覆有亚微米Si颗粒的复合物。
附图说明
从以下结合附图的详细描述中可以看出本发明的其他特征和优点，其中：
图1是根据本发明的提供阳极材料的方法的示意性框图；
图2和3是两种不同放大倍数的SEM照片，示出了根据本发明的冶金结合到Ta载体颗粒上的Si颗粒的纳米级纳米结构；
图4绘制了根据本发明制造的阳极材料的容量与时间的关系；
图5绘制了根据本发明制造的阳极材料的库仑效率与时间的关系；
图6绘制了根据本发明制造的锂离子电池阳极的微分电容与电池电压的关系；
图7是根据本发明的可充电电池的剖视图；和
图8是根据本发明制造的电池的透视图。
具体实施方式
在本发明的一个实施方式中，耐火金属由微米尺寸(例如横截面不大于约10微米)的钽颗粒形成，如在早先的美国专利号9,155,601、美国专利号5,869,196，美国专利号7,146,709和PCT WO2016/187143A1中所述，其内容通过引用并入本文。
参考图1，生产过程开始于制造阀金属丝，优选钽，通过在步骤10中将钽的细丝或导线与如铜的延性材料结合以形成坯料。然后在步骤12将坯料密封在挤出罐中。根据本人的美国专利‘196的教导，在步骤14中挤出和拉伸。然后将挤出和拉伸的细丝在切碎站16切割或切碎成短段，通常为1/16至1/4英寸长。优选地，切割的细丝都具有大致相同的长度。实际上，细丝越均匀越好。然后将切碎的细丝传送到蚀刻站18，在此使用合适的酸浸出韧性金属。例如，在铜是韧性金属的情况下，蚀刻剂可以包含硝酸。
在酸中的蚀刻从钽丝之间除去铜。
在蚀刻之后，留下多个短的钽丝。然后将钽丝在洗涤站20中在水中洗涤，并且部分倾析洗涤水以留下钽丝在水中的浆液。然后在涂覆站22中在水中将钽颗粒在水中的浆液与细颗粒，例如，4至200微米尺寸的二氧化硅颗粒混合，形成海绵状物质。然后将涂覆的海绵状物质干燥并在反应站24处通过在真空下或在惰性气体中在800至1200℃，优选900至1100℃，更优选950至1050℃下处理2至10小时，优选4-8小时，更优选5-6小时进行镁热反应。镁还原二氧化硅和钽纤维内的氧化物杂质，同时允许硅冶金结合到钽纤维上。产生的任何氧化镁可以保留，但优选通过例如酸蚀刻除去。另一方面，没有必要完全除去任何可能从挤出和拉伸步骤中遗留下来的铜，因为铜也会冶金地结合到硅上。所得到的结构是海绵状，高表面积，导电电化学稳定的钽金属基底物质，其涂覆有涂有MgO基质的亚微米Si颗粒的复合物。然后可以将所得到的海绵状物质与水混合，并在轧制站26处浇铸为垫。然后将得到的垫在干燥站28处进一步压缩和干燥。
作为涂覆和轧制的替代方案，可以通过将浆料喷射浇铸到基底上来形成薄片，除去过量的水并如前所述压制和干燥所得的垫。
结果得到厚度基本均匀的钽丝涂覆的Si/MgO复合物或Si的高度多孔的薄片。
如本人在上述PCT申请中所报道的，切碎的细丝的水性浆料将充分粘合在一起，使得纤维可以浇铸成片材，可将其压制并干燥成稳定的垫。这是令人惊讶的，因为金属丝本身不吸水。尽管如此，只要细丝基本上不厚于约10微米，它们就会粘在一起。另一方面，如果细丝远大于约10微米，它们将不会形成稳定的垫或片材。因此，优选细丝的厚度小于约10微米，优选小于1微米。为确保细丝均匀分布，从而确保生产均匀的垫。优选通过机械搅拌或振动对浆料进行剧烈混合。
所得钽垫的密度或孔隙率可以简单地通过改变垫的最终厚度来改变。
而且，如果需要，可以堆叠多个层以形成可能需要的较厚垫，例如，用于高密度应用。
得到的钽垫包括涂覆钽丝的亚微米尺寸的Si或Si/MgO复合物的多孔垫，它们彼此接触，形成导电垫。
或者，在本发明的一个优选实施方式中，原料钽丝可以通过上述铸造和轧制形成为电极材料的垫，然后通过如上所述的镁热还原涂覆硅纳米颗粒，例如通过将钽垫浸入含有二氧化硅在水中的水基溶液，然后如上所述在真空或惰性气体下加热。
如图2和3所示的Si/Ta结构是涂有纳米级纳米结构Si颗粒层的阀金属结构。在作为LIB阳极循环期间，MgO可以充当稳定缓冲剂以防止Si的降解。尽管优选使用无机酸除去MgO基质，以显示与Ta载体颗粒冶金结合的Si颗粒的纳米级纳米结构。
测试所得材料的容量随时间的变化，库仑效率随时间的变化以及微分电容随电池电压的变化，结果示于图4-6中。
所得的Si涂覆的耐火材料可以通过任何标准制造方法形成有用的LIB阳极，包括但不限于：沉积在集电器上的薄湿敷法(thin wet-lay method)、使用或不使用导电碳添加剂、压延织物、铸造等。例如，如图7和8所示，涂覆的垫在隔板(separator sheet)36之间堆叠组装，形成正(阳极)和负(阴极)电极38、40。电极38、40和隔板36在凝胶辊中缠绕在一起，***壳体42中，具有从组装站48中的凝胶辊延伸的正极接头44和负极接头46。然后可以将接头(tab)焊接到电极基底的暴露部分，并且壳体充满电解质且壳体密封。结果是高容量可再充电电池，其中电极材料包括极易延展的细金属复合细丝，其能够重复充电和排出而没有不利影响。还考虑了其他方法。
在不脱离本发明的精神和范围的情况下，可以对上述发明进行各种改变。例如，已经特别结合硅描述了本发明，可以有利地使用如锗的其他材料。在不脱离本发明的精神和范围的情况下，可以进行其他改变。

Claims (15)

1.一种用于锂离子电池的电活性电极材料，所述电化学活性材料电极材料包括阀金属基底材料，该阀金属基底材料由横截面不大于约10微米的阀金属细丝或颗粒形成，并涂有冶金结合的硅颗粒。
2.根据权利要求1所述的电活性电极材料，其中所述阀金属选自钽、铌、钽合金，铌合金、铪、钛和铝组成的组。
3.根据权利要求1或2所述的电活性电极材料，其中所述阀金属细丝的厚度小于约5-10微米，优选厚度小于约1微米。
4.根据权利要求1-3中任一项所述的电活性电极材料，其中所述硅涂层由纳米级纳米颗粒组成。
5.根据权利要求1-4中任一项所述的电活性电极材料，其中所述硅颗粒涂覆到在稳定的MgO基质中的所述阀金属基底上。
6.根据权利要求1-5中任一项所述的电活性电极材料，其形成为阳极。
7.一种形成可用于形成锂离子电池的电极基板的方法，包括以下步骤：
（a）提供阀金属基底材料，其由横截面不大于约10微米的阀金属细丝或颗粒形成；和，
（b）用通过镁与二氧化硅和阀金属的镁热反应形成的冶金结合硅涂覆阀金属基底材料。
8.根据权利要求7所述的方法，其中所述镁热反应在真空下或在惰性气体中在高温下进行。
9.根据权利要求8所述的方法，其中所述高温选自800-1200℃，900-1100℃和950-1050℃，和/或其中镁热反应进行选自2-10小时，4-8小时和5-6小时的时间。
10.根据权利要求7-9中任一项所述的方法，并且包括在反应后通过酸蚀刻除去至少一些氧化镁的步骤。
11.根据权利要求7-10中任一项所述的方法，其中所述阀金属选自由钽、铌、钽合金、铌合金、铪、钛和铝组成的组。
12.根据权利要求7-11中任一项所述的方法，其中所述细丝或纤维的厚度小于约5-10微米，优选厚度小于约1微米。
13.根据权利要求7-12中任一项所述的方法，其中所述电化学活性材料包括硅纳米颗粒。
14.一种锂离子电池，包括壳体，所述壳体包含彼此分离的阳极和阴极，以及电解质，其中所述阳极由权利要求1-5中任一项所述的电活性电极材料形成。
15.根据权利要求14所述的电池，其中所述阀金属选自由钽、铌、钽合金、铌合金、铪、钛和铝组成的组。
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