CN111261865A - 二次电池用负极活性物质及其制备方法 - Google Patents
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Abstract
本发明公开了一种二次电池用负极活性物质及其制备方法。本发明一实施例的硅类活性物质复合物包含硅及上述硅的至少一部分氧化而成的硅氧化物,相对于上述硅及上述硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间。
Description
本申请案是申请日期为2016年10月09日,申请号为201580018810.2,国际申请号为PCT/KR2015/003575,发明名称为“二次电池用负极活性物质及其制备方法”的专利申请案的分案申请。
技术领域
本发明涉及二次电池技术,特别涉及二次电池用负极活性物质及其制备方法。
背景技术
二次电池作为可通过使用可逆性优秀的电极材料来进行充电及放电的电池,代表性地,普遍使用锂二次电池。上述锂二次电池不仅可作为智能手机、便携式计算机及电子纸等IT设备的小型电源来使用,还期待作为通过装载于汽车等移动工具来使用或者用于智能电网等供电网络的电力储存场的中大型电源的应用。
将锂金属作为锂二次电池的负极材料来使用时,因枝晶的形成,会产生电池短路或者存在引发爆炸的危险性,因此,替代上述锂金属,作为负极,多使用可对锂实施嵌入(intercalation)及脱嵌(deintercalation),且具有372mAh/g的理论容量的石墨及人造石墨等的结晶质类碳或软碳、硬碳和碳类活性物质。但是,随着扩大对二次电池的应用,进一步需要二次电池的高容量化及高输出化,由此,可替代碳类负极材料的理论容量,且具有500mAh/g以上容量的硅(Si)、锡(Sn)或铝(Al)等可与锂形成合金的非碳类负极材料正备受瞩目。
在上述非碳类负极材料中,硅的理论容量达到约4200mAh/g,由此理论容量最大,因此在容量方面,其应用非常重要。但是,由于硅在充电时,体积会膨胀到4倍左右,因此,在充电、放电的过程中,进行因体积变化而破坏活性物质之间的电连接或者从集电体分离活性物质,而且因电解质而产生的活性物质的侵蚀而导致形成固体电解质界面层(SolidElectrolyte Interface,SEI)等不可逆反应,由此使电池寿命劣化,因而在将硅实用化方面存在障碍。
因此,为了适用硅材料,既要抑制在充电、放电时的体积变化,又要改善电池的不可逆容量。并且,随着对二次电池需求的爆发性增长,需要确保既可大量生产又经济的硅负极活性物质的制备技术。
发明内容
技术问题
因此,本发明所要解决的技术问题在于,提供如下的负极活性物质,即,通过利用硅来改善不可逆容量,而且缓解随着充电、放电发生的体积变化,从而既提高能量密度,又具有高容量、长寿命。
并且,本发明所要解决的另一技术问题在于,提供可经济、迅速地大量形成具有前述优点的硅负极活性物质的制备方法。
解决问题的方案
用于解决上述问题的本发明一实施方式的硅类活性物质复合物包含硅及上述硅的至少一部分氧化而成的硅氧化物。相对于上述硅及上述硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间。
在一实施例中,上述硅类活性物质复合物包含上述硅的芯部以及包围上述芯部的硅氧化物壳。上述硅氧化物壳的厚度可以在2nm至30nm的范围内。优选地,上述硅氧化物壳的厚度可以在3nm至15nm的范围内。在另一实施例中,上述硅类活性物质复合物可包含硅基质以及分散在上述硅基质内的上述硅氧化物。
上述硅活性物质复合物的平均直径在30nm至300nm的范围内,优选地,上述硅活性物质复合物的平均直径可以在30nm至200nm的范围内。在一实施例中,在上述硅类活性物质复合物的外围还可形成有导电层。上述导电层可包含非晶质碳膜或导电性金属氧化物粒子。
用于解决上述另一问题的本发明另一实施方式的硅类活性物质复合物的制备方法包括:提供硅的粒子的步骤;以及通过对上述硅的粒子进行氧化,来形成包含硅及上述硅的至少一部分氧化而成的硅氧化物的硅类活性物质复合物的步骤。在此情况下,相对于上述硅及上述硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间。
在一实施例中,在对上述硅的粒子进行氧化的步骤中,在含氧液相溶剂内,能够以化学氧化的方式对上述硅的粒子进行氧化。在此情况下,上述含氧液相溶剂包含甲醇、异丙醇(IPA)、过氧化氢(H2O2)、水或它们中的2种以上的混合溶剂。
在另一实施例中,在对上述硅的粒子进行氧化的步骤中,还能够向上述硅的粒子注入氧离子。在此情况下,为了既抑制因硅的热氧化而引起的致密化又使硅基质与注入的氧相结合,可在50℃至200℃以下的低温下额外地进行热处理。
发明的效果
本发明的实施例可提供硅类活性物质复合物,上述硅类活性物质复合物包含硅和硅的至少一部分氧化而成的硅氧化物,相对于上述硅及上述硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间,由此使纯硅复合化,从而相对于硅的理论容量,维持80%以上的容量,并提高寿命和可靠性。
并且,根据本发明的实施例,在含氧液相溶剂内使硅的粒子氧化或者通过注入氧离子来使硅氧化,从而提供既可大量生产又经济的具有前述优点的硅类活性物质复合物的制备方法。
附图说明
图1a及图1b为分别表示本发明多种实施例的硅类活性物质复合物的剖视图。
图2为示出本发明一实施例的硅类活性物质复合物的制备方法的流程图。
具体实施方式
以下,参照附图详细说明本发明的优选实施例。
本发明的多个实施例用于使本发明所属技术领域的普通技术人员更加完整地理解本发明,以下实施例能够以多种不同的方式变形,本发明的范围不局限于以下实施例。反而,这些实施例使本公开内容更充实、完整,用于向本发明所属技术领域的普通技术人员完整地传递本发明的思想。
并且,在以下附图中,为了便于说明及说明的明确性,以夸张的方式示出了各层的厚度或大小,在附图中,相同的附图标记表示相同的要素。如在本说明书中所使用,术语“和/或”包括相应列举的项目中的一种及一种以上的所有组合。
在本说明书中使用的术语用于说明特定实施例,而并非用于限制本发明。如在本说明书中所使用,只要在文脉上未明确指出其它情况,则单个形态可包括多个形态。并且,在本说明书中所使用的情况下,“包含(comprise)”和/或“包含的(comprising)”用于特定所提及的多个形状、数字、步骤、动作、部件、要素和/或它们的组合,而并非排除一种以上的其它形状、数字、动作、部件、要素和/或多个组合的存在或附加。
图1a及图1b为分别示出本发明多种实施例的硅类活性物质复合物100A、100B的剖视图。
参照图1a及图1b,硅活性物质复合物100A、100B具有粒子结构。图1a的硅活性物质复合物100A可包含硅的芯部10以及包围芯部10的硅氧化物壳20A。如图1b所示,硅活性物质复合物100B还可包含硅基质10以及分散在基质10的硅氧化物20B。
在部分实施例中,还可在硅活性物质复合物100A的最外围包括导电层30。导电层30还可包括石墨、软碳或石墨烯等碳类导电层。导电层30用于使相接触的硅活性物质复合物100A之间电连接,并减少集电体(未图示)为止的内部电阻。
在部分实施例中,上述碳类导电层可以为结晶质或至少局部为非晶质碳膜。当碳类导电层具有高结晶度时,可以为石墨,但在这种情况下,可在表面与电解液发生反应。但是,低结晶度或非晶质碳膜对上述电解质具有化学耐蚀性,因此在充电、放电时会抑制上述电解液的分解,从而具有可提高负极的寿命的优点。并且,在上述碳类导电层中,具有导电性的SP2石墨结构和具有绝缘性的SP3的钻石结构可以并存,为了使碳类导电层具有导电性,还可使上述SP2的摩尔分数大于SP3的摩尔份数,上述摩尔份数可通过热处理工序进行调节。
前述的碳类导电层为例示性的,本发明并不局限于此。例如,硅复合物活性物质100A的最外围还可以是锑锌氧化物或锑锡氧化物等导电性金属氧化物的纳米级粒子或者粒子层等的其它导电层。虽然未在图1b中示出,但在硅活性物质复合物100B上可额外地提供前述的导电层30。
在硅类活性物质复合物100A、100B中,相对于形成硅的芯部10及硅的基质10的硅、硅氧化物壳20A及分散的硅氧化物20B的总重量,氧的含量限制在9%至20%重量百分比之间。在上述氧的含量范围内,使初始充电率和容量维持特性均维持在80%以上,从而可提供适合于普遍使用的硅类活性物质复合物。硅的芯部10及硅的基质10可以为一次粒子,也可以为由上述一次粒子凝集而成的二次粒子。在此情况下,相对于硅类活性物质复合物的硅及硅氧化物的总重量,氧的含量为10%至20%重量百分比之间。
利用常用的元素分析仪(ELTRA ONH-2000)以红外线检测方式检测上述氧含量。具体采用如下方式,即,使用2~10mg的试样、8kW的热量、氦(纯度为99.995%)载气来将存在于样本内的氧变化成二氧化碳,并测定二氧化碳产生量来使氧量定量化。
表1为表示基于半电池的氧含量的初始效率及容量维持率的表,上述半电池具有利用本发明实施例的硅类活性物质复合物来制备的负极。容量维持率为在执行完50次充电、放电后的结果。作为基准的初始容量为作为硅的理论容量的4200mAh/g,表1中记载了根据氧含量来测定的复合物的重量比容量。
表1
当氧的含量小于9%重量百分比时,体积膨胀抑制效果微不足道,从而使硅类活性物质复合物的容量维持率较少到小于80%,由此无法改善根据体积变化的寿命劣化。但是,当氧的含量大于20%重量百分比时,虽然改善了容量维持率特性,但使初始充电效率减少到小于80%,从而使能量密度劣化。
在硅类活性物质复合物中,硅氧化物提供可对因硅在充电、放电时的体积变化而产生的应力进行吸收的机构,从而可抑制因充电、放电而引起的不可逆性,由此改善寿命,但相对于纯硅,具有较低的容量,因此需要以如表1所示的方式来限制硅氧化物的含量。作为用于解除硅的高体积膨胀的对策,所适用的硅氧化物因过度的氧容量而减少能量密度,但在本发明实施例的硅类活性物质复合物中,通过控制前述的氧含量来减少基于容量和体积变化的不可逆性,从而可以应用硅类活性物质复合物。
确认到如下情况,即,前述的硅类活性物质复合物的容量及容量维持率特性还依赖于粒子结构的硅活性物质复合物100A、100B的大小。硅活性物质复合物100A、100B可具有30nm至300nm范围内的平均粒径,优选地,具有30nm至200nm范围内的平均粒径。当粒子的平均直径小于30nm时,在活性物质浆料内,导电层或粒子形态的导电材料的相对比率变大,从而使电池容量降低到小于80%。并且,当粒子的平均直径大于300nm时,在芯壳式的复合物100A的情况下,使硅氧化物壳厚度增加,从而即使改善根据体积变化的不可逆性,也使容量急剧下降到50%以下。像这样,当使硅氧化物壳厚度增加时,即使有效控制硅氧化物的密度,也因硅氧化物更多地参与锂的氧化及还原反应,从而推测难以使内部的芯部起到活性物质的作用。
在一实施例中,芯壳结构的硅类活性物质复合物100A的壳20A的厚度为2nm至30nm,在此范围内,硅类活性物质复合物100A具有80%以上的初始容量。优选地,芯壳结构的硅类活性物质复合物100A的壳20A的厚度为3nm至15nm,在此范围内,硅类活性物质复合物100A具有90%以上的初始容量。当壳20A的厚度小于2nm时,由于低机械强度,无法阻止芯部10体积的膨胀,当壳20A的厚度大于30nm时,壳20A筛选出内部硅的芯部10,从而出现容量的减少。
图2为示出本发明一实施例的硅类活性物质复合物的制备方法的流程图。
参照图2,准备硅的粒子(步骤S10)。上述硅的粒子可以为多晶硅或单晶硅粗颗粒,甚至还可以为结晶度低的非晶质。可通过粉碎工序或磨碎工序使上述粗颗粒纳米粒子化,或者对大体积的硅材料,例如,通过对硅棒或晶圆进行电爆来准备上述硅的粒子。上述硅的粒子以可使通过后述的用于形成硅氧化物的工序形成的硅活性物质复合物具有30nm至300nm范围内的平均粒径,优选地,可具有30nm至200nm范围内的平均粒径的方式得到控制。
对被精细化的硅的粒子进行氧化,来形成包含硅及硅的至少一部分氧化而成的硅类活性物质复合物(步骤S20)。可通过热氧化来使硅的粒子氧化。但是,由于这种热氧化在热平衡状态下容易诱导硅的氧化反应,从而形成致密的硅氧化物(实质上满足化学计量学的SiO2)。但是,确认到如下情况,即,即使这种被热氧化的致密的硅氧化物可通过抑制芯部的体积变化来维持80%以上的容量维持率,也因可能筛选出内部的芯部,从而可使容量急剧下降至硅的理论容量的60%以下。
因此,在一实施例中,可通过在含氧液相溶剂内对硅的粒子进行化学氧化来使硅的粒子氧化。在以如上所述的方式形成的硅类活性物质复合物中,相对于硅和硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间。上述含氧液相溶剂可以为甲醇、异丙醇、过氧化氢、水或它们中的2种以上的混合溶剂,优选地,可以为环境负荷小的水。
上述甲醇作为相对于碳的氧含量最大的碳氢化合物,通过抑制在其它碳氢化合物的情况下可能产生的碳成分,从而有利于形成具有芯部及形成于上述芯部上的硅氧化物壳的硅类活性物质复合物。实际上,在其它碳氢化合物的情况下,为了防止在芯部上形成硅氧化物或者防止硅氧化物的形成,还存在如下问题,即,需要进行用于去除碳的额外的热处理,并且因热氧化而形成致密的SiO2。
在另一实施例中,可通过用于向被精细化的硅的粒子注入氧的氧离子注入工序来制备硅类活性物质复合物。上述硅的粒子成为硅基质,被注入离子的氧提供分散在上述硅基质内的硅氧化物。在上述注入离子的工序中,以相对于制备出的硅类活性物质复合物的硅和硅氧化物的总重量,氧的含量限制在9%至20%重量百分比之间的方式调节离子的注入能量和密度。为了既抑制因硅的热氧化而引起的致密化又使硅基质与注入的氧相结合,还可在50℃至200℃以下的低温下额外地进行热处理。
在另一实施例中,在上述硅的粒子中,可通过对硅的粗颗粒进行粉碎或磨碎的工序以及借助从上述粉碎或磨碎工序诱导出的压缩以及剪应力中的至少一种来使上述硅的粒子化学氧化,由此提供硅类活性物质复合物。在通过使用前述的含氧液相溶剂来制备硅的粒子的浆料之后,若对上述浆料进行粉碎及磨碎工序,则可使粒子细粒化且增加应力的灵敏度,从而可向硅的粒子诱导化学氧化。
并且,还可进行在硅类活性物质复合物上形成导电层的工序(步骤S30)。在适合的溶剂中与粘结剂一同制备分散有导电材料的溶液,使在上述溶液内的上述硅类活性物质复合物得到分散,从而在获得上述溶液后进行干燥,由此可提供于上述导电层。并且,在将聚丙烯腈(PAN)、聚乙烯(PE)、聚丙烯酸(PAA)或聚乙烯吡咯烷酮(PVP)等高分子前体物质溶解在适合的溶剂后,将硅类活性物质复合物分散于上述溶剂中,来获得被上述高分子前体物质润湿的中间粒子,对上述中间粒子进行干燥及低温热处理,也可由此获得上述导电层。
如上所述的本发明并不局限于前述的实施例及附图,在不脱离本发明的技术思想范围的情况下,可进行多种替换、变形及变更,这对于本发明所属技术领域的普通技术人员而言是非常明确的。
Claims (5)
1.一种硅类活性物质复合物,其特征在于,包含:
由一次粒子凝集而成的二次粒子,
所述一次粒子具有硅的芯部及硅氧化物壳,所述硅氧化物壳是由所述硅的至少一部分氧化而成,
相对于所述硅类活性物质复合物的所述硅及所述硅氧化物的总重量,氧的含量为10%至20%重量百分比之间,
其中所述硅的芯部为非晶质或具有低结晶度,
其中所述一次粒子的平均直径在30nm至300nm的范围内,
其中所述一次粒子是由以下的制备方法所制备,包括:
提供硅的粒子的步骤;以及
通过对所述硅的粒子进行氧化,来形成包含具有硅的芯部及硅氧化物壳的一次粒子的步骤;所述硅氧化物壳是由所述硅的一部分氧化而成;
在对所述硅的粒子进行氧化的步骤中,在含氧液相溶剂内,以化学氧化的方式对所述硅的粒子进行氧化;
所述硅的粒子包含通过对硅的粗颗粒进行粉碎或磨碎的工序获得的精细粒子;
所述粉碎或磨碎的工序是对含有硅的粗颗粒及含氧液相溶剂的浆料进行,同时借助从所述粉碎或磨碎工序诱导出的压缩以及剪应力中的至少一种来使所述硅的粒子化学氧化。
2.根据权利要求1所述的硅类活性物质复合物,其特征在于,所述硅氧化物壳的厚度在2nm至30nm的范围内。
3.根据权利要求1所述的硅类活性物质复合物,其特征在于,所述硅氧化物壳的厚度在3nm至15nm的范围内。
4.根据权利要求1所述的硅类活性物质复合物,其特征在于,所述一次粒子的平均直径在30nm至200nm的范围内。
5.根据权利要求1所述的硅类活性物质复合物,其特征在于,在所述一次粒子的外围形成有用于使相接触的所述一次粒子之间电连接的碳类导电层。
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