CN101341612A - 适用于锂离子电池的电极的含硅合金 - Google Patents

适用于锂离子电池的电极的含硅合金 Download PDF

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CN101341612A
CN101341612A CNA2006800477739A CN200680047773A CN101341612A CN 101341612 A CN101341612 A CN 101341612A CN A2006800477739 A CNA2006800477739 A CN A2006800477739A CN 200680047773 A CN200680047773 A CN 200680047773A CN 101341612 A CN101341612 A CN 101341612A
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黎丁巴
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Abstract

用于锂离子电池的电极组合物，如式SixSnqMyCz所示，其中q、x、y和z代表原子百分比值，并且(a)(q+x)＞2y+z；(b)q≥0，(c)z≥0；和(d)M为选自锰、钼、铌、钨、钽、铁、铜、钛、钒、铬、镍、钴、锆、钇或其组合的一种或多种金属。Si、Sn、M和C元素的配置形式为多相的微结构，包括：(a)包含的非晶相；(b)包含金属硅化物的纳米晶相；和(c))z＞0时，含碳化硅相的相；及(d))q＞0时，含Sn的非晶相。

Description

适用于锂离子电池的电极的含硅合金
相关申请的交叉引用
本申请要求2005年12月23日提交的美国申请60/743,075的优先权，该文献的公开内容全文以引用方式并入本文。
技术领域
本发明涉及适用于锂离子电池的电极组合物、这种组合物的制备方法以及包括这种组合物的电池。
背景技术
已经建议将金属合金作为锂离子电池的阳极。相对于诸如石墨的插层式阳极来说，这些合金型阳极通常显示出更高的容量。然而，这种合金的一个问题在于，它们常常显示出相对较差的循环寿命和较差的库仑效率，这是由于在与合金中的组合物变化相关的膨胀和收缩期间合金粒子破碎的缘故。
发明内容
本文描述一种用于锂离子电池的电极组合物，如式SixSnqMyCz所示，其中q、x、y和z代表原子百分比值，并且(a)(q+x)＞2y+z；(b)x＞0，(c)q和z各自独立地≥0；及(d)M为选自锰、钼、铌、钨、钽、铁、铜、钛、钒、铬、镍、钴、锆、钇及其组合的一种或多种金属。Si、Sn、M和C元素的配置形式为多相的微结构，包括：(a)包含硅的非晶相；(b)包含金属硅化物的纳米晶相；和(c)z＞0时，含碳化硅的相；及(d)q＞0时，含Sn的非晶相。
“非晶相”是一种缺乏长程原子秩序且其X射线衍射图缺乏尖锐、明确界定峰的相。
“纳米晶相”是晶粒不大于约50纳米的相，该相显示有长程原子秩序，并且X射线衍射图以尖锐、明确界定的峰为特征。
在一些实施例中，可以选择x值，使x≥60，并且可以选择z值，使z＞0、z≥10或z≥15。例如，在一个实施例中，x≥60、≥70或甚至更大，z＞0或≥10，M为选自钴、镍、铁、钛、钼及其组合的一种或多种金属。在另一实施例中，M包括Co，x≥60，z＞0。
可以将该电极组合物用于锂离子电池的阳极，所述锂离子电池还包括阴极和电解质。电解质可以包括任何已知的电解质，如氟代碳酸亚乙酯。优选的是，阳极的形式为包括电极组合物与粘结剂(任何已知的粘结剂，例如聚酰亚胺)和导电稀释剂(任何已知的导电稀释剂，如炭黑)组合的复合体。
当结合到锂离子电池中时，电极显示出良好的循环寿命和库仑效率。
下文的附图和描述中给出了本发明的一个或多个实施例的详情。从详细描述以及从权利要求中可以显而易见本发明的其它特征、目的及优点。
具体实施方式
本文的所有数字均可以被术语“约”修饰。用端点列举的数值范围可包括包含在该范围内的所有数字(如，1至5包含1、1.5、2、2.75、3、3.80、4、和5)。
所描述的电极组合物特别适合用于锂离子电池的阳极。该电极组合物的特征在于，用于锂离子电池的电极组合物如式SixSnqMyCz所示，其中q、x、y和z代表原子百分比值，并且(a)(q+x)＞2y+z；(b)q≥0，(c)z≥0；及(d)M为选自锰、钼、铌、钨、钽、铁、铜、钛、钒、铬、镍、钴、锆、钇及其组合的一种或多种金属。Si、Sn、M和C元素的配置形式为多相的微结构，包括：(a)包含硅的非晶相(因此x＞0)；(b)包含金属硅化物的纳米晶相；和(c)z＞0时，含碳化硅的相；及(d)q＞0时包含Sn的非晶相。优选的是，通过在高速剪切及高速冲击下将硅、(各种)金属和使用碳的实施例中的碳源(例如石墨)球磨适当的一段时间来制备电极组合物。可以使用球磨机，例如立式球磨机(ATTRITOR，Union Process Inc.，Akron，OH)、SPEXMILL(Spex CertiPrep，Metuchen，NJ)、卧式旋转球磨机(SIMOLOYER，ZozgmbH，Werden，Germany)或本领域中已知的其它球磨机。
该电极组合物特别适合用于锂离子电池的阳极。阳极优选为复合体，其中电极组合物与粘结剂和导电稀释剂结合。合适粘结剂的例子包括聚酰亚胺和聚偏二氟乙烯。合适的导电稀释剂的例子包括炭黑。
为制备电池，需将阳极与电解质和阴极(对电极)结合。电解质的形式可以为液体、固体或凝胶。固体电解质的例子包括聚合物电解质，例如聚环氧乙烷、含氟聚合物和共聚物(例如，聚四氟乙烯)及其组合。液体电解质的例子包括碳酸亚乙酯、碳酸二乙酯、碳酸亚丙酯、氟代碳酸亚乙酯(FEC)及其组合。向电解质提供锂电解质盐。合适的盐的例子包括LiPF6、LiBF4、双(乙二酸)硼酸锂、LiN(CF3SO2)2、LiN(C2F5SO2)2、LiAsF6、LiC(CF3SO2)3和LiClO4。合适的阴极组合物的例子包括LiCoO2、LiCo0.2Ni0.8O2和LiMn2O4。另外的例子包括在下列文献中描述的阴极组合物：(1)Lu等人，美国专利No.6,964,828；(2)Lu等人，美国专利No.7,078,128；(3)Le，美国专利申请公开2004/0121234；(4)Dahn等人，美国专利申请公开No.2003/0108793；(5)Eberman等人，美国专利申请公开No.2005/0112054；(6)Dahn等人，美国专利申请公开No.2004/0179993；(7)Obrovac等人，美国专利No.6,680,145；和(8)Dahn等人，美国专利No.5,900,385。
实例
硅、铁、镍、钛、钴和锡是从Alfa Aesar，Ward Hill，MA；AldrichChemical Company，Milwaukee，WI或Alcan Metal Powders，Berkeley，CA获得的。
使用配备了铜靶X射线管及衍射光束单色器的Siemens ModelKristalloflex 805D500衍射仪收集X射线衍射图。表1A和1B中标有“由X射线数据观测到的相”的一栏中给出的数据是基于每个列举的合金样品所得到的特征峰形。例如，当X射线衍射图上没有或缺乏尖锐、明确界定峰时认为是非晶相。由Scherer方程确定晶相的晶粒尺寸。当计算的晶粒尺寸小于50纳米时认为是纳米晶相。
在氩气氛下使用SPEX MILL(型号8000-D，Spex CertiPrep，Metuchen，NJ)，在45毫升碳化钨容器中用28个碳化钨球(每个5/16英寸，大约108克)将所标定量的硅片(Alfa Aesar，编号00311)、(各种)金属和石墨粉(MCMB-1028，MMM Carob，Belgium)碾磨4小时，由此制备表1A中列举的样品1-14。然后打开容器，打碎大块的粉团，在氩气氛下继续再碾磨一个小时。通过空气冷却将碳化钨容器的温度保持在约30℃。
通过与实例1-14相同的一般步骤制备表1A中列举的实例15-16样品，但有以下不同。使用硅粉(325目；Alfa Aesar，编号，35662)、锡粉(＜10微米，Aldrich，编号520373)和金属粉末(钴，1.6微米；Alfa Aesar，编号10455C Alfa Aesar；镍，Alcan Metal Powder，型号123)。在氩气氛下在SPEX MILL中用14个碳化钨球(直径0.415毫米；总重量大约54克)将实例15和16样品碾磨16小时。通过空气冷却将碳化钨容器的温度保持在约30℃。
将每个在表1A中列举的实例1-16样品形成为电极，并在具有锂金属对电极的电化学电池中进行表征。按以下的步骤制备电极。在45毫升不锈钢容器中使用四个碳化钨球(直径12.75mm)将量为1.8g的碾磨材料、0.06g导电碳(SUPER P，MMM Carbon，Belgium)和0.70g的PI2555(PYRALIN PI2555，在N-甲基-2-吡咯烷酮中的20重量百分比的溶液，得自HD Microsystems，Cheesequake Road，Parlin，NJ)混合。在行星式微碾磨机(PULVERISETTE 7，得自FritschgmbH，Idon-Oberstein，Germany)中以3档的速度设置进行混合2小时。然后使用带有0.0075英寸(76.2微米)间隙的槽口棒涂覆模头将得到的溶液涂布到13微米厚的铜箔上。将涂层在150℃下于真空炉中干燥2小时，然后用来构造2325型硬币式电池，所述电池包括380微米厚的锂金属箔对电极、两层平片聚丙烯膜隔板(CELGARD 2400，得自CELGARD Inc.，Charlotte，NC)和电解质(混合物，包含90份的碳酸亚乙酯与碳酸二乙酯的1∶2体积混合物以及10份得自SynQuest Laboratories of Alachua，Florida的氟代碳酸亚乙酯)中的1M LiPF6。使用前将该混合物用分子筛(3A型)干燥12小时。2325型硬币式电池的部件描述在A.M.Wilson和J.R.Dahn发表于J.Electrochem.Soc.，142，326-332(1995)的文章中。
使用电池测试器(Maccor Inc.，Tulsa OK)对由实例1-16制备的电化学电池在0.9V至5mV之间进行循环。在下次充电循环之前在较低的截止电压下使200mA/g的电流降至10mA/克。测得的充电效率和库仑效率值记录在表2中。
通过在ARC炉中熔化65.461克硅块(Alfa Aesar/99.999％，编号39101)、18.596克铁片(AlfaAesar/99.97％，编号10454)和15.943克海绵钛(Alfa Asear/99.7％，编号10582)制备实例17样品。将合金锭(Si70Fe10Ti10)破碎成小块，在锤磨机中进行处理，制成尺寸150微米的粉末。在SPEX MILL中的充氩的45毫升碳化钨容器(型号8001，Spex CertiPrep，Metuchen，NJ)中将Si70Fe10Ti10合金粉末(3.8462g)和石墨(0.1528g，SFG44/Tim Rex)与28个碳化钨球(每个10.5毫米，总重量108克)一起碾磨1小时。在碾磨期间喷射空气冷却容器。碾磨期间容器的温度约30℃。
通过如实例17那样在SPEX MILL中碾磨3.9409克按实例17步骤制得的Si70Fe10Ti10合金粉末和0.0591克石墨制备实例18样品。
通过与实例17中相同的步骤制备实例19样品，不同的是用64.605g硅块、27.528g铁片和7.867克海绵钛制备Si70Fe15Ti5合金粉末。然后如实例17那样在SPEX MILL中碾磨3.8481g的Si70Fe15Ti5合金粉末和0.1519克石墨。
通过如实例17那样在PSEX MILL中碾磨3.9417g按实例19步骤制得的Si70Fe15Ti5合金粉末和0.0583g石墨制备实例20样品。
将实例17-20的每个样品形成为电极，并在具有锂对电极的电化学电池中进行表征。按以下的步骤制备包含实例17-20样品的电极。在行星式微碾磨机中以1档的速度设置，使用四个碳化钨球(每个12.5毫米)将碾磨材料样品(1.84g)、导电碳(0.024g，Ketjen Black，AkzoNobel)和NMP(2g)在45毫升不锈钢容器里混合30分钟，然后加入PYRALIN PI2555(0.68g，在NMP中的20重量％PI2555固体)，以2档的速度设置混合1小时。使用设置有125微米间隙的槽口棒涂覆模头将得到的溶液涂布到13微米厚的铜箔上。将涂覆样品在150℃下于真空炉中干燥2小时。从涂层中冲压出圆板(直径16mm)。
在按照与实例1相同的方式装配的2325型硬币式电池中测试实例17-20中制备的涂层。除了采用250mA/克-合金的电流密度以及在每半个循环的末期采用15分钟的开路期之外，按实例1的方式对由实例17-20制备的硬币式电池进行循环。测得的充电效率和库仑效率值记录在表2中。
以反复循环的方式，在高速冲击的卧式碾磨机(Simoloyer，CM20-Solm，ZozgmbH)中在550rpm下用25kg铬钢球(5mm，100Cr6钢)将903.602g硅粉(-100+325目，Globe MetallurgicalInc.，Beverly，OH)、406.307g钴(纯度99.8％，1.6μm颗粒，得自Alfa Aesar，编号10455C)、134.885g镍粉(纯度99.9％，2-3μm颗粒，Alfa Aesar，编号10255)和55.206g石墨粉(Timrex SFG44，TimCal Ltd.，Bodio，Switzerland)碾磨45秒，再在300rpm下碾磨15秒，由此制备实例21的样品。实例21样品总共碾磨三个小时。按与实例21相同的步骤制备实例22和23样品，不同的是碾磨时间分别为5小时和7.5小时。
将每个实例21-23的样品形成为电极，如在实例17中那样用电化学电池进行表征，按与实例17中相同的步骤对电池进行循环。这些实例中的每个均包括含硅的非晶相。30次循环以后这些材料各自的比容量(mAh/g)为：实例21，1220；实例22，1050；实例23，920。
表1A：合金粉末的制备
  实例编号   化学计量式(原子百分比)   硅片(克)   金属(克)   碳或石墨(克)  由X射线数据观测到的相
  1   Si66Co22C12   2.813   Co，1.968   0.219  非晶Si非晶SiC，纳米晶CoSi2
  2   Si70Co20C10   3.011   Co，1.805   0.184  非晶Si非晶SiC纳米晶CoSi2
  3   Si73Co23C4   2.968   Co，1.962   0.070  非晶Si非晶SiC纳米晶CoSi2
  4   Si70Co15C15   3.244   Co，1.495   0.297  非晶Si非晶SiC纳米晶CoSi2
  5   Si70Ni20C10   3.015   Ni，1.800   0.184   非晶Si非晶SiC纳米晶NiSi2
  6   Si70Ni15C15   3.248   Ni，1.454   0.298   非晶Si非晶SiC纳米晶NiSi2
  7   Si70Fe15C15   3.294   Fe，1.404   0.302   非晶Si纳米晶FeSi2非晶SiC
  8   Si70Ti20C10   3.230   Ti，1.573   0.197   非晶Si非晶SiC纳米晶TiSi2
  9   Si70Mo15C15   2.742   Mo，2.007   0.251   非晶Si非晶SiC纳米晶MoSi2
  10   Si70Co15Ni5C10   3.012   Co，1.354Ni，0.4500   0.184   非晶Si，非晶NiSi2非晶SiC，纳米晶CoSi2
  11   Si70Co10Ni10C10   3.013   Co，0.903Ni，0.900   0.184   非晶Si非晶NiSi2非晶SiC纳米晶CoSi2
  12   Si70Co5Ni15C10   3.014   Co，0.452Ni，1.350   0.184   非晶Si非晶SiC纳米晶CoSi2纳米晶NiSi2
  13   Si70Fe5Ni10C15   3.263   Fe，0.464Ni，0.974   0.299   非晶Si非晶SiC非晶FeSi2纳米晶NiSi2
  14   Si70Co10Ni5C15   3.245   Co，0.973Ni，0.485   0.297   非晶Si非晶SiC非晶NiSi2，纳米晶CoSi2
  15   Si74Sn2Co24   1.672   Co，1.138Sn，0.191   0   非晶Si非晶Sn纳米晶CoSi2
  16   Si73Sn2Ni25   1.638   Ni，1.172Sn，0.190   0   非晶Si非晶Sn纳米晶NiSi2
表1B：合金粉末的制备
  实例编号   化学计量式(原子百分比)   由X射线数据观测到的相
  17   Si70Fe10Ti10C10   Si(晶粒尺寸～10-20nm)TiSi2(晶粒尺寸～10-20nm)FeSi2(晶粒尺寸～10-20nm)非晶FeSi2
  18   Si74.66Fe10.67Ti1067C4   Si(晶粒尺寸～10-20nm)TiSi2(晶粒尺寸～10-20nm)FeSi2(晶粒尺寸～10-20nm)非晶FeSi2
  19   Si70Fe15Ti5C10   Si(晶粒尺寸～10-20nm)TiSi2(晶粒尺寸～10-20nm)FeSi2(晶粒尺寸～10-20nm)非晶FeSi2
  20   Si74.67Fe16Ti5.33C4   Si(晶粒尺寸～10-20nm)TiSi2(晶粒尺寸～10-20nm)FeSi2(晶粒尺寸～10-20nm)非晶FeSi2
表2：电化学电池实例
  实例编号   40次循环后的容量mAh/克   库仑效率
  1   479   0.998
  2   718   0.994
  3   761   1.016
  4   896   0.997
  5   961   1.000
  6   1089   0.998
  7   758   0.998
  8   759   1.000
  9   607   0.998
  10   778   0.997
  11   814   0.997
  12   889   0.997
  13   903   0.992
  14   904   0.999
  15*   733   0.996
  16*   897   0.987
  17   1070   0.997
  18   1184   0.997
  19   890   0.997
  20   960   0.996
*实例15和16是在10次循环后测量的，不是40次后。
已经描述了本发明的多个实施例。不过应当理解的是，在不偏离本发明的精神和范围的情况下可以作出各种修改。因此，其它的实施例是在以下的权利要求范围之内的。

Claims (28)

1.一种用于锂离子电池的电极组合物，如式SixSnqMyCz所示，其中q、x、y和z代表原子百分比值，并且
(a)(q+x)＞2y+z；
(b)x大于0；
(c)q和z各自独立地大于或等于0；和
(d)M为选自锰、钼、铌、钨、钽、铁、铜、钛、钒、铬、镍、钴、锆、钇或其组合的一种或多种金属，
其中Si、Sn、M和C元素的配置形式为多相的微结构，包括：
(i)包含硅的非晶相；
(ii)包含金属硅化物的纳米晶相；
(iii)z＞0时，含碳化硅的相；和
(iv)q＞0时，含Sn的非晶相。
2.根据权利要求1所述的电极组合物，其中M为选自钴、镍、铁、钛、钼、钨或其组合的一种或多种金属。
3.根据权利要求1所述的电极组合物，其中x≥60。
4.根据权利要求1所述的电极组合物，其中z＞0。
5.根据权利要求1所述的电极组合物，其中z≥10。
6.根据权利要求1所述的电极组合物，其中z≥15。
7.根据权利要求1所述的电极组合物，其中x≥60，M为选自钴、镍、铁、钛、钼或其组合的一种或多种金属。
8.根据权利要求7所述的电极组合物，其中z＞0。
9.根据权利要求7所述的电极组合物，其中z≥10。
10.根据权利要求1所述的电极组合物，其中M包括Co。
11.根据权利要求10所述的电极组合物，其中z＞0。
12.根据权利要求10所述的电极组合物，其中x≥60。
13.一种锂离子电池，包括：
阳极；
阴极；和
电解质，
其中所述阳极包括如式SixSnqMyCz所示的组合物，其中q、x、y和z代表原子百分比值，并且
(a)(q+x)＞2y+z；
(b)q大于或等于0；
(c)z大于或等于0；并且
(d)M为选自锰、钼、铌、钨、钽、铁、铜、钛、钒、铬、镍、钴、锆、钇或其组合的一种或多种金属，
其中Si、Sn、M和C元素的配置形式为多相的微结构，包括：
(i)包含硅的非晶相；
(ii)包含金属硅化物的纳米晶相；
(iii)z＞0时，含碳化硅的相；和
(iv)q＞0时，含Sn的非晶相。
14.根据权利要求13所述的锂离子电池，其中M为选自钴、镍、铁、钛、钼、钨或其组合的一种或多种金属。
15.根据权利要求13所述的锂离子电池，其中x≥60。
16.根据权利要求13所述的锂离子电池，其中z＞0。
17.根据权利要求13所述的锂离子电池，其中z≥10。
18.根据权利要求13所述的锂离子电池，其中z≥15。
19.根据权利要求13所述的锂离子电池，其中x≥60，M为选自钴、镍、铁、钛、钼或其组合的一种或多种金属。
20.根据权利要求19所述的锂离子电池，其中z＞0。
21.根据权利要求19所述的锂离子电池，其中z≥10。
22.根据权利要求13所述的锂离子电池，其中M包括Co。
23.根据权利要求22所述的锂离子电池，其中z＞0。
24.根据权利要求22所述的锂离子电池，其中x≥60。
25.根据权利要求13所述的锂离子电池，其中所述阳极进一步包含粘结剂和导电稀释剂。
26.根据权利要求25所述的锂离子电池，其中所述粘结剂包括聚酰亚胺。
27.根据权利要求25所述的锂离子电池，其中所述导电稀释剂包括炭黑。
28.根据权利要求13所述的锂离子电池，其中所述电解质包括氟代碳酸亚乙酯。
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