CN1309102C - 锂聚合物电池的电池隔板 - Google Patents
锂聚合物电池的电池隔板 Download PDFInfo
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Classifications
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Abstract
披露了一种锂聚合物电池的电池隔板。该隔板有微孔膜和在它上面的涂覆层。该涂覆层是由形成凝胶的聚合物、第一溶剂和第二溶剂的混合物制备的。第一溶剂比第二溶剂更易挥发。第二溶剂是作为形成凝胶的聚合物的孔形成剂。
Description
发明的领域
本发明涉及锂聚合物电池或锂“凝胶”电池的电池隔板。
发明的背景
锂聚合物电池或锂凝胶电池是已熟知的,例如,见美国专利公布号2002/0168564A1,这里列为参考。这些锂聚合物电池与锂离子二次电池不同,两个大的差别是:使用凝胶电解质而不是使用液体电解质,常用的电池构件包含在柔韧性的封装中而不是这些构件包含于刚硬的罐形物(钮扣形或圆筒形或棱柱形)内。
起始时,聚合物电池的研制者们希望使用凝胶电解质作隔板。那就是用凝胶电解质来分离阳极与阴极。但这种方案至少由于两方面的原因而被抛弃。首先,凝胶电解质不能提供任何的断路能力,即降低了灾难性短路发生的安全性能。其次,在电池制造过程中柔软的凝胶电解质难以操作。电池通常是在其构件传动带的连续作业中制作的,而凝胶物传动带因没有足够的机械强度而难以承受制造过程中的酷烈的操作行为。
当今,凝胶电解质隔板被涂覆有凝胶聚合物而随后用液体电解质浸渍的微孔膜所取代。膜的包含克服了使用凝胶电解质时的前述问题。膜可提供断路本领和具有能承受电池制造过程中的酷烈的操作行为的机械强度。示范性的涂覆隔板在美国专利号5,639,573;5,681,357;5,688,293;5,750,284;5,837,015;5,853,916;6,322,923;6,328,770;6,337,101;美国专利公布号2002/0168564;WO99/54953;WO01/39296和WO01/39297中有所叙述,在此每个都作为参考。
在美国专利号6,322,923和美国专利公布号2002/0168564中,隔板包括有涂层的微孔膜。涂层是由形成凝胶的聚合物、增塑剂和溶剂的混合物制作的。溶剂溶解形成凝胶的聚合物和增塑剂,以便该混合物容易和均匀地施涂于膜上。溶剂也比其他组分较易挥发,以利于它易被驱除。涂覆隔板的剩留物(即包含形成凝胶的聚合物与增塑剂的涂覆物)不是多孔的,而在它成为多孔前是不易被电解液浸渍的。增塑剂是孔形成剂。为了形成孔必须将增塑剂如酯基质的邻苯二甲酸酯或有机碳酸酯抽提出去。这个抽提步骤增加了隔板的成本。
因此,在使用锂聚合物电池时,需求有一种较少昂贵的涂覆隔板。
发明的概要
披露了锂电池的一种电池隔板。该隔板有微孔膜和膜上有涂覆层。涂覆层是由形成凝胶的聚合物、第一溶剂与第二溶剂的混合物制作的。第一溶剂比第二溶剂更有挥发性。第二溶剂作为形成凝胶的聚合物的孔形成剂。
发明的细述
通常,电池包括阳极、阴极、隔板和电解质。阳极与阴极间插入隔板。电解质存在于隔板中,并与阳极和阴极有电化学联系。然后这些组分被封装于一外壳内。电池的这些组件是通用的与众所周知的。例如见:D.Linden,
电池手册,第二版,McGraw Hill出版社,纽约,NY(1995)和J.O.Besenhard,
电池材料手册,Wiley-VCH出版社,纽约,NY(1999)。
锂聚合物(或凝胶)电池是熟知的。见Linden,同上,36.37-36.42页,Besenhard,同上,513-517页,美国专利号5,418,091;5,456,000;和5,460,904,这里的每个可列参考。微孔膜作为聚合物电池隔板的部件的应用也是熟知的。见美国专利号5,518,838;5,604,660;5,631,103;5,639,573;5,681,357;5,688,293;5,750,284;5,837,015;5,853,916;5,658,685;5,849,433;5,665,265;5,716,421;5,834,135;6,322,923;6,328,770;6,337,101;美国专利公布号2002/0168564A1;WO 99/54953;WO 01/39297;WO 01/39296;A.Gozdz,“具有粘接的微孔隔板的塑性锂离子(PLIONTM)再充电式电池”,
Telecordia报告,2000年4月;和A.Gozdz等,“具有粘接的未处理微孔聚烯烃隔板的塑性锂离子电池的制造与使用特性”,
电化学协会198次会议,2000年10月22-27日;其中每个作为参考。
凝胶聚合物电池的隔板是一种有涂层的微孔膜,该涂层将在以下微孔膜的讨论中作详细论述。
微孔膜指的是任一种适当的微孔膜,该膜可以是对称的膜或不对称的膜,可由聚烯烃制备这种膜。示例性的聚烯烃包括但不限于聚乙烯(PE,包括LDPE,LLDPE,HDPE),超高分子量的聚乙烯(UHMWPE),聚丙烯(PP),聚甲基戊烯(PMP),上述物质的任一种的共聚物,及它们的混合物。该膜可由干拉伸法(也叫CELGARD法)或溶剂抽提法(也叫凝胶挤压法或相分离法或转相法)制备。膜可具有以下特性:透气度(Gurlely)不大于300sec/100cc(优选≤200sec/100cc,更优选≤150sec/100cc);厚度范围在5至500微米(μ)(优选10至100μ,更优选10至50μ);孔径范围在0.01至10微米(μ)(优选0.02至5μ,更优选0.02至0.5μ);孔隙率范围在35至85%(优选40至80%)。膜可是单层膜,三层膜(如PP/PE/PP或PE/PP/PE),或多层膜。膜优选断路隔膜,例如见美国专利号4,650,730;4,731,304;5,281,491;5,240,655;5,565,281;5,667,911;5,952,120;日本专利号2642206;和日本专利申请号98395/1994(提交于1994年5月12日);7/56320(提交于1995年3月15日);和UK专利申请号9604055.5(提交于1996年2月27日);所有这些在这里作为参考。合适的膜可从美国北卡罗莱纳州Charlotte的Celgard公司;日本东京的Asahi化学工业有限公司;日本东京的Tonen公司;日本东京的Ube工业公司;日本大坂的Nitto Denko KK;和由美国的俄勒冈州的Lebanon的Entek国际公司购得。
涂层至少是施涂于膜的一个外表面。优选的是涂层施涂于膜的两个外表面。优选的涂层基本上是(如≤25%,按体积)不渗入膜孔,更为优选的是不渗入膜孔。涂层的表面密度,仅基于形成凝胶聚合物而言,它的范围在0.12mg/cm2至0.7mg/cm2,优选在0.15mg/cm2至0.3mg/cm2,最为优选在约0.25mg/cm2。涂层应期望能有利于层状结构即阳极/隔板/阴极结构的粘接。另外,涂层有助于保持液体电解质于层状结构内,因而减低了电解质渗漏的危险。
涂层是作为形成凝胶的聚合物、第一溶剂和第二溶剂的混合物而施涂于膜上。下面详述的形成凝胶的聚合物有利于膜与电极的粘接和保持电解质于层状结构中。溶剂,即第一溶剂与第二溶剂,优选是在15℃或以下温度时至少有760毫米汞柱蒸气压的有机液。下面详述的第一溶剂用于溶解形成凝胶的聚合物和第二溶剂。第一溶剂使形成凝胶的聚合物和第二溶剂能完全混合,因而利于混合物均匀涂敷在膜的表面上:第一溶剂应能至少形成20%的其他组分的溶液。第一溶剂也容易从混合物中驱除出去。第一溶剂的沸点优选≤90℃。易于驱除优选意指少用或不用干燥用能源(如加热)溶剂便可蒸发。下面详述的第二溶剂也称为形成凝胶聚合物的孔形成剂;它与第一溶剂相比是一种较弱的溶剂或非溶剂;它可溶胀形成凝胶的聚合物,但不必完全溶解形成凝胶的聚合物。第一溶剂自混合物中驱除后,剩下的组分在膜表面形成无孔的涂层。当第二溶剂从涂层驱除时,在膜表面产生了形成凝胶聚合物的有孔涂层。第二溶剂比第一溶剂的挥发性低(即它不是如同第一溶剂那样容易驱除),以致第一溶剂去除时它仍剩留(或明显剩留)。优选好是第二溶剂的沸点比第一溶剂高约20℃或20℃以上,比第一溶剂的沸点高约30℃或30℃以上将更优选。优选第二溶剂的沸点不高于约150℃。可用干燥用能源(如加热)驱除第二溶剂。
形成凝胶的聚合物可选自但不限于聚偏氟乙烯(PVDF);聚氨基甲酸酯。聚环氧乙烷(PEO),聚环氧丙烷(PPO);聚丙烯腈(PAN),聚丙烯酰胺,聚丙烯酸甲酯,聚甲基丙烯酸甲酯,聚乙酸乙烯酯,聚乙烯基吡咯烷酮,聚二丙烯酸四甘醇酯;上述物质的共聚物,和它们的组合物。共聚用单体的一个选择标准是共聚用单体调整均聚物表面能的能力。表面能至少影响:共聚物溶解度,因而影响在膜上共聚物的涂覆;共聚物对膜的粘附,因而影响电池的制造与相应的使用性能;涂层的湿润性,因而影响液体电解质在隔板中的吸收。适宜的共聚用单体包括但不限于六氟丙烯(HFP),八氟-1-丁烷,八氟异丁烷,和四氟乙烯。共聚用单体含量优选范围按重量计在3至20%,优选7至15%。形成凝胶的聚合物优选的是聚偏氟乙烯的共聚物。优选的PVDF共聚物是聚偏氟乙烯与六氟丙烯的共聚物(PVDF∶HFP),最为优选的是重量比为91∶9的PVDF∶HFP。可从美国宾夕法尼亚州的费城的Atochem,比利时布鲁塞尔的Solvay SA和日本的Ibaraki市的Kureha化学工业有限公司购得PVDF聚合物与共聚物。优选的PVDF∶HFP共聚物是Atochem的KYNAR 2800。
第一溶剂可选自但不限于四氢呋喃,甲基乙基酮,丙酮,低分子量的甘醇二甲醚及它们的组合物。第一溶剂是形成涂层的混合物的主要组分。该混合物是稀溶液,其中第一溶剂按混合物重量计占80-99%,优选85-95%,更优选86-88%。优选的第一溶剂是丙酮。
第二溶剂是形成凝胶的聚合物的孔形成剂。第一溶剂比第二溶剂更具有挥发性(即在同一温度下第二溶剂比第一溶剂有较低的蒸气压)。第二溶剂可选自但并不限于丙醇,异丙醇,丁醇,和它们的混合物。除第二溶剂外还可加一些水。形成凝胶的聚合物对第二溶剂的重量比可以是1∶0.5至1∶4,优选在1∶2至1∶3范围。若水加入于第二溶剂,水对第二溶剂之比在0.25∶1至2∶1范围,优选0.5∶1。第二溶剂不是增塑剂。例如增塑剂是邻苯二甲酸酯为基质的酯,环碳酸酯,聚碳酸酯和它们的混合物。邻苯二甲酸酯为基质的酯选自但不限于邻苯二甲酸二丁酯。环碳酸酯选自但不限于碳酸亚乙酯(EC),碳酸亚丙酯(PC),碳酸亚丁酯(BC)和它们的混合物。聚碳酸酯选自但不限于聚碳酸亚乙烯基酯和线形聚碳酸亚丙基酯。
在制作上述涂覆的隔板时制备混合物。混合物可用任一种常规方法如涂覆、浸渍,喷雾涂覆于膜上。优选用浸涂法在膜双面涂覆混合物。优选不用加热使第一溶剂蒸发。此后,第二溶剂优选在烘箱中加热蒸发。对电池的制造商来说,涂覆隔板电阻的均一性是头等重要的事。用McMullin(麦克米伦)数来量度的电阻均一性取决于涂覆过程中控制的相对湿度(%RH)。已确定当%RH在45%以下,优选15-45%和更优选38-44%时,McMullin数(见美国专利号4,464,238对McMullin数的讨论,在此供作参考)可控制在5-12,优选5-6并有约0.25mg/cm2的涂覆密度。
制造具有上述隔板的锂聚合物电池时,在阳极与阴极间的上述隔板层压之前,隔板应当用溶剂和/或增塑剂处理以塑化(或软化)涂覆物,因而当它们叠合在一起时隔板能和电极粘接。通常使用压料辊加压并加热可实现层压。该处理优选是含有增塑剂与溶剂的溶液。这种溶液优选含有10至30%更为优选15至20%重量增塑剂的溶液。增塑剂包括碳酸亚烃酯,邻苯二甲酸二烷基酯,琥珀酸二烷基酯,已二酸二烷基酯,癸二酸二烷基酯,磷酸三烷基酯,聚亚烷基二醇醚,和它们的混合物。溶剂包括低级醇、酮、酯、脂肪烃,卤化溶剂,氯化烃,氯化的氟代烃,和它们的混合物。可用通常的涂覆、浸渍或喷雾的任一种方法施涂溶液。
上述内容将参照以下实例作进一步叙述。
实例
在以下的实例中,混合物包括280-285磅(127-130公斤)丙酮;8.5磅(3.8公斤)PVDF∶HFP共聚物(Kynar FLEX2800,购自Atofina化学品公司,费城,PA);22.7磅(10.3公斤)异丙醇;和11.3磅(5.1公斤)水。用浸涂法在双面施涂混合物。上面的施涂物约控制在0.25mg/cm2。令丙酮蒸发。异丙醇/水在烘箱中蒸发去除。在涂覆与干燥阶段中,已确定相对湿度控制在15-44%时可改善隔板的均一性(由McMullin数量度)
序号 | 实际的相对湿度% | McMullin数 | 施涂的涂覆物mg/cm2 |
1 | 17 | 14.3 | - |
2 | 17 | 18.9 | - |
3 | 8 | 6.8 | 0.24 |
4 | 9 | 23.9 | 0.20 |
5 | 10 | 7.5 | 0.23 |
6 | 9 | 17.1 | 0.47 |
7 | 9 | 9.5 | 0.25 |
8 | 9 | 10.1 | 0.28 |
9 | 10 | 14.5 | 0.24 |
10 | 41 | 8.1 | 0.23 |
11 | 42 | 6.5 | 0.23 |
12 | 42 | 6.6 | 0.24 |
13 | 9 | 15.0 | 0.23 |
14 | 9 | na | - |
15 | 10 | 10.5 | 0.22 |
16 | 9 | 11.0 | 0.22 |
17 | 9 | 12.6 | 0.23 |
18 | 10 | 14.5 | 0.21 |
19 | 13 | 12.6 | 0.21 |
20 | 44 | 6.8 | 0.27 |
21 | 49 | 8.5 | 0.28 |
22 | 54 | 8.1 | 0.27 |
23 | 49 | 11.2 | 0.27 |
24 | 54 | 8.4 | 0.29 |
25 | 52 | na | 0.24 |
26 | 45 | na | 0.25 |
27 | 48 | 9.1 | 0.22 |
28 | 45 | 5.5 | 0.23 |
29 | 44 | 10.7 | 0.23 |
30 | 54 | 10.3 | 0.23 |
31 | 48 | 12.2 | 0.24 |
32 | 45 | 11.7 | 0.22 |
33 | na | 11.4 | 0.23 |
34 | 41 | 6.0 | na |
35 | 41 | 5.8 | na |
36 | 42 | 5.9 | na |
37 | 42 | 5.9 | na |
na=未得到数据
在不违背本发明的精神与主要性质的条件下,本发明可采用其它的方式实施,相应地,本发明范围应当参照所附的权限而不是上述说明书。
Claims (28)
1.锂电池的电池隔板,包括
微孔膜,和
微孔膜上面的涂层,所述的涂层是由包含有形成凝胶的聚合物、第一溶剂和第二溶剂的混合物制备的,第一溶剂比第二溶剂更易挥发,和所述的第二溶剂适合于在形成凝胶的聚合物中生成孔,并且水加入所述的第二溶剂中,并且所述涂层在相对湿度在45%以下涂覆,
从而电池隔板的麦克米伦数控制在5-12。
2.权利要求1的电池隔板,其中所述的形成凝胶的聚合物选自聚偏氟乙烯,聚氨基甲酸酯,聚环氧乙烷,聚环氧丙烷,聚丙烯腈,聚丙烯酰胺,聚丙烯酸甲酯,聚甲基丙烯酸甲酯,聚乙酸乙烯酯,聚乙烯基吡咯烷酮,聚二丙烯酸四甘醇酯,上述物质的共聚物,和它们的混合物。
3.权利要求2的电池隔板,其中所述的凝胶聚合物是聚偏氟乙烯:六氟丙烯的共聚物。
4.权利要求1的电池隔板,其中所述的第一溶剂选自四氢呋喃,甲基乙基酮,丙酮,低分子量的甘醇二甲醚,和它们的混合物。
5.权利要求1的电池隔板,其中所述的第二溶剂选自丁醇,丙醇,异丙醇,和它们的混合物。
6.锂聚合物电池,包括
阳极,
阴极,和
夹持在所述的阳极与所述的阴极之间的隔板,所述的隔板包括微孔膜和它上面的涂层,所述的涂层是由包含形成凝胶的聚合物、第一溶剂和第二溶剂的混合物制备的,第一溶剂比第二溶剂更易挥发,和所述的第二溶剂适合于在形成凝胶的聚合物中生成孔,并且水加入所述的第二溶剂中,并且所述涂层在相对湿度在45%以下涂覆,
从而电池隔板的麦克米伦数控制在5-12。
7.权利要求6的锂聚合物电池,还包含浸渍在所述隔板中的和与所述阳极与所述阴极保持电化学联系的电解质。
8.权利要求6的锂聚合物电池,其中所述的形成凝胶的聚合物选自聚偏氟乙烯,聚氨基甲酸酯,聚环氧乙烷,聚环氧丙烷,聚丙烯腈,聚丙烯酰胺,聚丙烯酸甲酯,聚甲基丙烯酸甲酯,聚乙酸乙烯酯,聚乙烯基吡咯烷酮,聚二丙烯酸四甘醇酯,上述物质的共聚物,和它们的混合物。
9.权利要求8的锂聚合物电池,其中所述的形成凝胶的聚合物是聚偏氟乙烯:六氟丙烯的共聚物。
10.权利要求6的锂聚合物电池,其中所述的第一溶剂选自四氢呋喃,甲基乙基酮,丙酮,低分子量的甘醇二甲醚,和它们的混合物。
11.权利要求6的锂聚合物电池,其中所述的第二溶剂选自丁醇,丙醇,异丙醇,和它们的混合物。
12.制备锂聚合物电池的电池隔板的方法,包括以下步聚:
提供微孔膜,
提供形成凝胶的聚合物、第一溶剂和第二溶剂的混合物,第一溶剂比第二溶剂更易挥发,第二溶剂适合于在形成凝胶的聚合物中生成孔,并且水加入所述的第二溶剂中,
涂覆该混合物至微孔膜的至少一面上,
驱除第一溶剂,由此形成涂覆有形成凝胶的聚合物和形成孔的第二溶剂的非孔涂层的微孔膜,和
驱除第二溶剂,由此形成了由形成凝胶的聚合物的多孔涂层涂覆的微孔膜。
13.权利要求12的方法,其中的涂覆方法包括浸涂。
14.权利要求12的方法,基中驱除第二溶剂的步骤包括加热。
15.权利要求12的方法,其中所述的形成凝胶的聚合物选自聚偏氟乙烯,聚氨基甲酸酯,聚环氧乙烷,聚环氧丙烷,聚丙烯腈,聚丙烯酰胺,聚丙烯酸甲酯,聚甲基丙烯酸甲酯,聚乙酸乙烯酯,聚乙烯基吡咯烷酮,聚二丙烯酸四甘醇酯,上述物质的共聚物,和它们的混合物。
16.权利要求12的方法,其中所述的形成凝胶的聚合物是聚偏氟乙烯:六氟丙烯的共聚物。
17.权利要求12的方法,其中所述的第一溶剂选自四氢呋喃,甲基乙基酮,丙酮,低分子量的甘醇二甲醚,和它们的混合物。
18.权利要求12的方法,其中所述的第二溶剂选自丁醇,丙醇,异丙醇,和它们的混合物。
19.权利要求12的方法,其中在所述混合物的涂覆过程中控制相对湿度为45%以下。
20.形成锂聚合物电池的方法,包括以下步骤:
提供阳极,
提供阴极,
提供隔板,所述的隔板包括微孔膜和它上面的涂层,所述的涂层是由包括形成凝胶的聚合物、第一溶剂和第二溶剂的混合物制备的,第一溶剂比第二溶剂更易挥发,和第二溶剂适合于在形成凝胶的聚合物中生成孔,并且水加入所述的第二溶剂中,
用形成凝胶的聚合物用的增塑剂在用于该增塑剂的溶剂中的溶液处理隔板,
驱除增塑剂用的溶剂,
把经处理的隔板夹放在阳极与阴极之间,
和将阳极与阴极粘接到隔板上。
21.权利要求20的方法,其中的处理包括在所述的溶液中浸渍隔板。
22.权利要求20的方法,其中驱除增塑剂用的溶剂包括蒸发该溶剂。
23.权利要求20的方法,其中的粘接包括用加热与加压的层压方法。
24.权利要求20的方法,其中形成凝胶的聚合物选自聚偏氟乙烯,聚氨基甲酸酯,聚环氧乙烷,聚环氧丙烷,聚丙烯腈,聚丙烯酰胺,聚丙烯酸甲酯,聚甲基丙烯酸甲酯,聚乙酸乙烯酯,聚乙烯基吡咯烷酮,聚二丙烯酸四甘醇酯,上述物质的共聚物,和它们的混合物。
25.权利要求24的方法,其中所述的形成凝胶的聚合物是聚偏氟乙烯:六氟丙烯的共聚物。
26.权利要求20的方法,其中的第一溶剂选自四氢呋喃,甲基乙基酮,丙酮,低分子量的甘醇二甲醚,和它们的混合物。
27.权利要求20的方法,其中的第二溶剂选自丁醇,丙醇,异丙醇,和它们的混合物。
28.权利要求20的方法,其中在所述混合物的涂覆过程中控制相对湿度为45%以下。
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US10/446,380 US20040241550A1 (en) | 2003-05-28 | 2003-05-28 | Battery separator for lithium polymer battery |
US10/446,380 | 2003-05-28 |
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EP (1) | EP1482578A1 (zh) |
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KR (1) | KR100628606B1 (zh) |
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CN1574419A (zh) | 2005-02-02 |
SG115647A1 (en) | 2005-10-28 |
US20070134548A1 (en) | 2007-06-14 |
EP1482578A1 (en) | 2004-12-01 |
JP2011119276A (ja) | 2011-06-16 |
US20040241550A1 (en) | 2004-12-02 |
TWI299587B (en) | 2008-08-01 |
CA2462294A1 (en) | 2004-11-28 |
JP5309171B2 (ja) | 2013-10-09 |
JP2004356102A (ja) | 2004-12-16 |
KR100628606B1 (ko) | 2006-09-26 |
US7794511B2 (en) | 2010-09-14 |
TW200427122A (en) | 2004-12-01 |
KR20040103310A (ko) | 2004-12-08 |
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