CN110024192B - 储能器件用底涂层和储能器件电极用底涂箔 - Google Patents
储能器件用底涂层和储能器件电极用底涂箔 Download PDFInfo
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- CN110024192B CN110024192B CN201780073386.0A CN201780073386A CN110024192B CN 110024192 B CN110024192 B CN 110024192B CN 201780073386 A CN201780073386 A CN 201780073386A CN 110024192 B CN110024192 B CN 110024192B
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Abstract
厚度为1~200nm的储能器件用底涂层。具备该底涂层的底涂箔可有效率地进行超声波焊接,同时通过使用具有该底涂箔的电极,从而得到低电阻的储能器件。
Description
技术领域
本发明涉及储能器件用底涂层和储能器件电极用底涂箔。
背景技术
近年来,以锂离子二次电池、双电层电容器为首的储能器件为了应对电动汽车、电动设备等用途,需要高容量化和充放电的高速化。
作为用于满足该要求的一个对策,提出了在活性物质层与集电基板之间配置底涂层,使活性物质层和集电基板的粘接性变得牢固,同时降低它们的接触界面的电阻(例如参照专利文献1、2)。
一般地,在储能器件中,作为从正极和负极将电流取出的端子,分别在正极和负极将金属极片焊接。
通常将金属极片焊接于集电基板,即使是形成了底涂层的电极,也在集电基板上的没有形成底涂层和活性物质层的部位进行与金属极片的焊接(例如参照专利文献1)。
作为在形成了底涂层的集电基板上形成金属极片接合部位的方法,有在集电基板上的金属极片接合部位没有形成底涂层和活性物质层、将在集电基板上形成的底涂层和活性物质层部分地剥离等方法。
但是,在没有形成一部分底涂层的情况下,集电基板的通用性降低,必须准备各种电极各不相同的集电基板。另一方面,对于将暂时形成的底涂层等剥离的方法而言,由于增加一个工序,因此器件的生产率降低。
特别地,为了实现器件的高容量化,在将电极板多张重叠使用的情况下,与上述那样的集电基板露出部分的形成有关的问题变得更大。
从这样的观点出发,报道了如下技术:将集电基板与金属极片焊接时,在集电基板上形成底涂层且没有形成活性物质层的部分进行焊接(例如参照专利文献3)。
近来,随着对于电动汽车、电动设备等制品的针对安全性、生产率等的要求进一步提高,谋求与蓄电器件有关的技术的进一步的深化。
特别地,能够以更高的生产率制造更高安全性的蓄电器件的方法由于可直接地贡献于满足低价格且高安全性这样的近年来的市场需求的制品制造,因此在该技术领域中强烈地需要。
但是,根据本发明人的研究,在专利文献3涉及的制造方法中,即使在满足其条件的情况下,根据碳材料的种类,有时也不能再现性良好地进行超声波焊接。
现有技术文献
专利文献
专利文献1:日本特开2010-170965号公报
专利文献2:国际公开第2014/042080号
专利文献3:国际公开第2014/034113号
发明内容
发明要解决的课题
本发明鉴于上述实际情况而完成,目的在于提供可进行超声波焊接、同时给予低电阻的储能器件的储能器件电极用底涂层和具备其的储能器件用底涂箔。
用于解决课题的手段
本发明人从底涂层的焊接性和具备其的器件的低电阻化这样的观点出发反复认真研究,结果发现:通过使在集电基板的至少一面形成的底涂层的膜厚成为规定范围,从而在集电基板上形成了底涂层的部分可有效率地进行超声波焊接,同时发现即使在使用了具备具有该规定范围的膜厚的底涂层的底涂箔的电极的情况下,也得到低电阻的储能器件,完成了本发明。
即,本发明提供:
1.储能器件用底涂层,其特征在于,厚度为1~200nm;
2.1所述的储能器件用底涂层,其中,厚度为1~140nm;
3.2所述的储能器件用底涂层,其中,厚度为30~80nm;
4.1~3中任一项所述的储能器件用底涂层,其包含导电材料;
5.1~4中任一项所述的储能器件用底涂层,其中,所述导电材料包含选自炭黑、科琴黑、乙炔黑、碳晶须、碳纳米管、碳纤维、天然石墨、人造石墨、氧化钛、ITO、氧化钌、铝和镍中的1种或2种以上;
6.5所述的储能器件用底涂层,其中,所述导电材料包含碳纳米管;
7.1~6中任一项的储能器件用底涂层,其包含分散剂;
8.7所述的储能器件电极用底涂层,其中,所述分散剂为三芳基胺系高支化聚合物或在侧链中含有噁唑啉基的乙烯基系聚合物;
9.储能器件电极用底涂箔,是具有集电基板和在该集电基板的至少一面形成的储能器件用底涂层的储能器件电极用底涂箔,具备1~8中任一项的储能器件用底涂层作为所述储能器件用底涂层;
10.9所述的储能器件电极用底涂箔,其中,所述底涂层在所述集电基板的至少一面以将该面全体覆盖的形态形成;
11.9或10所述的储能器件电极用底涂箔,其中,所述底涂层包含基体高分子;
12.9~11中任一项所述的储能器件电极用底涂箔,其中,所述集电基板为铝箔或铜箔;
13.储能器件电极,其具有9~12中任一项所述的储能器件电极用底涂箔和在其底涂层的表面的一部分或全部形成的活性物质层;
14.13所述的储能器件电极,其中,所述活性物质层在所述底涂层的表面的一部分形成;
15.13或14所述的储能器件电极,其中,所述活性物质层以使所述底涂层的周缘残留、将其以外的部分全体覆盖的形态形成;
16.储能器件,其具备13~15中任一项所述的储能器件电极;
17.储能器件,具有至少一个具备一个或多个14或15所述的电极和金属极片而构成的电极结构体,将所述电极的至少一张在形成所述底涂层并且没有形成所述活性物质层的部分与所述金属极片超声波焊接;
18.17所述的储能器件,其中,所述金属极片含有选自铝、铜和镍中的至少一种的金属而构成;
19.储能器件的制造方法,是使用了一个或多个14或15所述的电极的储能器件的制造方法,其具有如下工序:将所述电极的至少一张在形成有所述底涂层并且未形成所述活性物质层的部分与金属极片超声波焊接。
发明的效果
根据本发明,能够提供可有效率地进行超声波焊接的储能器件电极用的底涂箔。通过使用具有该底涂箔的电极,从而能够提供低电阻的储能器件及其简便且有效率的制造方法。
具体实施方式
以下对本发明更详细地说明。
本发明涉及的储能器件电极用底涂层(以下称为底涂层),其特征在于,膜厚为1~200nm。
该底涂层如后述那样,在作为储能器件电极的构成部件的集电基板的至少一个面形成,构成电极的一部分。
作为本发明中的储能器件,例如可列举出双电层电容器、锂二次电池、锂离子二次电池、质子聚合物电池、镍氢电池、铝固体电容器、电解电容器、铅蓄电池等各种储能器件,本发明的底涂层能够适合用于双电层电容器、锂离子二次电池用的电极。
本发明的底涂层优选包含导电材料。
作为导电材料的具体例,可列举出炭黑、科琴黑、乙炔黑、碳晶须、碳纳米管(CNT)、碳纤维、天然石墨、人造石墨、氧化钛、ITO、氧化钌、铝、镍等,从形成均匀的薄膜的观点出发,优选使用CNT。
CNT一般采用电弧放电法、化学气相沉积法(CVD法)、激光烧蚀法等制作,本发明中所使用的CNT可采用任何方法得到。另外,在CNT中有将1张碳膜(石墨烯片)卷绕成圆筒状的单层CNT(以下也简写为SWCNT)和将2张石墨烯片卷绕成同心圆状的2层CNT(以下也简写为DWCNT)和将多个石墨烯片卷绕成同心圆状的多层CNT(以下也简写为MWCNT),在本发明中能够将SWCNT、DWCNT、MWCNT各自单独地使用或者将多个组合使用。
再有,在采用上述方法制作SWCNT、DWCNT或MWCNT时,有时镍、铁、钴、钇等催化剂金属残存,因此有时需要用于将该杂质除去的精制。对于杂质的除去,与采用硝酸、硫酸等的酸处理一起进行超声波处理是有效的。但是,对于使用硝酸、硫酸等的酸处理而言,有可能破坏构成CNT的π共轭系,损害CNT本来的特性,因此希望在适当的条件下进行精制而使用。
作为本发明中可使用的CNT的具体例,可列举出超速成长法CNT[国立研究开发法人新能源·产业技术综合开发机构制造]、eDIPS-CNT[国立研究开发法人新能源·产业技术综合开发机构制造]、SWNT系列[(株)名城纳米碳制造:商品名]、VGCF系列[昭和电工(株)制造:商品名]、FloTube系列[CNano Technology公司制造:商品名]、AMC[宇部兴产(株)制造:商品名]、NANOCYL NC7000系列[Nanocyl S.A.公司制造:商品名]、Baytubes[Bayer公司制造:商品名]、GRAPHISTRENGTH[爱勒化学公司制造:商品名]、MWNT7[保土谷化学工业(株)制造:商品名]、Hyperion CNT[Hypeprion Catalysis International公司制造:商品名]等。
本发明的底涂层优选使用包含上述的导电材料、优选CNT和溶剂的含有导电材料的组合物(分散液)制作。
作为溶剂,只要是以往在含有CNT等导电材料的组合物的制备中使用的溶剂,则并无特别限定,例如可列举出水;四氢呋喃(THF)、乙醚、1,2-二甲氧基乙烷(DME)等醚类;二氯甲烷、氯仿、1,2-二氯乙烷等卤代烃类;N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)等酰胺类;丙酮、甲乙酮、甲基异丁基酮、环己酮等酮类;甲醇、乙醇、异丙醇、正丙醇等醇类;正庚烷、正己烷、环己烷等脂肪族烃类;苯、甲苯、二甲苯、乙基苯等芳香族烃类;乙二醇单乙基醚、乙二醇单丁基醚、丙二醇单甲基醚等二醇醚类;乙二醇、丙二醇等二醇类等有机溶剂,这些溶剂能够各自单独地使用或者将2种以上混合使用。
特别地,在使用CNT作为导电材料的情况下,从可提高其孤立分散的比例的方面出发,优选水、NMP、DMF、THF、甲醇、异丙醇,这些溶剂能够各自单独地使用或者将2种以上混合使用。
另外,上述含有导电材料的组合物根据需要可含有基体高分子。
作为基体高分子的具体例,可列举出聚偏氟乙烯(PVdF)、聚四氟乙烯、四氟乙烯-六氟丙烯共聚物、偏氟乙烯-六氟丙烯共聚物[P(VDF-HFP)]、偏氟乙烯-氯三氟乙烯共聚物[P(VDF-CTFE)]等氟系树脂、聚乙烯基吡咯烷酮、乙烯-丙烯-二烯三元共聚物、PE(聚乙烯)、PP(聚丙烯)、EVA(乙烯-醋酸乙烯酯共聚物)、EEA(乙烯-丙烯酸乙酯共聚物)等聚烯烃系树脂;PS(聚苯乙烯)、HIPS(高抗冲聚苯乙烯)、AS(丙烯腈-苯乙烯共聚物)、ABS(丙烯腈-丁二烯-苯乙烯共聚物)、MS(甲基丙烯酸甲酯-苯乙烯共聚物)、苯乙烯-丁二烯橡胶等聚苯乙烯系树脂;聚碳酸酯树脂;氯乙烯树脂;聚酰胺树脂;聚酰亚胺树脂;聚丙烯酸、聚丙烯酸铵、聚丙烯酸钠、PMMA(聚甲基丙烯酸甲酯)等(甲基)丙烯酸系树脂;PET(聚对苯二甲酸乙二醇酯)、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯、聚萘二甲酸丁二醇酯、PLA(聚乳酸)、聚-3-羟基丁酸、聚己内酯、聚琥珀酸丁二醇酯、聚琥珀酸/己二酸乙二醇酯等聚酯树脂;聚苯醚树脂;改性聚苯醚树脂;聚缩醛树脂;聚砜树脂;聚苯硫醚树脂;聚乙烯醇树脂;聚乙醇酸;改性淀粉;醋酸纤维素、羧甲基纤维素、三醋酸纤维素;甲壳素、壳聚糖;木质素等热塑性树脂、聚苯胺和作为其半氧化体的本征态聚苯胺;聚噻吩;聚吡咯;聚亚苯基亚乙烯基;聚亚苯基;聚乙炔等导电性高分子、以及环氧树脂;氨基甲酸酯丙烯酸酯;酚醛树脂;蜜胺树脂;脲醛树脂;醇酸树脂等热固化性树脂、光固化性树脂等,在本发明的导电性碳材料分散液中,优选使用水作为溶剂,因此作为基体高分子,优选水溶性的基体高分子,例如聚丙烯酸、聚丙烯酸铵、聚丙烯酸钠、羧甲基纤维素钠、水溶性纤维素醚、海藻酸钠、聚乙烯醇、聚苯乙烯磺酸、聚乙二醇等,特别优选聚丙烯酸、聚丙烯酸铵、聚丙烯酸钠、羧甲基纤维素钠等。
基体高分子也能够作为市售品得到,作为这样的市售品,例如可列举出アロンA-10H(聚丙烯酸、东亚合成(株)制造、固体成分浓度26质量%、水溶液)、アロンA-30(聚丙烯酸铵、东亚合成(株)制造、固体成分浓度32质量%、水溶液)、聚丙烯酸钠(和光纯药工业(株)制造、聚合度2,700~7,500)、羧甲基纤维素钠(和光纯药工业(株)制造)、海藻酸钠(关东化学(株)制造、超纯级)、METOLOSE SH系列(羟丙基甲基纤维素、信越化学工业(株)制造)、METOLOSE SE系列(羟乙基甲基纤维素、信越化学工业(株)制造)、JC-25(完全皂化型聚乙烯醇、JAPAN VAM&POVAL CO.,LTD.制造)、JM-17(中间皂化型聚乙烯醇、JAPAN VAM&POVALCO.,LTD.制造)、JP-03(部分皂化型聚乙烯醇、JAPAN VAM&POVAL CO.,LTD.制造)、聚苯乙烯磺酸(Aldrich公司制造、固体成分浓度18质量%、水溶液)等。
对基体高分子的含量并无特别限定,在组合物中优选设为0.0001~99质量%左右,更优选设为0.001~90质量%左右。
进而,为了提高组合物中的导电材料的分散性,上述含有导电材料的组合物优选含有分散剂。
作为分散剂,并无特别限定,能够从公知的分散剂中适当地选择使用,作为其具体例,可列举出羧甲基纤维素(CMC)、聚乙烯基吡咯烷酮(PVP)、丙烯酸系树脂乳液、水溶性丙烯酸系聚合物、苯乙烯乳液、有机硅乳液、丙烯酸有机硅乳液、氟树脂乳液、EVA乳液、醋酸乙烯酯乳液、氯乙烯乳液、聚氨酯树脂乳液、国际公开第2014/04280号记载的三芳基胺系高支化聚合物、国际公开第2015/029949号记载的在侧链具有噁唑啉基的乙烯基系聚合物等,本发明中,优选国际公开第2014/04280号记载的三芳基胺系高支化聚合物、国际公开第2015/029949号记载的在侧链具有噁唑啉基的乙烯基系聚合物。
具体地,优选使用通过在酸性条件下使由下述式(1)和(2)表示的、三芳基胺类与醛类和/或酮类缩聚而得到的高支化聚合物。
[化1]
上述式(1)和(2)中,Ar1~Ar3各自独立地表示由式(3)~(7)表示的任一个二价的有机基团,特别优选由式(3)表示的取代或未取代的亚苯基。
[化2]
(式中,R5~R38各自独立地表示氢原子、卤素原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的烷氧基、羧基、磺基、磷酸基、膦酸基、或者它们的盐。)
另外,在式(1)和(2)中,Z1和Z2各自独立地表示氢原子、碳原子数1~5的可具有分支结构的烷基、或者由式(8)~(11)表示的任一个一价的有机基团(不过,Z1和Z2不会同时成为上述烷基。),作为Z1和Z2,各自独立地优选氢原子、2-或3-噻吩基、由式(8)表示的基团,特别地,Z1和Z2中的任一者为氢原子,另一者为氢原子、2-或3-噻吩基、由式(8)表示的基团,特别地,更优选R41为苯基的基团或者R41为甲氧基的基团。
再有,在R41为苯基的情况下,在后述的酸性基团引入法中,有时使用了在聚合物制造后引入酸性基团的方法,也有时在该苯基上引入酸性基团。
作为上述碳原子数1~5的可具有分支结构的烷基,可列举出与上述例示的基团同样的基团。
[化3]
{式中,R39~R62各自独立地表示氢原子、卤素原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、苯基、OR63、COR63、NR63R64、COOR65(这些式中,R63和R64各自独立地表示氢原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、或者苯基,R65表示碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、或者苯基。)、羧基、磺基、磷酸基、膦酸基、或者它们的盐。}。
上述式(2)~(7)中,R1~R38各自独立地表示氢原子、卤素原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的烷氧基、或者羧基、磺基、磷酸基、膦酸基或者它们的盐。
其中,作为卤素原子,可列举出氟原子、氯原子、溴原子、碘原子。
作为碳原子数1~5的可具有分支结构的烷基,可列举出甲基、乙基、正丙基、异丙基、正丁基、仲丁基、叔丁基、正戊基等。
作为碳原子数1~5的可具有分支结构的烷氧基,可列举出甲氧基、乙氧基、正丙氧基、异丙氧基、正丁氧基、仲丁氧基、叔丁氧基、正戊氧基等。
作为羧基、磺基、磷酸基和膦酸基的盐,可列举出钠、钾等碱金属盐;镁、钙等第2族金属盐;铵盐;丙胺、二甲胺、三乙胺、乙二胺等脂肪族胺盐;咪唑啉、哌嗪、吗啉等脂环式胺盐;苯胺、二苯胺等芳香族胺盐;吡啶鎓盐等。
上述式(8)~(11)中,R39~R62各自独立地表示氢原子、卤素原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、苯基、OR63、COR63、NR63R64、COOR65(这些式中,R63和R64各自独立地表示氢原子、碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、或者苯基,R65表示碳原子数1~5的可具有分支结构的烷基、碳原子数1~5的可具有分支结构的卤代烷基、或者苯基。)、或者羧基、磺基、磷酸基、膦酸基或者它们的盐。
其中,作为碳原子数1~5的可具有分支结构的卤代烷基,可列举出二氟甲基、三氟甲基、溴二氟甲基、2-氯乙基、2-溴乙基、1,1-二氟乙基、2,2,2-三氟乙基、1,1,2,2-四氟乙基、2-氯-1,1,2-三氟乙基、五氟乙基、3-溴丙基、2,2,3,3-四氟丙基、1,1,2,3,3,3-六氟丙基、1,1,1,3,3,3-六氟丙烷-2-基、3-溴-2-甲基丙基、4-溴丁基、全氟戊基等。
再有,作为卤素原子、碳原子数1~5的可具有分支结构的烷基,可列举出与上述式(2)~(7)中例示的基团同样的基团。
特别地,如果考虑进一步提高与集电基板的密合性,优选上述高支化聚合物在由式(1)或(2)表示的重复单元的至少一个芳香环中具有选自羧基、磺基、磷酸基、膦酸基和它们的盐中的至少一种的酸性基团,更优选具有磺基或其盐。
作为上述高支化聚合物的制造中使用的醛化合物,可列举出甲醛、多聚甲醛、乙醛、丙醛、丁醛、异丁醛、戊醛、己醛、2-甲基丁醛、己醛、十一醛、7-甲氧基-3,7-二甲基辛醛、环己烷甲醛、3-甲基-2-丁醛、乙二醛、丙二醛、丁二醛、戊二醛、己二醛等饱和脂肪族醛类;丙烯醛、异丁烯醛等不饱和脂肪族醛类;糠醛、吡啶醛、噻吩醛等杂环式醛类;苯甲醛、甲基苯甲醛、三氟甲基苯甲醛、苯基苯甲醛、水杨醛、茴香醛、乙酰氧基苯甲醛、对苯二甲醛、乙酰基苯甲醛、甲酰基苯甲酸、甲酰基苯甲酸甲酯、氨基苯甲醛、N,N-二甲基氨基苯甲醛、N,N-二苯基氨基苯甲醛、萘甲醛、蒽甲醛、菲甲醛等芳香族醛类、苯基乙醛、3-苯基丙醛等芳烷基醛类等,其中,优选使用芳香族醛类。
另外,作为用于上述高支化聚合物的制造的酮化合物,为烷基芳基酮、二芳基酮类,例如可列举出苯乙酮、苯丙酮、二苯基酮、苯基萘基酮、二萘基酮、苯基甲苯基酮、二(甲苯基)酮等。
本发明中使用的高支化聚合物如下述方案1中所示那样,例如,使由下述式(A)表示的、可给予上述的三芳基胺骨架的三芳基胺化合物与例如由下述式(B)表示的醛化合物和/或酮化合物在酸催化剂的存在下缩聚而得到。
再有,作为醛化合物,例如,在使用对苯二甲醛等苯二甲醛类这样的、二官能化合物(C)的情况下,也有时不仅发生由方案1表示的反应,而且发生由下述方案2表示的反应,得到2个官能团都有助于缩合反应的、具有交联结构的高支化聚合物。
[化4]
方案1
(式中,Ar1~Ar3和Z1~Z2表示与上述相同的含义。)
[化5]
方案2
(式中,Ar1~Ar3和R1~R4表示与上述相同的含义。)
在上述缩聚反应中,相对于三芳基胺化合物的芳基1当量,能够以0.1~10当量的比例使用醛化合物和/或酮化合物。
作为上述酸催化剂,例如能够使用硫酸、磷酸、高氯酸等无机酸类;对甲苯磺酸、对甲苯磺酸一水合物等有机磺酸类;甲酸、草酸等羧酸类等。
就酸催化剂的使用量而言,根据其种类进行各种选择,通常,相对于三芳基胺类100质量份,为0.001~10000质量份,优选为0.01~1000质量份,更优选为0.1~100质量份。
上述的缩合反应即使无溶剂也可进行,但通常使用溶剂进行。作为溶剂,只要不阻碍反应,则全部能够使用,例如可列举出四氢呋喃、1,4-二噁烷等环状醚类;N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)等酰胺类;甲基异丁基酮、环己酮等酮类;二氯甲烷、氯仿、1,2-二氯乙烷、氯苯等卤代烃类;苯、甲苯、二甲苯等芳香族烃类等,特别优选环状醚类。这些溶剂能够各自单独地使用或者将2种以上混合使用。
另外,如果使用的酸催化剂例如为甲酸这样的液体的酸催化剂,则也能够使酸催化剂兼具作为溶剂的职能。
缩合时的反应温度通常为40~200℃。就反应时间而言,根据反应温度进行各种选择,通常为30分钟至50小时左右。
以上这样得到的聚合物的重均分子量Mw通常为1000~2000000,优选为2000~1000000。
在高支化聚合物中引入酸性基团的情况下,可采用在作为聚合物原料的、上述三芳基胺化合物、醛化合物、酮化合物的芳香环上预先引入、使用其来制造高支化聚合物的方法引入;也可采用对得到的高支化聚合物用可在其芳香环上引入酸性基团的试剂进行处理的方法引入,如果考虑制造的简便性,优选使用后者的方法。
在后者的方法中,作为在芳香环上引入酸性基团的方法,并无特别限制,可根据酸性基团的种类从现有公知的各种方法中适当地选择。
例如,在引入磺基的情况下,能够采用使用过量的硫酸进行磺化的方法等。
对上述高支化聚合物的平均分子量并无特别限定,重均分子量优选1000~2000000,更优选2000~1000000。
应予说明,本发明中的重均分子量是采用凝胶渗透色谱的测定值(聚苯乙烯换算)。
作为具体的高支化聚合物,可列举出由下述式表示的高支化聚合物,但并不限定于这些。
[化6]
另一方面,作为在侧链具有噁唑啉基的乙烯基系聚合物(以下称为噁唑啉聚合物),优选为对式(12)中所示的在2位具有含有聚合性碳-碳双键的基团的噁唑啉单体进行自由基聚合而得到的、具有在噁唑啉环的2位与聚合物主链或间隔基结合的重复单元的聚合物。
[化7]
上述X表示含有聚合性碳-碳双键的基团,R100~R103相互独立地表示氢原子、卤素原子、碳原子数1~5的可具有分支结构的烷基、碳原子数6~20的芳基、或者碳原子数7~20的芳烷基。
作为噁唑啉单体具有的含有聚合性碳-碳双键的基团,只要含有聚合性碳-碳双键,则并无特别限定,优选含有聚合性碳-碳双键的链状烃基,例如优选乙烯基、烯丙基、异丙烯基等碳原子数2~8的烯基等。
作为卤素原子、碳原子数1~5的可具有分支结构的烷基,可列举出与上述同样的卤素原子、碳原子数1~5的可具有分支结构的烷基。
作为碳原子数6~20的芳基的具体例,可列举出苯基、二甲苯基、甲苯基、联苯基、萘基等。
作为碳原子数7~20的芳烷基的具体例,可列举出苄基、苯基乙基、苯基环己基等。
作为由式(12)表示的在2位具有含有聚合性碳-碳双键的基团的噁唑啉单体的具体例,可列举出2-乙烯基-2-噁唑啉、2-乙烯基-4-甲基-2-噁唑啉、2-乙烯基-4-乙基-2-噁唑啉、2-乙烯基-4-丙基-2-噁唑啉、2-乙烯基-4-丁基-2-噁唑啉、2-乙烯基-5-甲基-2-噁唑啉、2-乙烯基-5-乙基-2-噁唑啉、2-乙烯基-5-丙基-2-噁唑啉、2-乙烯基-5-丁基-2-噁唑啉、2-异丙烯基-2-噁唑啉、2-异丙烯基-4-甲基-2-噁唑啉、2-异丙烯基-4-乙基-2-噁唑啉、2-异丙烯基-4-丙基-2-噁唑啉、2-异丙烯基-4-丁基-2-噁唑啉、2-异丙烯基-5-甲基-2-噁唑啉、2-异丙烯基-5-乙基-2-噁唑啉、2-异丙烯基-5-丙基-2-噁唑啉、2-异丙烯基-5-丁基-2-噁唑啉等,从获得容易性等方面出发,优选2-异丙烯基-2-噁唑啉。
另外,如果考虑使用水系溶剂来制备含有导电材料的组合物,优选噁唑啉聚合物为水溶性。
这样的水溶性的噁唑啉聚合物可以是由上述式(12)表示的噁唑啉单体的均聚物,为了进一步提高在水中的溶解性,优选为使上述噁唑啉单体与具有亲水性官能团的(甲基)丙烯酸酯系单体的至少2种单体进行自由基聚合而得到的产物。
作为具有亲水性官能团的(甲基)丙烯酸系单体的具体例,可列举出(甲基)丙烯酸、丙烯酸2-羟基乙酯、丙烯酸甲氧基聚乙二醇酯、丙烯酸与聚乙二醇的单酯化物、丙烯酸2-氨基乙酯及其盐、甲基丙烯酸2-羟基乙酯、甲基丙烯酸甲氧基聚乙二醇酯、甲基丙烯酸与聚乙二醇的单酯化物、甲基丙烯酸2-氨基乙酯及其盐、(甲基)丙烯酸钠、(甲基)丙烯酸铵、(甲基)丙烯腈、(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-(2-羟基乙基)(甲基)丙烯酰胺、苯乙烯磺酸钠等,这些可单独地使用,也可将2种以上组合使用。这些中,优选(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸与聚乙二醇的单酯化物。
另外,在不对噁唑啉聚合物的导电材料分散能力产生不良影响的范围,能够将上述噁唑啉单体和具有亲水性官能团的(甲基)丙烯酸系单体以外的其他单体并用。
作为其他单体的具体例,可列举出(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸全氟乙酯、(甲基)丙烯酸苯酯等(甲基)丙烯酸酯单体;乙烯、丙烯、丁烯、戊烯等α-烯烃系单体;氯乙烯、偏氯乙烯、偏氟乙烯等卤代烯烃系单体;苯乙烯、α-甲基苯乙烯等苯乙烯系单体;醋酸乙烯酯、丙酸乙烯酯等羧酸乙烯酯系单体;甲基乙烯基醚、乙基乙烯基醚等乙烯基醚系单体等,这些可各自单独地使用,也可将2种以上组合使用。
在本发明中使用的噁唑啉聚合物制造中使用的单体成分中,就噁唑啉单体的含有率而言,从进一步提高得到的噁唑啉聚合物的导电材料分散能力的方面出发,优选10质量%以上,更优选20质量%以上,进一步优选30质量%以上。再有,单体成分中的噁唑啉单体的含有率的上限值为100质量%,这种情况下,得到噁唑啉单体的均聚物。
另一方面,从进一步提高得到的噁唑啉聚合物的水溶性的方面出发,单体成分中的具有亲水性官能团的(甲基)丙烯酸系单体的含有率优选10质量%以上,更优选20质量%以上,进一步优选30质量%以上。
另外,单体成分中的其他单体的含有率如上所述,为对得到的噁唑啉聚合物的导电材料分散能力不产生影响的范围,另外,由于因其种类而异,因此不能一概地决定,可在5~95质量%、优选10~90质量%的范围适当地设定。
对噁唑啉聚合物的平均分子量并无特别限定,重均分子量优选1000~2000000,更优选2000~1000000。
本发明中可使用的噁唑啉聚合物能够采用以往公知的自由基聚合用上述单体合成,也能够作为市售品得到,作为这样的市售品,例如可列举出EPOCROS WS-300((株)日本触媒制造、固体成分浓度10质量%、水溶液)、EPOCROS WS-700((株)日本触媒制造、固体成分浓度25质量%、水溶液)、EPOCROS WS-500((株)日本触媒制造、固体成分浓度39质量%、水/1-甲氧基-2-丙醇溶液)、聚(2-乙基-2-噁唑啉)(Aldrich)、聚(2-乙基-2-噁唑啉)(AlfaAesar)、聚(2-乙基-2-噁唑啉)(VWR International,LLC)等。
再有,作为溶液已市售的情况下,可直接使用,也可置换为目标的溶剂后使用。
本发明的含有导电材料的组合物中的导电材料与分散剂的混合比率用质量比表示,优选1000:1~1:100左右。
另外,组合物中的分散剂的浓度只要是可使导电材料在溶剂中分散的浓度,则并无特别限定,在组合物中优选设为0.001~30质量%左右,更优选设为0.002~20质量%左右。
进而,组合物中的导电材料的浓度根据目标的底涂层的膜厚、所要求的机械特性、电特性、热特性等而变化,另外,在CNT的情况下,只要至少其一部分孤立分散,能够用本发明中规定的膜厚制作底涂层,则是任意的,在组合物中优选设为0.0001~50质量%左右,更优选设为0.001~20质量%左右,进一步优选设为0.001~10质量%左右。
再有,在本发明中使用的含有导电材料的组合物中,可包含与使用的分散剂发生交联反应的交联剂、自交联的交联剂。这些交联剂优选在使用的溶剂中溶解。
作为三芳基胺系高支化聚合物的交联剂,例如可列举出三聚氰胺系、取代脲系、或者它们的聚合物系交联剂等,这些交联剂能够各自单独地使用或者将2种以上混合使用。再有,优选为具有至少2个交联形成取代基的交联剂,作为例子,可列举出CYMEL(注册商标)、甲氧基甲基化甘脲、丁氧基甲基化甘脲、羟甲基化甘脲、甲氧基甲基化三聚氰胺、丁氧基甲基化三聚氰胺、羟甲基化三聚氰胺、甲氧基甲基化苯并胍胺、丁氧基甲基化苯并胍胺、羟甲基化苯并胍胺、甲氧基甲基化脲、丁氧基甲基化脲、羟甲基化脲、甲氧基甲基化硫脲、甲氧基甲基化硫脲、羟甲基化硫脲等化合物、和这些化合物的缩合体。
作为噁唑啉聚合物的交联剂,只要是例如具有2个以上的羧基、羟基、硫醇基、氨基、亚磺酸基、环氧基等具有与噁唑啉基的反应性的官能团的化合物,则并无特别限定,优选具有2个以上的羧基的化合物。再有,具有在薄膜形成时的加热或酸催化剂的存在下产生上述官能团并引起交联反应的官能团例如羧酸的钠盐、钾盐、锂盐、铵盐等的化合物也能够用作交联剂。
作为与噁唑啉基引起交联反应的化合物的具体例,可列举出在酸催化剂的存在下发挥交联反应性的、聚丙烯酸、其共聚物等合成高分子和羧甲基纤维素、海藻酸这样的天然高分子的金属盐;通过加热而发挥交联反应性的、上述合成高分子和天然高分子的铵盐等,特别优选在酸催化剂的存在下或加热条件下发挥交联反应性的聚丙烯酸钠、聚丙烯酸锂、聚丙烯酸铵、羧甲基纤维素钠、羧甲基纤维素锂、羧甲基纤维素铵等。
这样的与噁唑啉基引起交联反应的化合物也能够作为市售品获得,作为这样的市售品,例如可列举出聚丙烯酸钠(和光纯药工业(株)制造、聚合度2,700~7,500)、羧甲基纤维素钠(和光纯药工业(株)制造)、海藻酸钠(关东化学(株)制造、鹿1级)、アロンA-30(聚丙烯酸铵、东亚合成(株)制造、固体成分浓度32质量%、水溶液)、DN-800H(羧甲基纤维素铵、DAICEL FINECHEM LTD.制造)、海藻酸铵((株)キミカ制造)等。
作为自交联的交联剂,例如可列举出对于羟基具有醛基、环氧基、乙烯基、异氰酸酯基、烷氧基、对于羧基具有醛基、氨基、异氰酸酯基、环氧基、对于氨基具有异氰酸酯基、醛基等在同一分子内具有相互反应的交联性官能团的化合物、具有在相同的交联性官能团之间反应的羟基(脱水缩合)、巯基(二硫醚键)、酯基(克莱森缩合)、硅烷醇基(脱水缩合)、乙烯基、丙烯酰基等的化合物等。
作为进行自交联的交联剂的具体例,可列举出在酸催化剂的存在下发挥交联反应性的多官能丙烯酸酯、四烷氧基硅烷、具有封闭异氰酸酯基的单体和具有羟基、羧酸、氨基中的至少1个的单体的嵌段共聚物等。
这样的进行自交联的交联剂也能够作为市售品得到,作为这样的市售品,例如,就多官能丙烯酸酯而言,可列举出A-9300(环氧化异氰脲酸三丙烯酸酯、新中村化学工业(株)制造)、A-GLY-9E(乙氧基化甘油三丙烯酸酯(EO 9mol)、新中村化学工业(株)制造)、A-TMMT(季戊四醇四丙烯酸酯、新中村化学工业(株)制造),就四烷氧基硅烷而言,可列举出四甲氧基硅烷(东京化成工业(株)制造)、四乙氧基硅烷(东横化学(株)制造),就含有封闭异氰酸酯基的聚合物而言,可列举出エラストロン系列E-37、H-3、H38、BAP、NEW BAP-15、C-52、F-29、W-11P、MF-9、MF-25K(第一工业制药(株)制造)等。
这些交联剂的添加量根据使用的溶剂、使用的基材、所要求的粘度、所要求的膜形状等而变动,相对于分散剂,为0.001~80质量%,优选为0.01~50质量%,更优选为0.05~40质量%。这些交联剂也有时发生自缩合引起的交联反应,但还是与分散剂引起交联反应,在分散剂中存在交联性取代基的情况下,利用这些交联性取代基来促进交联反应。
在本发明中,作为用于促进交联反应的催化剂,能够添加对-甲苯磺酸、三氟甲磺酸、对甲苯磺酸吡啶鎓、水杨酸、磺基水杨酸、柠檬酸、苯甲酸、羟基苯甲酸、萘甲酸等酸性化合物、和/或2,4,4,6-四溴环己二烯酮、苯偶姻甲苯磺酸酯、甲苯磺酸2-硝基苄酯、有机磺酸烷基酯等热致产酸剂。
就催化剂的添加量而言,相对于分散剂,为0.0001~20质量%,优选为0.0005~10质量%,更优选为0.001~3质量%。
对用于形成底涂层的含有导电材料的组合物的制备法并无特别限定,可将CNT等导电材料、溶剂、以及根据需要使用的分散剂、基体聚合物和交联剂按任意的顺序混合来制备分散液。
此时,优选对混合物进行分散处理,通过该处理,能够使CNT等导电材料的分散比例进一步提高。作为分散处理,可列举出作为机械处理的使用球磨机、珠磨机、喷射磨等的湿式处理、使用总线型、探针型的Sonicator的超声波处理,特别优选使用了喷射磨的湿式处理、超声波处理。
分散处理的时间是任意的,但优选1分钟至10小时左右,更优选5分钟至5小时左右。此时,可根据需要实施加热处理。
再有,在使用交联剂和/或基体高分子的情况下,它们可在制备了由分散剂、CNT等导电材料和溶剂构成的混合物后加入。
将以上说明的含有导电材料的组合物涂布于集电基板的至少一面,将其自然或加热干燥,形成底涂层,能够制作本发明的底涂箔。
此时,优选将含有导电材料的组合物涂布于集电基板的整个面,在整个集电基板面形成底涂层。
本发明中,为了在箔的底涂层部分采用超声波焊接等焊接高效率地使底涂箔与后述的金属极片接合,使底涂层的膜厚成为200nm以下,优选140nm以下,更优选80nm以下。
另一方面,为了确保底涂层的功能,再现性良好地得到优异的特性的电池,使集电基板的每一面的底涂层的膜厚优选成为1nm以上,更优选成为30nm以上。
本发明中的底涂层的膜厚例如能够从底涂箔中切出适当的大小的试验片,采用将其用手撕开等方法使截面露出,通过扫描电子显微镜(SEM)等的显微镜观察,从在截面部分中底涂层露出的部分求出。
另一方面,集电基板的每一面的底涂层的单位面积质量只要满足上述膜厚,则并无特别限定,如果考虑超声波焊接等的焊接性,优选设为0.1g/m2以下,更优选设为0.09g/m2以下,进一步优选设为不到0.05g/m2,如果考虑确保底涂层的功能、再现性良好地获得优异的特性的电池,优选设为0.001g/m2以上,更优选设为0.005g/m2以上,进一步优选设为0.01g/m2以上,更进一步优选设为0.015g/m2以上。
本发明中的底涂层的单位面积质量为底涂层的质量(g)相对于底涂层的面积(m2)的比例,在将底涂层形成为图案状的情况下,该面积为底涂层单独的面积,不包含在形成为图案状的底涂层之间露出的集电基板的面积。
就底涂层的质量而言,例如能够从底涂箔中切出适当的大小的试验片,测定其质量W0,然后,从底涂箔将底涂层剥离,测定将底涂层剥离后的质量W1,由其差(W0-W1)算出,或者预先测定集电基板的质量W2,然后,测定形成了底涂层的底涂箔的质量W3,由其差(W3-W2)算出。
作为将底涂层剥离的方法,例如可列举出使底涂层浸渍于底涂层溶解或溶胀的溶剂中、用布等将底涂层擦除等方法。
单位面积质量、膜厚能够采用公知的方法进行调整。例如,通过涂布形成底涂层的情况下,能够通过改变用于形成底涂层的涂布液(含有导电材料的组合物)的固体成分浓度、涂布次数、涂布机的涂布液投入口的间隙等来调整。
在想要使单位面积质量、膜厚增大的情况下,提高固体成分浓度,增加涂布次数,或者增大间隙。在想要使单位面积质量、膜厚减小的情况下,降低固体成分浓度,减少涂布次数,或者减小间隙。
作为集电基板,可从以往用作储能器件电极的集电基板的集电基板中适当地选择,例如能够使用铜、铝、镍、金、银和它们的合金、碳材料、金属氧化物、导电性高分子等的薄膜,在应用超声波焊接等焊接制作电极结构体的情况下,优选使用由铜、铝、镍、金、银和它们的合金制成的金属箔。
对集电基板的厚度并无特别限定,在本发明中,优选1~100μm。
作为含有导电材料的组合物的涂布方法,例如可列举出旋涂法、浸涂法、流涂法、喷墨法、喷涂法、棒涂法、凹版涂布法、狭缝涂布法、辊涂法、苯胺印刷法、转印印刷法、毛刷涂布、刮板涂布法、气刀涂布法等,从作业效率等方面出发,优选喷墨法、流延法、浸涂法、棒涂法、刮板涂布法、辊涂法、凹版涂布法、苯胺印刷法、喷涂法。
进行加热干燥时的温度也是任意的,优选50~200℃左右,更优选80~150℃左右。
本发明的储能器件电极能够通过在上述底涂箔的底涂层上形成活性物质层而制作。
其中,作为活性物质,能够使用以往用于储能器件电极的各种活性物质。
例如,在锂二次电池、锂离子二次电池的情况下,作为正极活性物质,能够使用可吸附和脱离锂离子的硫属化合物或含有锂离子的硫属化合物、聚阴离子系化合物、硫单质及其化合物等。
作为这样的可吸附和脱离锂离子的硫属化合物,例如可列举出FeS2、TiS2、MoS2、V2O6、V6O13、MnO2等。
作为含有锂离子的硫属化合物,例如可列举出LiCoO2、LiMnO2、LiMn2O4、LiMo2O4、LiV3O8、LiNiO2、LixNiyM1-yO2(其中,M表示选自Co、Mn、Ti、Cr、V、Al、Sn、Pb和Zn中的至少一种以上的金属元素,0.05≤x≤1.10,0.5≤y≤1.0)等。
作为聚阴离子系化合物,例如可列举出LiFePO4等。
作为硫化合物,例如可列举出Li2S、红氨酸等。
另一方面,作为构成上述负极的负极活性物质,能够使用碱金属、碱金属合金、吸储和放出锂离子的选自周期表第4~15族的元素中的至少一种的单质、氧化物、硫化物、氮化物、或可可逆地吸储和放出锂离子的碳材料。
作为碱金属,可列举出Li、Na、K等,作为碱金属合金,例如可列举出Li-Al、Li-Mg、Li-Al-Ni、Na-Hg、Na-Zn等。
作为吸储放出锂离子的选自周期表第4~15族的元素中的至少一种的元素的单质,例如可列举出硅、锡、铝、锌、砷等。
作为其氧化物,例如可列举出锡硅氧化物(SnSiO3)、锂氧化铋(Li3BiO4)、锂氧化锌(Li2ZnO2)、锂氧化钛(Li4Ti5O12)等。
作为其硫化物,可列举出锂硫化铁(LixFeS2(0≤x≤3))、锂硫化铜(LixCuS(0≤x≤3))等。
作为其氮化物,可列举出含有锂的过渡金属氮化物,具体地,可列举出LixMyN(M=Co、Ni、Cu、0≤x≤3、0≤y≤0.5)、锂铁氮化物(Li3FeN4)等。
作为可可逆地吸储和放出锂离子的碳材料,可列举出石墨、炭黑、焦炭、玻璃状碳、碳纤维、碳纳米管、或它们的烧结体等。
另外,在双电层电容器的情况下,能够使用碳质材料作为活性物质。
作为该碳质材料,可列举出活性炭等,例如可列举出将酚醛树脂碳化后进行活化处理而得到的活性炭。
活性物质层能够通过将包含以上说明的活性物质、粘结剂聚合物和根据需要使用的溶剂的电极浆料在底涂层上涂布,进行自然或加热干燥而形成。
活性物质层的形成部位可根据使用的器件的电池形态等适当地设定,可以是底涂层的表面全部,也可以是其一部分,为了用于层叠体电池等,在作为将金属极片与电极通过超声波焊接等焊接接合的电极结构体使用的情况下,为了使焊接部残留,优选在底涂层的表面的一部分涂布电极浆料,形成活性物质层。特别地,在层叠体电池用途中,优选将使底涂层的周缘残留的部分以外的部分涂布电极浆料来形成活性物质层。
作为粘结剂聚合物,能够从公知的材料中适当地选择使用,例如可列举出聚偏氟乙烯(PVdF)、聚乙烯基吡咯烷酮、聚四氟乙烯、四氟乙烯-六氟丙烯共聚物、偏氟乙烯-六氟丙烯共聚物[P(VDF-HFP)]、偏氟乙烯-三氟氯乙烯共聚物[P(VDF-CTFE)]、聚乙烯醇、聚酰亚胺、乙烯-丙烯-二烯三元共聚物、苯乙烯-丁二烯橡胶、羧甲基纤维素(CMC)、聚丙烯酸(PAA)、聚苯胺等导电性高分子等。
再有,就粘结剂聚合物的添加量而言,相对于活性物质100质量份,优选0.1~20质量份,特别优选1~10质量份。
作为溶剂,可列举出上述含有导电材料的组合物中例示的溶剂,可从它们中根据粘结剂的种类适当地选择,在PVdF等非水溶性的粘结剂的情况下,优选NMP,在PAA等水溶性的粘结剂的情况下,优选水。
再有,上述电极浆料可包含导电助剂。作为导电助剂,例如可列举出炭黑、科琴黑、乙炔黑、碳晶须、碳纤维、天然石墨、人造石墨、氧化钛、氧化钌、铝、镍等。
作为电极浆料的涂布方法,可列举出与上述的含有导电材料的组合物同样的方法。
另外,加热干燥时的温度也是任意的,但优选50~400℃左右,更优选80~150℃左右。
另外,就电极而言,能够根据需要进行压制。就压制法而言,能够使用一般所采用的方法,特别优选模压法、辊压法。对辊压法中的压制压力并无特别限定,优选0.2~3吨/cm。
本发明涉及的储能器件具备上述的储能器件电极,更具体地,具备至少一对正极和负极、介于这些各极间的分隔体、和电解质而构成,正极和负极中的至少一者由上述的储能器件电极构成。
该储能器件在使用上述的储能器件电极作为电极上具有其特征,因此作为其他的器件构成部件的分隔体、电解质等能够从公知的材料中适当地选择使用。
作为分隔体,例如可列举出纤维素系分隔体、聚烯烃系分隔体等。
作为电解质,液体、固体的电解质均可,另外水系、非水系的电解质均可,本发明的储能器件电极在应用于使用了非水系电解质的器件的情况下也可发挥实用上充分的性能。
作为非水系电解质,可列举出将电解质盐溶解于非水系有机溶剂而成的非水系电解液。
作为电解质盐的具体例,可列举出四氟硼酸锂、六氟磷酸锂、高氯酸锂、三氟甲磺酸锂等锂盐;四甲基铵六氟磷酸盐、四乙基铵六氟磷酸盐、四丙基铵六氟磷酸盐、甲基三乙基铵六氟磷酸盐、四乙基铵四氟硼酸盐、四乙基铵高氯酸盐等季铵盐;双(三氟甲磺酰基)亚胺锂、双(氟磺酰基)亚胺锂等亚胺锂等。
作为非水系有机溶剂的具体例,可列举出碳酸亚丙酯、碳酸亚乙酯、碳酸亚丁酯等碳酸亚烷基酯;碳酸二甲酯、碳酸甲乙酯、碳酸二乙酯等碳酸二烷基酯;乙腈等腈类;二甲基甲酰胺等酰胺类等。
对储能器件的形态并无特别限定,能够采用圆筒型、扁平卷绕方型、层叠方型、硬币型、扁平卷绕层叠型、层叠层压型等以往公知的各种形态的电池。
应用于硬币型的情况下,可将上述的本发明的储能器件电极冲切为规定的圆盘状而使用。
例如,锂离子二次电池能够通过在硬币型电池的焊接了垫片与间隔物的盖部设置规定张数的冲切成规定形状的锂箔,在其上重叠使电解液浸渍了的相同形状的分隔体,进而使活性物质层为下、从上重叠本发明的储能器件电极,放置外壳和垫圈,用硬币型电池压接机密封而制作。
在应用于层叠层压型的情况下,可使用在将活性物质层在底涂层表面的一部分形成的电极中的、形成有底涂层并且未形成活性物质层的部分(焊接部)与金属极片焊接而得到的电极结构体。
这种情况下,构成电极结构体的电极可以是一个,也可以是多个,一般地,正负极都使用多个。
用于形成正极的多个电极优选与用于形成负极的多张电极板各自一个一个地交替地重叠,此时,优选使上述的分隔体介于正极与负极之间。
金属极片可以在多个电极的最外侧的电极的焊接部进行焊接,也可在多张电极中的任意地邻接的2个电极的焊接部间夹持金属极片进行焊接。
就金属极片的材质而言,只要是一般在储能器件中所使用的材质,则并无特别限定,例如可列举出镍、铝、钛、铜等金属;不锈钢、镍合金、铝合金、钛合金、铜合金等合金等,如果考虑焊接效率,优选包含选自铝、铜和镍中的至少1种金属而构成。
金属极片的形状优选箔状,其厚度优选0.05~1mm左右。
焊接方法能够使用在金属之间的焊接中使用的公知的方法,作为其具体例,可列举出TIG焊接、点焊、激光焊接、超声波焊接等,如上所述,为了使本发明的底涂层成为特别适合超声波焊接的膜厚,优选采用超声波焊接将电极与金属极片接合。
作为超声波焊接的方法,例如可列举出将多张电极配置于砧与焊头之间、将金属极片配置于焊接部、施加超声波来一齐进行焊接的方法;先将电极之间焊接、然后将金属极片焊接的方法等。
本发明中,在所有的方法中,都不仅将金属极片与电极在上述焊接部焊接,而且也将多个电极之间在形成底涂层并且没有形成活性物质层的部分相互地超声波焊接。
对焊接时的压力、频率、输出功率、处理时间等并无特别限定,可考虑使用的材料、底涂层的膜厚等来适当地设定。
通过将如以上那样制作的电极结构体容纳在层叠包装中,注入上述的电解液后,进行热封,从而得到层叠体电池。
这样得到的储能器件具有至少一个具备金属极片和一个或多个电极而构成的电极结构体,电极具有集电基板、在该集电基板的至少一面形成的底涂层、和在该底涂层的表面的一部分形成的活性物质层,在使用了多个电极的情况下,具有如下的构成:将它们在形成有底涂层并且未形成活性物质层的部分相互地超声波焊接,同时将电极中的至少一个在形成有底涂层并且未形成活性物质层的部分与金属极片超声波焊接。
实施例
以下列举实施例和比较例对本发明更具体地说明,但本发明并不限定于下述的实施例。应予说明,使用的测定装置如下所述。
(1)探针型超声波照射装置(分散处理)
装置:Hielscher Ultrasonics公司制UIP1000
(2)线棒涂布器(薄膜制作)
装置:(株)SMT制PM-9050MC
(3)超声波焊接机(超声波焊接试验)
装置:日本エマソン(株)制造、2000Xea 40:0.8/40MA-XaeStand
(4)充放电测定装置(二次电池评价)
装置:北斗电工(株)制造HJ1001SM8A
(5)测微计(粘结剂、活性层的膜厚测定)
装置:(株)ミツトヨ制造IR54
(6)Homo Disper(电极浆料的混合)
装置:T.K.ROBOMIX(带有Homo Disper2.5型(φ32))(PRIMIX(株)制造)
(7)薄膜旋转型高速混合机(电极浆料的混合)
装置:FILMIX 40型(PRIMIX(株)制造)
(8)自转-公转混合机(电极浆料的脱泡)
装置:THINKY MIXER(ARE-310)((株)THINKY制造)
(9)辊压装置(电极的压缩)
装置:超小型台式热辊压机HSR-60150H(宝泉(株)制造)
(10)扫描电子显微镜(SEM)
装置:日本电子(株)制造、JSM-7400F
[1]底涂箔的制造
[实施例1-1]
使作为分散剂采用与国际公开第2014/042080号的合成例2同样的方法合成的、由下述式表示的PTPA-PBA-SO3H0.50g溶解于作为分散介质的2-丙醇43g和水6.0g中,在该溶液中添加MWCNT(Nanocyl公司制“NC7000”外径10nm)0.50g。对该混合物,使用探针型超声波照射装置在室温(约25℃)下进行30分钟超声波处理,得到了无沉淀物、MWCNT均匀地分散的黑色的含有MWCNT的分散液。
在得到的含有MWCNT的分散液50g中加入作为包含聚丙烯酸(PAA)的水溶液的アロンA-10H(东亚合成(株)、固体成分浓度25.8质量%)3.88g和2-丙醇46.12g,搅拌,得到了底涂液A1。用2-丙醇稀释到2倍,得到了底涂液A2。
用线棒涂布器(OSP2、湿膜厚2μm)将得到的底涂液A2在作为集电基板的铝箔(厚15μm)均匀地展开后,在120℃下干燥10分钟,形成底涂层,制作底涂箔B1。
膜厚的测定如下所述进行。将上述制作的底涂箔切出1cm×1cm,在其中央部分用手撕开,用SEM以10000~60000倍观察截面部分中底涂层露出的部分,设为膜厚。如上所述测定的底涂箔B1的底涂层的厚度为约16nm。
进而在得到的底涂箔B1的相反侧的面也同样地将底涂液A2涂布、干燥,从而制作在铝箔的两面形成了底涂层的底涂箔C1。
[化8]
[实施例1-2]
除了使用了实施例1-1中制作的底涂液A1以外,与实施例1-1同样地制作底涂箔B2和C2,与实施例1-1同样地测定了底涂箔B2的底涂层的厚度,结果为23nm。
[实施例1-3]
除了使用了线棒涂布器(OSP3、湿膜厚3μm)以外,与实施例1-2同样地制作底涂箔B3和C3,测定了底涂箔B3的底涂层的厚度,结果为31nm。
[实施例1-4]
除了使用了线棒涂布器(OSP4、湿膜厚4μm)以外,与实施例1-2同样地制作底涂箔B4和C4,测定了底涂箔B4的底涂层的厚度,结果为41nm。
[实施例1-5]
除了使用了线棒涂布器(OSP6、湿膜厚6μm)以外,与实施例1-2同样地制作底涂箔B5和C5,测定了底涂箔B5的底涂层的厚度,结果为60nm。
[实施例1-6]
除了使用了线棒涂布器(OSP8、湿膜厚8μm)以外,与实施例1-2同样地制作底涂箔B6和C6,测定了底涂箔B6的底涂层的厚度,结果为80nm。
[比较例1-1]
除了使用了线棒涂布器(OSP22、湿膜厚22μm)以外,与实施例1-2同样地制作底涂箔B7和C7,测定了底涂箔B7的底涂层的厚度,结果为210nm。
[比较例1-2]
除了使用了线棒涂布器(OSP30、湿膜厚30μm)以外,与实施例1-2同样地制作底涂箔B8和C8,测定了底涂箔B8的底涂层的厚度,结果为250nm。
[超声波焊接试验]
对于实施例1-1~1-6和比较例1-1~1-2中制作的各底涂箔,采用下述方法进行了超声波焊接试验。
使用日本エマソン(株)的超声波焊接机(2000Xea,40:
0.8/40MA-XaeStand),在砧上的铝极片(宝泉(株)制造、厚0.1mm、宽5mm)上层叠在两面形成了底涂层的底涂箔5张,从上安放焊头而给予超声波振动,进行焊接。焊接面积设为3×12mm,焊接后,将没有使与角状物(horn)接触的底涂箔破损、要使极片与底涂箔剥离的情况下使箔破损的情形记为○,将在极片与箔间剥离的情形记为×。将结果示于表1中。
[表1]
底涂箔 | 膜厚度(nm) | 能否焊接 | |
实施例1-1 | C1 | 16 | ○ |
实施例1-2 | C2 | 23 | ○ |
实施例1-3 | C3 | 31 | ○ |
实施例1-4 | C4 | 41 | ○ |
实施例1-5 | C5 | 60 | ○ |
实施例1-6 | C6 | 80 | ○ |
比较例1-1 | C7 | 210 | × |
比较例1-2 | C8 | 250 | × |
如表1中所示那样,关于具备膜厚超过200nm的底涂层的底涂箔,在极片-底涂箔间的焊接强度不充分,在极片-底涂箔间剥离,就膜厚为200nm以下的底涂层而言,在极片-底涂箔间的焊接强度充分,即使在极片-底涂箔间使其剥离,也使底涂箔破裂。
由以上确认:为了将底涂箔与金属极片用充分的强度进行焊接,必须使底涂层的膜厚成为200nm以下。
[2]将LFP用于活性物质的电极和锂离子电池的制造
[实施例2-1]
将作为活性物质的磷酸铁锂(LFP、TATUNG FINE CHEMICALS CO.)17.3g、作为粘结剂的聚偏氟乙烯(PVdF)的NMP溶液(12质量%、(株)クレハ、KF聚合物L#1120)12.8g、作为导电助剂的乙炔黑0.384g和N-甲基吡咯烷酮(NMP)9.54g使用HOMO DISPER以3,500rpm混合了5分钟。接下来,使用薄膜旋转型高速混合机以线速度20m/秒进行60秒的混合处理,进而使用自转-公转混合机以2,200rpm进行30秒脱泡,从而制作了电极浆料(固体成分浓度48质量%、LFP:PVdF:AB=90:8:2(质量比))。
将得到的电极浆料在实施例1-1中制作的底涂箔B1均匀(湿膜厚200μm)地展开后,在80℃下干燥30分,接下来在120℃下干燥30分,在底涂层上形成活性物质层,进而使用辊压机进行压接,从而制作活性物质层的厚度为50μm的电极。
将得到的电极冲切为直径10mm的圆盘状,测定了质量后,在100℃下真空干燥15小时,转移到用氩充满的手套箱中。
在2032型的硬币型电池(宝泉(株)制造)的焊接了垫圈和间隔物的极片设置将6张冲切为直径14mm的锂箔(本荘化学(株)制造、厚0.17mm)重叠而成的产物,在其上重叠一张使电解液(キシダ化学(株)制造、碳酸亚乙酯:碳酸二乙酯=1:1(体积比)、包含1mol/L的作为电解质的六氟磷酸锂。)渗入24小时以上的、冲切为直径16mm的分隔体(セルガード(株)制造、2400)。进而,使涂布了活性物质的面为下,从上重叠电极。滴下1滴电解液后,放置外壳和垫圈,用硬币型电池压接机密封。然后,静置24小时,制成了试验用的二次电池。
[实施例2-2]
除了使用了实施例1-2中得到的底涂箔B2以外,与实施例2-1同样地制作了试验用的二次电池。
[实施例2-3]
除了使用了实施例1-3中得到的底涂箔B3以外,与实施例2-1同样地制作了试验用的二次电池。
[实施例2-4]
除了使用了实施例1-4中得到的底涂箔B4以外,与实施例2-1同样地制作了试验用的二次电池。
[实施例2-5]
除了使用了实施例1-5中得到的底涂箔B5以外,与实施例2-1同样地制作了试验用的二次电池。
[实施例2-6]
除了使用了实施例1-6中得到的底涂箔B6以外,与实施例2-1同样地制作了试验用的二次电池。
[比较例2-1]
除了使用了比较例1-1中得到的底涂箔B7以外,与实施例2-1同样地制作了试验用的二次电池。
[比较例2-2]
除了使用了比较例1-2中得到的底涂箔B8以外,与实施例2-1同样地制作了试验用的二次电池。
[比较例2-3]
除了使用了无垢的铝箔以外,与实施例2-1同样地制作了试验用的二次电池。
对于上述实施例2-1~2-6和比较例2-1~2-3中制作的锂离子二次电池,使用充放电测定装置在下述的条件下评价了电极的物性。将5C放电时的平均电压示于表2。
·电流:0.5C恒电流充电、5C恒电流放电(使LFP的容量为170mAh/g)
·截止电压:4.50V-2.00V
·温度:室温
[表2]
如表2中所示那样,在比较例2-3中所示的使用了未形成底涂层的无垢的铝箔的电池中,确认了由于电池的电阻高,因此5C放电时的平均电压低。而如实施例2-1~2-6和比较例2-1~2-2中所示那样,确认了如果使用底涂箔,则电池的电阻降低,因此5C放电时的平均电压升高。
由以上的结果确认:通过使底涂层的膜厚成为1~200nm,从而能够制造可焊接、并且得到低电阻的储能器件的底涂箔。
Claims (15)
1.储能器件电极,其特征在于,是具有储能器件电极用底涂箔和活性物质层的储能器件电极,该储能器件电极用底涂箔具有集电基板和在该集电基板的至少一面形成的储能器件用底涂层,该活性物质层是在该底涂层的表面的部分形成的活性物质层,
该储能器件电极在形成有所述底涂层并且没有形成所述活性物质层的部分与金属极片被超声波焊接,
所述底涂层的厚度为1~80nm。
2.根据权利要求1所述的储能器件电极,其中,所述底涂层的厚度为16~80nm。
3.根据权利要求2所述的储能器件电极,其中,所述底涂层的厚度为30~80nm。
4.根据权利要求1~3中任一项所述的储能器件电极,其中,所述底涂层包含导电材料。
5.根据权利要求4所述的储能器件电极,其中,所述导电材料包含选自炭黑、科琴黑、乙炔黑、碳晶须、碳纳米管、碳纤维、天然石墨、人造石墨、氧化钛、ITO、氧化钌、铝和镍中的1种或2种以上。
6.根据权利要求5所述的储能器件电极,其中,所述导电材料包含碳纳米管。
7.根据权利要求1~3中任一项所述的储能器件电极,其中,所述底涂层包含分散剂。
8.根据权利要求7所述的储能器件电极,其中,所述分散剂为三芳基胺系高支化聚合物或在侧链中含有噁唑啉基的乙烯基系聚合物。
9.根据权利要求1~3中任一项所述的储能器件电极,其中,所述底涂层包含基体高分子。
10.根据权利要求1~3中任一项所述的储能器件电极,其中,所述集电基板为铝箔或铜箔。
11.根据权利要求1~3中任一项所述的储能器件电极,其中,所述活性物质层是以使所述底涂层的周缘残留、将其以外的部分全部覆盖的形态形成的。
12.储能器件,其具备根据权利要求1~11中任一项所述的储能器件电极。
13.储能器件,具有至少一个的具备一个或多个根据权利要求1~11中任一项所述的电极和金属极片而构成的电极结构体,所述电极的至少一个在形成有所述底涂层并且没有形成所述活性物质层的部分与所述金属极片被超声波焊接。
14.根据权利要求13所述的储能器件,其中,所述金属极片含有选自铝、铜和镍中的至少一种的金属而构成。
15.储能器件的制造方法,是使用了一个或多个根据权利要求1~11中任一项所述的电极的储能器件的制造方法,其具有如下工序:将所述电极的至少一个在形成有所述底涂层并且未形成所述活性物质层的部分与金属极片超声波焊接。
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EP (1) | EP3550646B1 (zh) |
JP (2) | JP6531868B2 (zh) |
KR (2) | KR20230162126A (zh) |
CN (1) | CN110024192B (zh) |
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EP3550646B1 (en) * | 2016-12-02 | 2022-09-28 | Nissan Chemical Corporation | Undercoat layer for energy storage device, and undercoat foil for energy storage device electrode |
JPWO2021106592A1 (zh) * | 2019-11-29 | 2021-06-03 | ||
WO2024071255A1 (ja) * | 2022-09-28 | 2024-04-04 | 積水化学工業株式会社 | 非水電解質二次電池 |
CN115911262B (zh) * | 2022-12-09 | 2024-06-25 | 厦门海辰储能科技股份有限公司 | 电极极片及其回收方法、电化学装置 |
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- 2017-11-29 EP EP17875545.0A patent/EP3550646B1/en active Active
- 2017-11-29 US US16/465,922 patent/US20190288292A1/en not_active Abandoned
- 2017-11-29 CN CN201780073386.0A patent/CN110024192B/zh active Active
- 2017-11-29 JP JP2018524305A patent/JP6531868B2/ja active Active
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JP6531868B2 (ja) | 2019-06-19 |
JPWO2018101305A1 (ja) | 2018-11-29 |
EP3550646B1 (en) | 2022-09-28 |
TW201840472A (zh) | 2018-11-16 |
KR20190087536A (ko) | 2019-07-24 |
CN110024192A (zh) | 2019-07-16 |
KR20230162126A (ko) | 2023-11-28 |
JP2019140119A (ja) | 2019-08-22 |
WO2018101305A1 (ja) | 2018-06-07 |
US20190288292A1 (en) | 2019-09-19 |
EP3550646A1 (en) | 2019-10-09 |
EP3550646A4 (en) | 2020-06-24 |
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