CN112639018B - 组合物和层积体 - Google Patents
组合物和层积体 Download PDFInfo
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- CN112639018B CN112639018B CN201980055655.XA CN201980055655A CN112639018B CN 112639018 B CN112639018 B CN 112639018B CN 201980055655 A CN201980055655 A CN 201980055655A CN 112639018 B CN112639018 B CN 112639018B
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Abstract
本发明提供无机填料的分散性以及耐氧化性优异的组合物。一种组合物,其特征在于,其包含无机填料、氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物、以及溶剂。
Description
技术领域
本发明涉及组合物和层积体。
背景技术
在油墨、橡胶、导电性膜、电化学器件(电池等)等使用无机填料的领域中,为了使无机填料均匀分散在分散介质中,通常使用分散剂。
例如,在锂离子电池等二次电池领域中,作为用于分散作为正极用导电助剂使用的碳填料(乙炔黑、油炉黑、碳纳米管、石墨烯等)的分散剂,广泛使用了聚乙烯吡咯烷酮(PVP)(例如参照专利文献1~3)。
另外,在分散剂以外的领域,作为亲水化剂、防止水生生物附着的材料、生物相容性材料等,提出了使用四氟乙烯与N-乙烯基吡咯烷酮的共聚物的提案(例如参照专利文献4~6)。
现有技术文献
专利文献
专利文献1:日本特开2005-162877号
专利文献2:日本特开2017-54649号
专利文献3:日本特开2016-25077号
专利文献4:国际公开第2016/133206号
专利文献5:国际公开第2016/204142号
专利文献6:国际公开第2016/204217号
发明内容
发明所要解决的课题
本发明的目的在于提供无机填料的分散性以及耐氧化性优异的组合物。
用于解决课题的手段
本发明涉及一种组合物,其特征在于,其包含无机填料;氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物;以及溶剂。
上述无机填料与上述共聚物的质量比(无机填料/共聚物)优选为0.1~100。
优选上述共聚物为选自由四氟乙烯和六氟丙烯组成的组中的至少一种氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物,相对于全部单体单元,氟单体单元为65~7摩尔%、具有酰胺键的聚合性乙烯基化合物单元为35~93摩尔%。
上述无机填料优选为碳填料。
上述无机填料还优选为纤维状碳。
上述无机填料还优选为碳纳米管。
本发明还涉及一种层积体,其具备基材、以及形成在上述基材上的由上述组合物形成的涂膜。
本发明还涉及一种导电性构件,其具备上述层积体。
本发明还涉及一种分散剂,其是用于使无机填料分散在溶剂中的分散剂,其特征在于,其含有:氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物。
发明的效果
根据本发明,能够提供无机填料的分散性以及耐氧化性优异的组合物。
具体实施方式
以下对本发明进行具体说明。
本发明涉及一种组合物,其特征在于,其包含:无机填料;氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物;以及溶剂。
本发明的组合物由于包含上述共聚物,因此与使用聚乙烯吡咯烷酮(PVP)等的情况相比,无机填料的分散性(无机填料相对于溶剂的分散性)以及耐氧化性优异。
另外,本发明的组合物中,即使上述共聚物为较少量,无机填料的分散性以及耐氧化性也优异。
另外,本发明的组合物即使经过长时间(例如制备后7天以上),无机填料的分散性也优异。
另外,本发明的组合物的粘度变化小。
作为上述无机填料,可以举出碳填料、陶瓷填料、金属填料等。
作为上述碳填料,可以举出炭黑(科琴黑、乙炔黑、炉黑、槽法炭黑等)、纤维状碳(碳纤维、碳纳米管、碳纳米纤维、碳纳米突、碳纳米刷等)、片状碳(石墨烯等)、球状碳(富勒烯等)、纳米孔碳、石墨(天然石墨、人造石墨)等。
其中优选纤维状碳,更优选碳纳米管(CNT)。
上述炭黑的平均粒径优选为0.1nm~100μm、更优选为1nm~50μm。
上述平均粒径可以利用粒度分布计或电子显微镜(SEM)进行测定。
上述纤维状碳的平均纤维径优选为0.1nm~500nm、更优选为1~200nm。
另外,上述纤维状碳的平均纤维长度/平均纤维径的比例优选为1~5000、更优选为1~500。
上述平均纤维径和平均纤维长度可以利用粒度分布计或电子显微镜(SEM)进行测定。
上述片状碳可以为单层或者几个片层积而成的多层,在为多层的情况下,优选为50层以下、更优选为10层以下。
上述层积数可以通过拉曼分光法进行测定。
上述片状碳中,一层的平均厚度优选为0.1~1nm、更优选为0.2~0.4nm。
上述片状碳中,将片扩展后的最长部分的平均长度优选为0.1nm~1000μm、更优选为1nm~100μm。
上述平均长度可以利用电子显微镜(SEM)进行测定。
上述球状碳的平均粒径优选为0.1nm~100μm、更优选为0.1nm~1μm。
上述平均粒径可以利用粒度分布计或电子显微镜(SEM)进行测定。
作为上述陶瓷填料,可以举出锆、钽、钛、钨、硅、铝、铍等的无机氮化物类、碳化物类、硼化物类、氧化物类等的颗粒,具体地说,可以举出氧化铝、氧化锆、氮化铝、氧化铍、氮化锆、硼化锆、氮化钛、氧化钛、氧化硅、碳化钽、碳化钨、碳化锆、碳化钛、碳化硅、硼化铝、硼化钛等的颗粒。
其中优选氧化铝、氧化钛、氧化硅。
上述陶瓷填料的平均粒径优选为0.01nm~100μm、更优选为0.1nm~10μm。
上述平均粒径可以利用粒度分布计或电子显微镜(SEM)进行测定。
作为上述金属填料,可以举出金、银、铜、镍、钯、锡、铝等金属颗粒。
其中优选金、银、铜。
上述金属填料的平均粒径优选为0.01nm~100μm、更优选为0.1nm~1μm。
上述平均粒径可以利用粒度分布计或电子显微镜(SEM)进行测定。
作为上述无机填料,优选导电性无机填料,更优选碳填料、金属填料,进一步优选碳填料。
上述共聚物为包含氟单体单元和具有酰胺键的聚合性乙烯基化合物单元的共聚物,本说明书中,有时记载为氟单体/具有酰胺键的聚合性乙烯基化合物共聚物。
本发明的组合物中,上述共聚物可以起到使上述无机填料分散在上述溶剂中的分散剂的功能。
作为上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物,出于进一步提高分散性和耐氧化性的原因,相对于全部单体单元,优选氟单体单元为99.9~0.1摩尔%、具有酰胺键的聚合性乙烯基化合物单元为0.1~99.9摩尔%。并且更优选氟单体单元为65~7摩尔%、具有酰胺键的聚合性乙烯基化合物单元为35~93摩尔%。另外,进一步优选氟单体单元为55~15摩尔%、具有酰胺键的聚合性乙烯基化合物单元为45~85摩尔%。另外,特别优选氟单体单元为45~20摩尔%、具有酰胺键的聚合性乙烯基化合物单元为55~80摩尔%。
具有酰胺键的聚合性乙烯基化合物单元大于99.9摩尔%时,耐氧化性可能会恶化。另外,具有酰胺键的聚合性乙烯基化合物单元小于0.1摩尔%时,表面活性能降低,分散性可能会恶化。
另外,特别是氟单体单元与具有酰胺键的聚合性乙烯基化合物单元的摩尔比(氟单体单元/具有酰胺键的聚合性乙烯基化合物单元)优选为0.07~1.50的范围、更优选为0.25~1.25的范围。进一步优选为0.25~0.82的范围。摩尔比若过小,则耐氧化性可能会恶化,摩尔比若过大,则分散性可能会恶化。
作为上述氟单体,可以举出:(1)具有与sp2杂化碳原子键合的氟原子的烯烃;(2)通式:CH2=CX-COORf(式中,X为Cl、H或烷基,Rf为氟代烷基)所表示的单体;(3)通式:CH2=CH-Rf(式中,Rf为氟代烷基)所表示的单体;(4)通式:CH2=CH-ORf(式中,Rf为氟代烷基)所表示的单体等。
作为上述烷基,可以举出碳原子数1~3的烷基,优选甲基。
作为上述氟代烷基,优选碳原子数1~12的直链或带支链的氟代烷基。
作为上述氟单体,出于能够将与构成聚合物主链的碳原子键合的氟原子导入到上述共聚物中、由此提高上述共聚物的耐氧化性的原因,优选(1),更优选为选自由偏二氟乙烯、三氟乙烯、四氟乙烯、六氟丙烯、三氟氯乙烯、单氟乙烯、三氟苯乙烯、以及通式:CH2=CFRf1(式中,Rf1为碳原子数1~12的直链或带支链的氟代烷基)所表示的氟单体组成的组中的至少一种,进一步优选为选自由偏二氟乙烯、三氟乙烯、四氟乙烯、六氟丙烯、三氟氯乙烯以及三氟苯乙烯组成的组中的至少一种。
另外,作为上述氟单体,优选为选自由四氟乙烯(TFE)、六氟丙烯(HFP)、三氟氯乙烯(CTFE)、偏二氟乙烯、三氟乙烯、单氟乙烯、氟代烷基乙烯基醚、氟代烷基乙烯、三氟丙烯、五氟丙烯、三氟丁烯、四氟异丁烯、六氟异丁烯、三氟苯乙烯以及通式:CH2=CFRf1(式中,Rf1为碳原子数1~12的直链或带支链的氟代烷基)所表示的氟单体组成的组中的至少一种,更优选为选自由TFE、CTFE、偏二氟乙烯和HFP组成的组中的至少一种,进一步优选为选自由TFE和偏二氟乙烯组成的组中的至少一种。
另外,从进一步提高分散性和耐氧化性的方面出发,上述氟单体优选为选自由氟化乙烯(1个以上的氢原子被氟原子取代的乙烯)和氟化丙烯(1个以上的氢原子被氟原子取代的丙烯)组成的组中的至少一种,更优选为选自由四氟乙烯(TFE)和六氟丙烯(HFP)组成的组中的至少一种。
上述聚合性乙烯基化合物具有酰胺键,除了酰胺键以外还具有聚合性乙烯基。上述酰胺键是指羰基与氮原子间的键合。
作为上述聚合性乙烯基,可以举出乙烯基、烯丙基、乙烯基醚基、乙烯基酯基、丙烯酰基等。
作为上述具有酰胺键的聚合性乙烯基化合物,可以举出N-乙烯基-β-丙内酰胺、N-乙烯基-2-吡咯烷酮、N-乙烯基-γ-戊内酰胺、N-乙烯基-2-哌啶酮、N-乙烯基-庚内酰胺等N-乙烯基内酰胺化合物、N-乙烯基甲酰胺、N-甲基-N-乙烯基乙酰胺等非环状的N-乙烯基酰胺化合物、N-烯丙基-N-甲基甲酰胺、烯丙基脲等非环状的N-烯丙基酰胺化合物、1-(2-丙烯基)-2-吡咯烷酮等N-烯丙基内酰胺化合物、(甲基)丙烯酰胺、N,N-二甲基丙烯酰胺、N-异丙基丙烯酰胺等丙烯酰胺化合物。
作为上述具有酰胺键的聚合性乙烯基化合物,还可以举出
[化1]
(式中,R1和R2独立地为H或碳原子数1~10的烷基)所表示的化合物、
[化2]
(式中,R1和R2独立地为H或碳原子数1~10的烷基)所表示的化合物等。
其中优选N-乙烯基内酰胺化合物或非环状的N-乙烯基酰胺化合物,更优选为选自由N-乙烯基-β-丙内酰胺、N-乙烯基-2-吡咯烷酮、N-乙烯基-γ-戊内酰胺、N-乙烯基-2-哌啶酮以及N-乙烯基-庚内酰胺组成的组中的至少一种,进一步优选为选自由N-乙烯基-2-吡咯烷酮以及N-乙烯基-2-哌啶酮组成的组中的至少一种,特别优选为N-乙烯基-2-吡咯烷酮。
上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物可以在无损于本发明组合物的效果的范围内具有氟单体单元和具有酰胺键的聚合性乙烯基化合物单元以外的其他单体单元。作为其他单体单元,可以举出乙烯基酯单体单元、乙烯基醚单体单元、在侧链具有聚乙二醇的(甲基)丙烯酸单体单元、在侧链具有聚乙二醇的乙烯基单体单元、具有长链烃基的(甲基)丙烯酸单体单元、具有长链烃基的乙烯基单体单元等。其他单体单元的合计可以为0~50摩尔%、可以为0~40摩尔%、可以为0~30摩尔%、可以为0~15摩尔%、也可以为0~5摩尔%。
上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物优选实质上仅由氟单体单元和具有酰胺键的聚合性乙烯基化合物单元形成。
上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物的重均分子量优选为10000以上、更优选为15000以上、进一步优选为20000以上、特别优选为30000以上。更优选为15000~500000、进一步优选为20000~300000、特别优选为30000~300000。上述重均分子量可以通过凝胶渗透色谱(GPC)求出。
本发明的组合物中,上述无机填料与上述共聚物的质量比(无机填料/共聚物)优选为0.1~100。上述质量比更优选为0.2以上、进一步优选为0.4以上,并且更优选为50以下、进一步优选为10以下、特别优选为5以下。
本发明的组合物中,即使上述共聚物为较少量(上述质量比较大),无机填料的分散性以及耐氧化性也优异。
本发明的组合物进一步包含溶剂。作为上述溶剂,可以举出水、有机溶剂,优选有机溶剂。
作为上述有机溶剂,例如可以举出N-甲基-2-吡咯烷酮、N,N-二甲基乙酰胺、二甲基甲酰胺等含氮系有机溶剂;丙酮、甲基乙基酮、环己酮、甲基异丁基酮等酮系溶剂;乙酸乙酯、乙酸丁酯等酯系溶剂;四氢呋喃、二氧六环、乙基溶纤剂、甲基溶纤剂、二甘醇二甲醚、三甘醇二甲醚等醚系溶剂;二甲苯、甲苯、溶剂石脑油等芳香族烃系溶剂;正戊烷、正己烷、正庚烷、正辛烷、正壬烷、正癸烷、正十一烷、正十二烷、矿物精油等脂肪族烃系溶剂;这些的混合溶剂;等等。
上述溶剂的量相对于上述无机填料100质量份优选为10万~1000万质量份、更优选为50万~500万质量份。
本发明的组合物优选为上述无机填料分散在上述溶剂中的分散液。本发明的组合物由于包含上述共聚物,因此上述无机填料非常良好地分散在上述溶剂中。
本发明的组合物可以为涂料组合物。
本发明的组合物可以根据用途等进一步包含其他成分。作为上述其他成分,可以举出氟系聚合物(其中不包含上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物)、非氟系聚合物、有机填料、电极活性物质等电极材料、油墨颜料等。
上述氟系聚合物是将含氟烯键式单体聚合而成的,可以是含氟烯键式单体与非含氟烯键式单体聚合而成的。含氟烯键式单体与非含氟烯键式单体分别可以使用1种或2种以上。
作为上述含氟烯键式单体,例如可以举出四氟乙烯、偏二氟乙烯、三氯氟乙烯、三氟氯乙烯、氟化乙烯、六氟丙烯、2,3,3,3-四氟丙烯(1234yf)、下述通式(i):
CX1 2=CX2(CF2)nX3 (i)
(式中,X1、X2和X3相同或不同,表示氢原子或氟原子,n表示1~10的整数)所表示的氟代烯烃、下述通式(ii):
CF2=CF-ORf2 (ii)
(式中,Rf2表示碳原子数1~5的全氟烷基)所表示的全氟(烷基乙烯基醚)等。
作为上述非含氟烯键式单体,可以举出乙烯、丙烯、1-丁烯、2-丁烯、氯乙烯、下述通式(iii):
[化3]
(式中,R11~R13各自独立地为氢原子、氯原子或碳原子数1~5的烷基,X11为主链由原子数1~19构成的分子量472以下的原子团)所表示的单体(iii)等。
作为上述单体(iii),优选下述式(iii-1):
[化4]
(式中,R11~R13如上所述,X111为主链由原子数1~18构成的分子量456以下的原子团)所表示的单体(iii-1)。
作为上述氟系聚合物,优选偏二氟乙烯均聚物、包含偏二氟乙烯和四氟乙烯的共聚物、包含偏二氟乙烯和单体(iii)的共聚物、包含偏二氟乙烯和四氟乙烯和单体(iii)的共聚物、包含偏二氟乙烯和四氟乙烯和六氟丙烯的共聚物、包含偏二氟乙烯和四氟乙烯和六氟丙烯和单体(iii)的共聚物、包含偏二氟乙烯和六氟丙烯和单体(iii)的共聚物等。
本发明的组合物可以适当地用作锂离子电池等二次电池的电极形成用组合物。
二次电池的电极中包含导电剂,但若导电剂的分散性差,则不能对电极整体赋予导电性、性能恶化。另外,若希望增加导电剂来解决该问题,则能量密度可能会降低。
本发明的组合物中,在上述无机填料为导电剂(碳填料等导电性无机填料)的情况下,其分散性也优异。另外,即使上述共聚物为较少量,也能够发挥出优异的分散性。其结果能够提高二次电池的性能。
另外,以往在电池领域中通常作为分散剂使用的PVP的耐氧化性低,在4.45V以上的高电压下发生分解,可能成为气体产生或电阻增加的原因。
本发明的组合物的耐氧化性优异,因此也能够适用于高电压的二次电池中。
另外,与作为分散剂使用PVP的情况相比,本发明的组合物在作为电极合剂浆料的情况下的粘度变化小。
将本发明的组合物用作二次电池的电极形成用组合物的情况下,优选包含上述导电性无机填料、上述共聚物和上述溶剂,可以进一步包含电极活性物质、粘合剂、增稠剂等。作为上述粘合剂,例如可以举出上述氟系聚合物(其中不包含上述氟单体/具有酰胺键的聚合性乙烯基化合物共聚物)。
本发明的组合物特别适合用作二次电池的正极形成用组合物。
本发明还涉及一种层积体,其具备基材、以及形成在上述基材上的由上述本发明的组合物形成的涂膜。
作为上述基材的材料,可以举出金属、陶瓷、树脂、玻璃等。
作为上述金属,可以举出铁、不锈钢、铜、铝、镍、钛等。作为上述陶瓷,可以举出陶器、磁器、氧化铝材、氧化锆材、氧化硅材等。作为上述树脂,可以举出聚对苯二甲酸乙二醇酯树脂、聚碳酸酯树脂、有机硅树脂、氟硅树脂、聚酰胺树脂、聚酰胺酰亚胺树脂、聚酰亚胺树脂、聚酯树脂、环氧树脂、聚苯硫醚树脂、酚树脂、丙烯酸类树脂、聚醚砜树脂等。
上述基材可以为二次电池用的集电体。作为上述集电体(正极集电体和负极集电体),例如可以举出铁、不锈钢、铜、铝、镍、钛等金属箔或者金属网等。其中,作为正极集电体,优选铝箔等,作为负极集电体,优选铜箔等。
本发明的层积体可以通过将本发明的组合物涂布于上述基材并根据需要进行干燥、固化、压制等来制造。
由上述组合物形成的涂膜可以直接形成在上述基材上,也可以隔着其他层来形成。
由上述组合物形成的涂膜的厚度取决于用途,例如可以为1~1000μm。
本发明的层积体能够适当地用作导电性构件。这种情况下,上述无机填料优选为导电性无机填料。
具备本发明的层积体的导电性构件也是本发明之一。上述导电性构件例如优选为二次电池的电极。
本发明还涉及一种分散剂,其是用于使无机填料分散在溶剂中的分散剂,其特征在于,其含有:氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物。
本发明的分散剂由于含有上述共聚物,因此与含有聚乙烯吡咯烷酮(PVP)等的分散剂相比,无机填料的分散性(无机填料相对于溶剂的分散性)以及耐氧化性优异。
另外,本发明的分散剂即使用量为较少量,无机填料的分散性以及耐氧化性也优异。
另外,本发明的分散剂即使经过长时间(例如制备后7天以上),也能够提供无机填料的分散性优异的组合物(无机填料分散液)。
另外,本发明的分散剂还能够提供粘度变化小的组合物(无机填料分散液)。
作为本发明的分散剂中的上述共聚物,可以使用与本发明的组合物中的氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物同样的共聚物,优选的示例也相同。
本发明的分散剂可以仅由上述共聚物形成。
关于作为应用本发明的分散剂的对象的无机填料和溶剂,可以举出与能够在本发明的组合物中使用的无机填料和溶剂同样的物质,优选的示例也相同。
本发明的分散剂优选以上述无机填料与上述共聚物的质量比(无机填料/共聚物)为0.1~100的比例使用。上述质量比更优选为0.2以上、进一步优选为0.4以上,并且优选为50以下、优选为10以下、特别优选为5以下。
本发明的分散剂即使用量为较少量(上述质量比较大),无机填料的分散性以及耐氧化性也优异。
本发明的分散剂优选为用于将上述无机填料分散在相对于100质量份的上述无机填料为10万~1000万质量份的上述溶剂中的分散剂,更优选为用于将上述无机填料分散在相对于100质量份的上述无机填料为50万~500万质量份的上述溶剂中的分散剂。
本发明的组合物、层积体和分散剂能够适当地用于要求无机填料的分散性、耐氧化性的各种领域中。
例如可适当地用于油墨、橡胶、导电性膜、电化学器件(电池等)等。其中优选用于二次电池、更优选用于二次电池的电极。
实施例
接着举出实施例更详细地说明本发明,但本发明并不仅限于这些实施例。
实施例和比较例中使用下述成分。
SWCNT:单层CNT(CNTs2、SUSN公司制造)
氧化铝:平均粒径0.5μm的氧化铝颗粒(市售品)
NMP:N-甲基-2-吡咯烷酮(水溶性有机溶剂、东京化成公司制造)
PVP K30:重均分子量4.0×104的聚乙烯吡咯烷酮(东京化成公司制造)
分散剂1:重均分子量4.6×104、四氟乙烯单元48mol%、N-乙烯基-2-吡咯烷酮单元52mol%的共聚物
分散剂2:重均分子量4.5×104、四氟乙烯单元36mol%、N-乙烯基-2-吡咯烷酮单元64mol%的共聚物
添加剂1:PVdF(聚偏二氟乙烯)(#7200、KUREHA制)
<分散液的制备>
实施例1
将SWCNT(10mg)和分散剂1(100mg)加入到NMP(100g)中,利用超声波(37kHz)进行1小时处理,制备SWCNT的分散液1。
实施例2
将实施例1的分散剂1由100mg变更为50mg,制备分散液2。
实施例3
将实施例1的分散剂1由100mg变更为20mg,制备分散液3。
实施例4
将实施例1的分散剂1由100mg变更为10mg,制备分散液4。
实施例5
将实施例3的分散剂1变更为分散剂2(20mg),制备分散液5。
实施例6
将实施例3的无机填料变更为氧化铝(10mg),制备分散液6。
实施例7
将实施例6的分散剂1变更为分散剂2(20mg),制备分散液7。
实施例8
向实施例3的分散液3中追加添加剂1(100mg),制备分散液8。
实施例9
向实施例5的分散液5中追加添加剂1(100mg),制备分散液9。
比较例1
将SWCNT(10mg)加入到NMP(100g)中,利用超声波(37kHz)进行1小时处理,制备SWCNT的分散液10。
比较例2
将SWCNT(10mg)和PVP K30(100mg)加入到NMP(100g)中,利用超声波(37kHz)进行1小时处理,制备SWCNT的分散液11。
比较例3
将比较例2的PVP K30由100mg变更为20mg,制备分散液12。
比较例4
向比较例3的分散液12中追加添加剂1(100mg),制备分散液13。
<分散性评价>
将分散液1~13在室温静置5小时,向5mL螺口管中加入各样品约2mL,目视观察确认有无沉淀。进一步将该分散液静置,确认7天后有无沉淀。将观察到沉淀的情况评价为×、未观察到沉淀的情况评价为○。
结果示于表1。
<耐氧化性评价>
进行基于LSV(线性扫描伏安法)法的测定,对耐氧化性进行评价。LSV测定中,使用1.0M的LiPF6作为电解质、使用碳酸亚乙酯与碳酸甲乙酯以体积比3:7混合而成的溶液作为标准测定溶剂。向标准测定溶剂中分别添加1.0重量%的PVP K30、分散剂1、分散剂2,进一步向各溶液中添加0.1质量%的SWCNT,制备3种测定溶液。向测定容器中加入预先制备的各测定溶液,并浸入作为工作电极的铂电极、作为对电极和参比电极的锂电极,将其作为LSV测定用电池单元,由OCV(开路电压,Open Circuit Voltage)以扫描速度5mV/s在氧化侧进行电位扫描至8V(vs.Li+/Li)为止,测定反应起始电位。反应起始电位被判断为应答电流达到5mA/cm2的时刻的电位。
结果示于表2。
[表2]
分散剂 | LSV测定结果[V vs Li/Li+] |
分散剂1 | 6.75 |
分散剂2 | 6.73 |
PVP K30 | 6.70 |
Claims (8)
1.一种组合物,其特征在于,其包含:无机填料;氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物;以及溶剂,
所述无机填料为选自由碳填料和陶瓷填料组成的组中的至少一种,
所述氟单体为选自由偏二氟乙烯、三氟乙烯、四氟乙烯、六氟丙烯、三氟氯乙烯、单氟乙烯、三氟苯乙烯以及通式:CH2=CFRf1所表示的氟单体组成的组中的至少一种,其中,CH2=CFRf1中,Rf1为碳原子数1~12的直链或带支链的氟代烷基,
所述具有酰胺键的聚合性乙烯基化合物为选自由N-乙烯基内酰胺化合物、非环状的N-乙烯基酰胺化合物、非环状的N-烯丙基酰胺化合物和N-烯丙基内酰胺化合物组成的组的至少一种,
所述共聚物中,相对于全部单体单元,氟单体单元为55~15摩尔%,具有酰胺键的聚合性乙烯基化合物单元为45~85摩尔%,其他单体单元为0~5摩尔%,
所述无机填料与所述共聚物的质量比即无机填料/共聚物为0.1~1.0。
2.如权利要求1所述的组合物,其中,所述氟单体为选自由四氟乙烯和六氟丙烯组成的组中的至少一种氟单体。
3.如权利要求1或2所述的组合物,其中,所述无机填料为碳填料。
4.如权利要求1或2所述的组合物,其中,所述无机填料为纤维状碳。
5.如权利要求1或2所述的组合物,其中,所述无机填料为碳纳米管。
6.一种层积体,其具备基材、以及形成在所述基材上的由权利要求1~5中任一项所述的组合物形成的涂膜。
7.一种导电性构件,其具备权利要求6所述的层积体。
8.共聚物作为分散剂的应用,其是用于使无机填料分散在溶剂中的分散剂,所述共聚物是氟单体与具有酰胺键的聚合性乙烯基化合物的共聚物,其中,
所述无机填料为选自由碳填料和陶瓷填料组成的组中的至少一种,
所述氟单体为选自由偏二氟乙烯、三氟乙烯、四氟乙烯、六氟丙烯、三氟氯乙烯、单氟乙烯、三氟苯乙烯以及通式:CH2=CFRf1所表示的氟单体组成的组中的至少一种,其中,CH2=CFRf1中,Rf1为碳原子数1~12的直链或带支链的氟代烷基,
所述具有酰胺键的聚合性乙烯基化合物为选自由N-乙烯基内酰胺化合物、非环状的N-乙烯基酰胺化合物、非环状的N-烯丙基酰胺化合物和N-烯丙基内酰胺化合物组成的组的至少一种,
所述共聚物中,相对于全部单体单元,氟单体单元为55~15摩尔%,具有酰胺键的聚合性乙烯基化合物单元为45~85摩尔%,其他单体单元为0~5摩尔%,
所述无机填料与所述共聚物以质量比即无机填料/共聚物为0.1~1.0的比例使用。
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