CN106893545B - 用于电容去离子电极的粘结剂与其形成方法 - Google Patents
用于电容去离子电极的粘结剂与其形成方法 Download PDFInfo
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Abstract
本发明提供用于电容去离子电极的粘结剂及其形成方法。所述粘结剂是由疏水性的聚醚多元醇、二异氰酸酯、与具有疏水性侧链的二醇反应而成。上述粘结剂可粘结活性材料,以形成电容去离子电极。活性材料与粘结剂的重量比可介于90:5至90:25之间。
Description
技术领域
本发明是关于电极的粘结剂,更特别关于用于电容去离子电极的粘结剂,及其形成方法。
背景技术
碳电极在制备的过程中常需使用高分子粘结剂(polymer binder),用以粘结电极材料颗粒并固定电极材料颗粒与集电板(current collector)。高分子粘结剂接合的效果对电极的功能影响甚巨,故高分子粘结剂特性的调控非常重要。一般电极制备常使用氟系高分子作为粘结剂,其中以PVDF(polyvinylidene fluoride)最为普遍。PVDF粘结剂可形成化学安定网络结构(chemically inert network),其机械强度可有效且大范围支撑活性材料颗粒间的相互连结,于适当用量下不会影响到活性材料的电化学特性。然而PVDF粘结剂具有成本高、可挠性(flexibility)低、及环境友善性低等缺点。
综上所述,目前亟需新的粘结剂组成取代PVDF粘结剂,以用于粘结电极材料颗粒并将其固定至集电板。
发明内容
本发明的目的在于提供一种可取代PVDF粘结剂、用于电极的新型粘结剂,以用于粘结电极材料颗粒并将其固定至集电板。
本发明一实施例提供的用于电容去离子电极的粘结剂,包括:具有疏水性的聚醚多元醇、二异氰酸酯、与具有疏水性侧链的二醇反应而成的产物。
本发明一实施例提供的用于电容去离子电极的粘结剂的形成方法,包括:混合疏水性的聚醚多元醇、二异氰酸酯、与具有疏水性侧链的二醇,反应形成粘结剂。
本发明的优点在于:本发明利用具有疏水性的聚醚多元醇、二异氰酸酯与具有疏水性侧链的二醇反应而成的产物(聚氨酯)作为粘结剂,该聚氨酯在干燥时,具有良好热稳定性、高化学稳定性、且能被电解质湿润,因此含有上述聚氨酯作为粘结剂的电极具有多种用途,例如:上述电极可搭配对电极与两者之间的水相溶液以作电容去离子之用,或将上述聚氨酯作为粘结剂的电极用于其他诸如锂电池、燃料电池、超级电容器或储氢装置等的装置中。
附图说明
图1A是不同分子量的PU电极的虚部阻抗对实部阻抗的曲线图;
图1B是图1A的部份放大图;
图2是不同分子量的PU电极的相角对频率的曲线图;
图3A是PU电极与PVDF电极的虚部阻抗对实部阻抗的曲线图;
图3B是图3A的部份放大图;
图4是PU电极与PVDF电极的相角对频率的曲线图。
具体实施方式
本发明一实施例提供的聚氨酯,是由1摩尔份的疏水性的聚醚多元醇(HO-R2-OH)、3至20摩尔份的二异氰酸酯(ONC-R1-NCO)、与1至6摩尔份的具有疏水性侧链的二醇(HO-R3-OH)反应而成。上述反应如式1所示:
在式1中,R1、R2、与R3取决于二异氰酸酯、疏水性的聚醚多元醇、与具有疏水性侧链的二醇的种类,而x与y取决于疏水性的聚醚多元醇与具有疏水性侧链的二醇的摩尔比例。
另一方面,聚氨酯为无规共聚物,即上述对应x的重复单元与对应y的重复单元的排列方式为无规。
在一实施例中,疏水性的聚醚多元醇种类的碳氢主链(hydrocarbon backbone)为具高挠曲性与疏水特性,而具有疏水性侧链的二醇种类则为控制链段软硬程度,以及侧链疏水增加粘结剂防水性。
在一实施例中,聚氨酯的数目平均分子量大于1.6×105以上。若聚氨酯的数目平均分子量过低,则无法有效粘结活性材料以作为电极。若聚氨酯的数目平均分子量过高,则粘度(viscosity)过高且结构弹性(elasticity)过低,不利于配制电极浆料并降低电极效能。
举例来说,二异氰酸酯可为六亚甲基二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、或上述的组合。
疏水性的聚醚多元醇可为聚丁二醇、聚丙二醇、或上述的组合。疏水性的聚醚多元醇的挠曲性高且具疏水特性。在一实施例中,聚醚多元醇的数目平均分子量介于1000至5000之间。若疏水性的聚醚多元醇的数目平均分子量过低,分子结构会较硬及脆,不易服帖。若聚醚多元醇的数目平均分子量过高,则分子结构会较软,且内聚强度变弱。具有疏水性侧链的二醇可为C12-26的单脂肪酸甘油酯、C12-26的二聚脂肪酸(dimer acids)、或上述的组合。
具有疏水性侧链的二醇可作为聚氨酯的硬段,控制聚氨酯的软硬程度。另一方面,具有疏水性侧链的二醇的疏水侧链可增加聚氨酯的疏水性,且侧链碳数愈高则疏水性愈高。
在一实施例中,可混合90重量份的活性材料与5至25重量份的粘结剂如上述聚氨酯、与溶剂(如N-甲基吡咯烷酮(NMP)、异丙醇、乙醇、或上述的组合)以形成浆料。接着将浆料涂布于集电板(如铜、铝、钛、其他金属、或上述的合金)上烘干,即形成电极。若粘结剂的比例过低,则无法有效粘结活性及导电材料与集电板而有脱落问题。若粘结剂的比例过高,则可能会增加电极电阻而降低电极效能。举例来说,活性材料可为活性碳材、纳米碳管、石墨烯、或上述的组合等高比表面积的材料。上述活性材料的比表面积介于300m2/g至3000m2/g之间,且其孔洞大小介于1至1000nm。若活性材料的比表面积过小,则会影响电吸附离子容量。若活性材料导电度不足(如活性碳材料),可添加5至20重量份的导电材料帮助导电,且导电材料可为石墨、碳黑、乙炔黑、或上述的组合。但值得注意的是,添加量过多(如石墨或碳黑)的导电材料,会使活性碳的材料重量比例含量下降,导致吸附离子的有效面积降低,进而使其吸附电容下降。
上述聚氨酯在干燥时,具有良好热稳定性、高化学稳定性、且能被电解质湿润,因此含有上述聚氨酯作为粘结剂的电极具有多种用途。在一实施例中,上述电极可搭配对电极与两者之间的水相溶液,以作电容去离子之用。在其他实施例中,上述聚氨酯作为粘结剂的电极可用于其他装置如锂电池、燃料电池、超级电容器、或储氢装置。
为了让本发明的上述和其他目的、特征、和优点能更明显易懂,下文特举数实施例作详细说明如下:
实施例
实施例1
取1摩尔份的聚丁二醇(PTMEG,购自立大化工,数目平均分子量为2000)与3摩尔份的硬脂酸甘油酯(GMS)加入300mL的除水NMP中,加热至70℃形成均相溶液。接着将上述溶液降温至50℃后,将3摩尔份的甲苯二异氰酸酯(TDI)加入上述溶液,待温度稳定后再加热上述反应物至70℃并于70℃下反应。在反应3小时后,每隔一小时取样确认反应物中的-NCO官能基残留量,待-NCO官能基残留量不再降低后,可进一步添加溶剂稀释产物,再加入额外TDI以增加产物分子量。上述链延长反应可进行多次,即可得多种不同数目平均分子量的聚氨酯。PTMEG与TDI(起始用量与后续添加量的总合)的摩尔比介于1:6至1:16之间。聚氨酯产物依数目平均分子量高低可分为含6摩尔份TDI的PU(A)、含7摩尔份TDI的PU(B)、含8摩尔份TDI的PU(C)、含10.5摩尔份TDI的PU(D)、与含13.5摩尔份TDI的PU(E),其数目平均分子量如表1所示。
秤取80重量份的活性碳(activated carbon,AC)作为活性材料、10重量份的石墨粉(购自EMAXWIN)作为导电材、与10重量份上述制备的聚氨酯溶液(15wt%,PU(A)至PU(E))作为粘结剂,均匀搅拌24小时使之成为糊状浆料。接着以涂布间隙300μm的刮刀将糊状物均匀涂布在50μm钛箔上,送入120℃烘箱中烘干4小时,完成PU电极。
比较例
秤取80重量份的活性碳(activated carbon,AC)作为活性材料、10重量份的石墨粉(购自EMAXWIN)作为导电材、与10重量份的聚偏二氟乙烯(Poly(vinylidene fluoride,PVDF)溶液(5wt%,数目平均分子量为534,000,购自Aldrich)作为粘结剂,均匀搅拌24小时使之成为糊状浆料。接着以涂布间隙300μm的刮刀将糊状物均匀涂布在50μm钛箔上,送入120℃烘箱中烘干4小时,完成PVDF电极。
粘结剂最基本的要求是对高比表面积活性材料、导电材料、与集电板有好的粘着性,利用万能拉力机测定活性碳涂层在钛集电板的剥离强度。将制备好的碳电极裁切为2.5cm宽的长条状,再将标准胶带粘上、并以2公斤滚轮来回压合3次,即可制备成T peel拉伸的样品,以万能拉力机定速率30cm/min测试剥离强度,荷重模头显示的力量数值即是剥离强度,单位为kg/25mm。上述粘结剂的剥离强度如表1所示。
表1、不同分子量PU粘结剂的剥离强度
较低分子量的PU(A)及PU(B)其分子特性较为软粘且不成膜,以致电极无法完整成膜,因此活性碳涂层在集电板上易剥离,活性碳分子之间作用力低。由剥离强度的结果也可看出,较低分子量的PU粘结剂接着强度差。随着PU粘结剂分子量提高,可看出PU(C)、(D)、(E)接着强度有提升趋势,由于分子量越大,PU弹性体所含极性胺基比例愈高,与碳材间的接着作用力愈佳,因而粘结剂展现的强度愈高、表面更不沾粘。如表1所示,某些PU粘结剂的接着强度优于PVDF。
接着以循环伏安法(cyclic voltammetry,CV)分析PU电极与PVDF电极的电容值。测试溶液为0.5M NaCl水溶液,工作电极面积1cm x 1cm,对电极为白金线,参考电极为氯化银电极(AgCl/Ag),电位扫描范围为-0.5~0.5V,扫描速率为10mV/s,对CV曲线积分得到的电荷变化量,除以电位窗及电极活性材料重量即得电极的比电容值。
在剥离强度测试(peel test)中得知较低分子量的PU(A)及PU(B)会导致电极涂布的均匀性及接着强度差,以致电极无法完整成膜而无法测得比电容值。如表2所示,随着PU粘结剂分子量提高,可观察到电极涂布均匀性及接着强度有提升趋势(比电容值也从54.0F/g增加至91.1F/g)。由于高分子量的PU粘结剂可形成网状结构,可大范围包覆颗粒、藉由网状强度支撑使颗粒相互连结。较长的PU分子链可避免发生小分子粘结剂阻塞活性碳材孔洞结构,进而提高其比电容值。
表2
另外,利用交流阻抗频谱分析(electrochemical impedance spectroscopy,EIS)进行比较不同分子量的PU电极的阻抗特性,如图1A与图1B所示。图1B是图1A的部份放大图。在图1A与图1B中,纵轴读值为虚部阻抗(capacitance impedance),而横轴读值为实部阻抗电阻值(resistance)。由图1A可知,采用高分子量的PU(E)作为粘结剂的电极,在中高频区域(半圆区间)所产生的阻值,比采用低分子量PU(C)及PU(D)作为粘结剂的电极低,因此具有较高的比电容值。而不同频率与相角的变化如图2所示,PU(E)电极在低频区域,其相角明显高于PU(C)及PU(D)电极,显示PU(E)电极较偏向电容反应。推估应是PU(E)的较长分子链不易深入活性碳材孔洞结构,降低孔洞被堵塞的情形,有助于减少碳电极的界面电阻。综上所述,PU(E)电极具有较高比电容值。
实施例2
固定活性碳与石墨粉的重量比为80:10,并调整PU粘结剂的添加重量比为5至20重量份,以确认PU粘结剂添加比例对电容的影响,如表3所示。结果显示当碳材、导电材与PU重量比为80:10:5的时候,碳电极接着性为中,而随着PU添加比例增加而提升至高,此外,不同PU添加比例的碳电极均匀性皆为高。在电容表现的方面,活性碳与PU粘结剂的重量比为80:10、80:15与80:20的电极比电容值相近,而以活性碳与PU粘结剂的重量比为80:15时有最高比电容值为101F/g,值得注意的是,在活性碳与PU粘结剂的重量比为80:5时,电极比电容值67.1F/g表现最低,推论原因当添加的PU粘结剂量过少时,会影响碳颗粒与集电板间有效的连结性,因此反而造成更大的界面电阻而使电容表现较差。
表3
实施例3
取PU(E)电极与PVDF电极进行循环伏安分析比较,如表4所示。结果显示PVDF电极的比电容值为87.3F/g,而PU(E)电极的比电容值为91.1F/g,优于PVDF电极。
表4
粘结剂 | 活性碳:石墨:粘结剂 | 电极均匀性 | 接着性 | 比电容值(F/g) |
PU(E) | 80:10:10 | 高 | 高 | 91.1 |
PVDF | 80:10:10 | 高 | 高 | 87.3 |
另外,利用交流阻抗频谱分析(electrochemical impedance spectroscopy,EIS)进行比较PU电极与PVDF电极的阻抗特性,如图3A与图3B所示。图3B是图3A的部份放大图。由图3A可知,采用PU(E)作为粘结剂的电极,在中高频区域(半圆区间)所产生的阻值,比采用PVDF作为粘结剂的电极低,因此具有较高的比电容值。而不同频率与相角的变化如图4所示,PU(E)电极在低频区域,其相角较PVDF电极接近90°,显示相较于PVDF电极,PU(E)电极较偏向电容反应,因此以PU(E)粘结剂制备电极的比电容值高于PVDF电极。综上所述,PU可取代PVDF作为电极中活性材料的粘结剂。
虽然本发明已以数个实施例发明如上,然其并非用以限定本发明,任何本技术领域中具有通常知识者,在不脱离本发明的精神和范围内,当可作任意的更动与润饰,因此本发明的保护范围当视后附的申请专利范围所界定者为准。
Claims (15)
1.一种用于电容去离子电极的粘结剂,是由:
1摩尔份的疏水性的聚醚多元醇、3至20摩尔份的二异氰酸酯与1至6摩尔份的具有疏水性侧链的二醇反应而成的产物,
其中所述二异氰酸酯为六亚甲基二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、或上述的组合;
其中,
所述粘结剂是用以粘结电极中的活性材料,且所述活性材料与所述粘结剂的重量比介于90:5至90:25之间;
所述粘结剂的数目平均分子量大于1.6×105;
所述疏水性的聚醚多元醇的数目平均分子量介于1000~5000之间;以及
所述活性材料的比表面积介于300m2/g至3000m2/g之间,且其孔洞大小介于1至1000nm。
2.如权利要求1所述的用于电容去离子电极的粘结剂,其中所述疏水性的聚醚多元醇为聚丁二醇、聚丙二醇、或上述的组合。
3.如权利要求1所述的用于电容去离子电极的粘结剂,其中所述具有疏水性侧链的二醇为C12-26的单脂肪酸甘油酯、C12-26的二聚脂肪酸、或上述的组合。
4.如权利要求1所述的用于电容去离子电极的粘结剂,其中所述活性材料为活性碳材、纳米碳管、石墨烯、或上述的组合。
5.如权利要求4所述的用于电容去离子电极的粘结剂,其中该电极更包含5至20重量份的导电材料,且该导电材料包括石墨、碳黑、乙炔黑、或上述的组合。
6.一种用于电容去离子电极的粘结剂的形成方法,是:
混合1摩尔份的疏水性的聚醚多元醇、3至20摩尔份的二异氰酸酯与1至6摩尔份的具有疏水性侧链的二醇,反应形成粘结剂,
其中所述二异氰酸酯为六亚甲基二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、或上述的组合;
其中,
所述粘结剂是用以粘结电极中的活性材料,且所述活性材料与所述粘结剂的重量比介于90:5至90:25之间;
所述粘结剂的数目平均分子量大于1.6×105;
所述疏水性的聚醚多元醇的数目平均分子量介于1000~5000之间;以及
所述活性材料的比表面积介于300m2/g至3000m2/g之间,且其孔洞大小介于1至1000nm。
7.如权利要求6所述的用于电容去离子电极的粘结剂的形成方法,其中所述疏水性的聚醚多元醇为聚丁二醇、聚丙二醇、或上述的组合。
8.如权利要求6所述的用于电容去离子电极的粘结剂的形成方法,其中所述具有疏水性侧链的二醇为C12-26的单脂肪酸甘油酯、C12-26的二聚脂肪酸、或上述的组合。
9.如权利要求6所述的用于电容去离子电极的粘结剂的形成方法,其中所述活性材料为活性碳材、纳米碳管、石墨烯、或上述的组合。
10.如权利要求9所述的用于电容去离子电极的粘结剂的形成方法,其中所述电极更包含5至20重量份的导电材料,且所述导电材料为石墨、碳黑、乙炔黑、或上述的组合。
11.一种电容去离子电极,包括:
活性材料,
用以粘结活性材料并固定活性材料与集电板的粘结剂;
其中,所述粘结剂是由1摩尔份的疏水性的聚醚多元醇、3至20摩尔份的二异氰酸酯与1至6摩尔份的具有疏水性侧链的二醇反应而成的产物,
其中所述二异氰酸酯为六亚甲基二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、或上述的组合;
其中,
所述活性材料与所述粘结剂的重量比介于90:5至90:25之间;
所述粘结剂的数目平均分子量大于1.6×105;
所述疏水性的聚醚多元醇的数目平均分子量介于1000~5000之间;以及
所述活性材料的比表面积介于300m2/g至3000m2/g之间,且其孔洞大小介于1至1000nm。
12.如权利要求11所述的电容去离子电极,其中所述疏水性的聚醚多元醇为聚丁二醇、聚丙二醇、或上述的组合。
13.如权利要求11所述的电容去离子电极,其中所述具有疏水性侧链的二醇为C12-26的单脂肪酸甘油酯、C12-26的二聚脂肪酸、或上述的组合。
14.如权利要求11所述的电容去离子电极,其中所述活性材料为活性碳材、纳米碳管、石墨烯、或上述的组合。
15.如权利要求11所述的电容去离子电极,其中所述电极更包含5至20重量份的导电材料,且所述导电材料为石墨、碳黑、乙炔黑、或上述的组合。
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CN106893545A (zh) | 2017-06-27 |
US20170174820A1 (en) | 2017-06-22 |
TWI568792B (zh) | 2017-02-01 |
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