CN1194310A - 在活性金属材料表面通过电化学氧化获得聚合物膜层的方法 - Google Patents
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Abstract
一种在活性金属材料表面通过电化学氧化获得聚合物膜层的方法,其特征在于:电化学溶液由以液态氯代烷烃作溶剂,以铵根阳离子中的烃基碳在六个以下的季铵盐为支特电解质,及形成聚合物的单体物质三部分构成,支持电解质浓度在0.01~0.5mol/l,单体物质浓度在10-3~10mol/l。本发明特别适合于活性金属材料,且操作程序和工艺较为简单。
Description
本发明涉及金属材料的表面处理技术,特别提供了一种在活性金属材料表面通过电化学氧化获得聚合物膜层的方法。
电化学聚合方法作为一种化学修饰电极技术方法,与其它方法相比,1)在电化学聚合成膜过程中,膜缺陷或较薄处的电流密度较大,因而有自身修复或完善的功能;2)由于膜是从基体表面上直接和逐渐形成,所以与基体的结合较好;3)厚度可以根据聚合时间或所消耗的电量进行控制,所以由于这种方法可以在电极表面获得均匀、附着性好和可控厚度的性能优良的功能性或保护性的聚合物膜层,已开始受到各有关方面学者的关注。
在惰性材料电极上,由于电极是惰性的,电化学聚合可以在很广泛的条件(如溶剂、支持电解质和电极电位或槽压等)下实现表面聚合物膜的制备,而电极基体本身不会发生显著的变化,这方面的研究探讨已有一些文献报道,如乙腈作溶剂时,呋喃在铂电极上的电化学氧化聚合(M.J.Gonzalez-Tejera,I.Carrillo,I.Hernandez-Fuentes,Synthetic Metals,73,1995:p135)。
随着经济技术的发展,在活性金属材料(指除了铂、金等化学性质稳定的金属及其合金以外的金属及合金)表面处理上功能性或保护性覆层的要求日益增多,当电极是活性的或惰性较差时,由于电化学氧化聚合往往需较高的氧化电位,活性材料电极会在通常所用的介质(如水、乙腈等的溶液)中阳极溶解或氧化,或与单体聚合反应竞争部分地被氧化,其结果,或根本无法得到聚合物膜层,或由于部分氧化破坏使该电极(被处理的器件)机械性能或强度发生损失,如果该材料电极是精密或细小器件,这种性能的损失将是严重和不允许的。在水溶液中,有人尝试采用将铁电极(活性金属材料)进行前处理以及分步施加阳极电位的作法,在铁电极表面获得了聚苯胺防护膜层(赵颖力,宋诗哲,李国华,中国腐蚀与防护学报,11(3),1991:p246)。虽然最终得到了聚苯胺防护层,但聚合初期铁电极一定程度的氧化难以避免,而且操作程序或工艺过程相当烦琐。
本发明提供了一种在活性金属材料表面通过电化学氧化获得聚合物膜层的方法,其特征在于:电化学溶液由以液态氯代烷烃作溶剂,以铵根阳离子中的烃基碳在六个以下的季铵盐为支特电解质,及形成聚合物的单体物质三部分构成,支持电解质浓度在0.01~0.5mol/L,单体物质浓度在10-3~10mol/L。
本发明用具有较高抗电化学氧化能力的液态氯代烷烃作溶剂,这类溶剂没有强的配位性,也基本没有与活性金属离子发生反应的倾向;用溶于所用溶剂并且本身具有较好的电化学稳定性的季铵(铵根阳离子中的烃基碳在六个以下)盐类物质作支持电解质;用欲形成聚合物的单体物质作聚合的主要原料,这类物质是可以通过电化学氧化形成阳离子自由基或自由基并发生聚合反应的有机化合物。上述三部分组成电化学溶液体系,以欲被在其表面制备聚合物膜的金属材料作阳极,进行恒电位、恒电流或电位循环扫描的电化学氧化操作,诱导单体聚合形成聚合物膜层。
所用溶剂和支持电解质均需要进行较严格的除水干燥,视所用溶剂、支持电解质以及单体物质的具体纯度和工艺要求,有时需要对它们作必要的纯化处理。为了消除氧的影响,在聚合之前,电化学溶液体系应除氧,在聚合操作过程中,应保持无氧状态。
在电极上没有聚合过程发生的条件下,本发明所用的溶剂和支持电解质在一定的阳极电位,如2.0V(vs.SCE)以上,会有一定程度的自身氧化。但这种作用在本发明中,会被电氧化聚合反应所形成的聚合物膜迅速抑制。因此,即使工作电极的电位较高,亦不会产生溶剂或支持电解质的明显氧化现象。
本发明可用各种形式如三电极或二电极的电化学池。总之,本发明具有下述优点:
1.可实现在活性金属材料电极上需较高电极电位的电化学氧化诱导的聚合反应的发生和相应聚合物膜层的制备;
2.活性金属本身在聚合物膜形成的过程中,不发生因氧化引起的性能或强度的明显损失;
3.可避免水的氧化析氧对膜层性能的影响以及水的氧化还原所引起的副反应对聚合过程的不利干扰;
4.工艺过程简单,不需要复杂的前处理。
下面通过实施例详述本发明。
实施例1
在三电极电化学池中,铁(工业纯)电级作为工作电极,辅助电极是大面积的铂片,参比电极用饱和甘汞电极(SCE)时,以二氯甲烷作溶剂,高氯酸四丁基铵作支持电解质(0.1mol/L),苯作为单体物质(0.3mol/L),在3.5V(vs.SCE)恒电位操作,即可在铁电极表面获得聚合物层。
实施例2
同实施例一电化学池条件,以1,2-二氯乙烷作溶剂,六氟磷酸四丁基铵作支持电解质(0.2mol/L),用氯乙烯作为单体物质(约0.3mol/L),在3V(vs.SEC)恒电位操作,在铁电极表面获得聚合物层。
实施例3
以不锈钢(18-8)作工作电极,其它电化学池条件与实施例一相同,以1,2-二氯乙烷作溶剂,高氯酸四丁基铵作支持电解质(0.2mol/L),用苯胺作单体物质(0.5mol/L),在4V(vs.SCE)的电极电位下恒电位操作,在不锈钢表面获得聚合物层。
实施例4
以铜(纯度99.9%)作工作电极,其它电化学池条件同实施例一,以1,2-二氯乙烷作溶剂,六氟磷酸四丁基铵作支持电解质(0.2mol/L),用联苯作为单体物质(0.15mol/L),在2V(vs.SCE)恒电位操作,在铜电极表面获得聚合物层。
实施例5
同实施例1电化学池条件,以氯代环已烷作溶剂,高氯酸四己基铵作支持电解质(0.2mol/L),用氯乙烯作为单体物质(约0.3mol/L),在3V(vs.SCE)恒电位操作,在铁电极表面获得聚合物层。
实施例6
以镍(99.99%)作工作电极,其它电化学池条件同实施例一,以1,4-二氯环乙烷作溶剂,六氟磷酸四已基铵作支持电解质(0.2mol/L),用氯乙烯作为单体物质(约0.3mol/L),在3V(vs.SCE)恒电位操作,在镍电极表面获得聚合物层。
实施例7
同实施例1电化学池条件,以1,2-二氯乙烷作溶剂,六氟磷酸四丁基铵作支持电解质(0.1mol/L),用呋喃作为单体物质(0.5mol/L),在2.3V(vs.SCE)恒电位操作,在铁电极表面获得聚合物层。
实施例8
同实施例1电化学池条件,以1,2-二氯乙烷作溶剂,四氟磷酸四丁基铵作支持电解质(0.1mol/L),用噻吩作为单体物质(0.5mol/L),在2.5V(vs.SCE)恒电位操作,在铁电极表面获得聚合物层。
实施例9
同实施例1电化学池条件,以1,2-二氯乙烷作溶剂,高氯酸四丁基铵作支持电解质(0.1mol/L),用吡咯作为单体物质(0.5mol/L),在2.5V(vs.SCE)恒电位操作,在铁电极表面获得聚合物层。
实施例10
以黄铜(H68)作工作电极,其它电化学池条件同实施例1.以二氯甲烷作溶剂,高氯酸四丁基铵作支持电解质(0.1mol/L),用邻二苯胺作为单体物质(0.2mol/L),在2.5V(vs.SCE)恒电位操作,在黄铜电极表面获得聚合物层。
实施例11
以铁(工作纯)电极作阳极的二电极电化学池,以1,2-二氯乙烷作溶剂,六氟磷酸四丁基铵作支持电解质(0.1mol/L),用吡咯作为单体物质(0.5mol/L),恒电流2mA/cm2操作,在铁电极表面获得聚合物层。
实施例12
以铜(99.9%)电极作阳极的二电极电化学池,以1-氯辛烷作溶剂,高氯酸四己基铵作支持电解质(0.1mol/L),用苯胺作为单体物质(0.5mol/L),恒电流0.05mA/cm2操作,在铜电极表面获得聚合物层。
实施例13
以不锈钢(18-8)电极作阳极的二电极电化学池,以二氯甲烷作溶剂,高氯酸四丁基铵作支持电解质(0,.1mol/L),用苯胺作为单体物质(0.5mol/L),恒电流0.05mA/cm2操作,在不锈钢电极表面获得聚合物层。
实施例14
以铁(工业纯)电级作阳极的二电极电化学池,以1,4-二氯丁烷作溶剂,高氯酸四己基铵作支持电解质(0.1mol/L),用联苯作为单体物质(0.2mol/L),恒电流3mA/cm2操作,在铁电极表面获得聚合物层。
实施例15
以铜(99.9%)电极作阳极的二电极电化学池,以1,2-二氯乙烷仟溶剂,高氯酸四丁基铵作支持电解质(0.1mol/L),用丙烯作为单体物质(约0.1mol/L),恒电流2mA/cm2操作,在铜电极表面获得聚合物层。
实施例16
以铁(工业纯)电级作阳极的二电极电化学池,以1-氯-2-甲基丁烷作溶剂,高氯酸四己基铵作支持电解质(0.1mol/L),用联苯作为单体物质(0.5mol/L),恒电流0.05mA/cm2操作,在铁电极表面获得聚合物层。
实施例17
同实施例1电化学池条件,以二氯甲烷作溶剂,高氯酸四乙基铵作支持电解质(0.1mol/L),用苯胺作为单体物质(0.5mol/L),在3.0~-0.5V(vs.SCE)循环电位扫描(100mV/s)操作,在铁电极表面获得聚合物层。
实施例18
以铜(99.9%)作工作电极,其它三电极电化学池条件同实施例1,以1,2-二氯乙烷作溶剂,高氯酸四丁基铵作支持电解质(0.1mol/L),用联苯作为单体(0.15mol/L),在3.0~-0.5V(vs.SCE)循环电位扫描(100mV/s)操作,在铜电极表面获得聚合物层。
Claims (1)
1.一种在活性金属材料表面通过电化学氧化获得聚合物膜层的方法,其特征在于:电化学溶液由以液态氯代烷烃作溶剂,以铵根阳离子中的烃基碳在六个以下的季铵盐为支特电解质,及形成聚合物的单体物质三部分构成,支持电解质浓度在0.01~0.5mol/L,单体物质浓度在10-3~10mol/L。
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