CN113322670B - 高导电有机纤维、导电纱以及导电纤维结构体及制备方法 - Google Patents
高导电有机纤维、导电纱以及导电纤维结构体及制备方法 Download PDFInfo
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Abstract
本发明公开一种高导电有机纤维、导电纱以及导电纤维结构体及制备方法,将分散在溶剂中的一维导电纳米材料及粘结剂浆料,涂敷在连续纤维表面,通过控制纤维涂覆工艺中的浸润纤维液滴尺寸,实现浸润液膜及导电层均匀包覆纤维表面,控制导电层厚度,交替涂敷具有一定导电性和渗透性的粘结层浆料,粘结层与一维导电纳米材料网络形成连续粘结层,制成的高导电纤维具有良好物理特性(耐磨性,延伸稳定性),纤维比电阻在100~104欧姆/厘米可调节,实现高速连续化生产,解决了现有高导电性纤维在良好导电性、应变电导稳定性、耐折弯性、耐摩性、低成本和高生产效率不能综合具备的问题,在智能纺织品、航空航天、国防军工等领域具有广泛的应用前景。
Description
技术领域
本发明涉及导电纤维技术领域,具体为高导电有机纤维、导电纱以及导电纤维结构体及制备方法。
背景技术
赋予有机纤维高导电性具有重要的应用价值,以导电有机纤维为基础,在众多应用领域可以制成各种具有新性能的产品,例如在生物医学领域,以织造性能良好的导电纤维为信号传输线,可以制成人体生理指标监测服装,对人体表心电、血氧、血糖、脉搏进行实时监测;在消费电子产品领域,将导电纤维与红外发射材料复合,可以制成红外发射电热产品,用于电热服装和室内采暖;在国防军工领域,将导电纤维与磁性纳米材料复合,可以制成电磁吸收性能可调节的电磁吸收材料,为电磁屏蔽和微波隐身提供基础材料。现有金属纤维纤维或碳纤维不同程度受耐形变折弯性能差的限制,柔软性和可纺性远低于有机纤维,远不能达到普通化学纤维的普遍应用。近年来许多人将碳基新材料与有机纤维复合,制成多种导电纤维,典型技术为将石墨烯或碳纳米管涂敷在单丝或束丝表面,形成连续导电层,由于导电相混入聚合物会降低导电性,单纯用增加碳纳米管层厚度达到高电导率,会引起导电层耐磨性降低,折弯稳定性下降,且纤维耐延伸应变能力弱,有人提出在有机纤维表面先涂敷粘合层,在涂敷导电层,形成连续导电纤维,或用碳纳米管与壳聚糖共混湿法纺丝得到导电芯材,再在其表面涂覆银纳米线,得到更高导电性,这些方法也难以同时达到高导电性、高延伸稳定性、高生产效率。
高性能导电纤维要求满足高导电性的同时,纤维具有良好综合性能,包括加工高效、导电性稳定、具有一定应变耐受度、成本较低、细度适当、导电层在单丝表面覆盖均匀,采用束丝浸渍方法难以达到导电层在单丝表面均匀包覆,采用简单的碳纳米管与粘结层涂敷,难以同时达到高导电性、高生产效率,为了增加导电性,碳纳米管厚度增加,耐折弯性下降,采用银纳米线作为导电相,纯银纳米线耐延伸性较低,与聚合物复合损失导电性,增加复合导电层厚度,增加银含量,不利于规模化使用。因此需要有一种综合解决生产效率、导电性、力学特性、质量稳定性的技术路线。
发明内容
本发明的目的在于提供一维纳米材料多层涂敷连续高导电有机纤维的制备方法,以解决上述背景技术中提出的问题。
为解决上述技术问题,本发明提供如下技术方案:
与现有技术相比,本发明的有益效果是:一维纳米材料多层涂敷连续高导电有机纤维的制备方法,包括如下步骤:
将经过预处理后的有机纤维芯材依次通过若干个胶池;胶池的出口液滴直径φ≤3D;D为有机纤维芯材的直径;
并且,有机纤维芯材在进入胶池前/后进行干燥工序;
至少包括两组胶池:一组胶池中盛装有导电粘结剂浆料,另一组胶池中盛装有一维导电纳米材料浆料。
此处的预处理为现有技术中的电晕处理。通过控制纤维穿过胶池出入口尖端液滴直径,使得液滴直径不大于3倍纤维直径条件下,可以使得在一定速度下(该速度在0.1~5米/秒之间),纤维表面的液层厚度低于Pleteau-Rayleigh失稳厚度,抑制由于液膜失稳产生的不连续液滴及干燥后导电层不均匀,达到在纤维表面均匀涂覆薄导电层,通过反复涂覆,调节层数,可以得到不同导电性的连续纤维。
基于上述本发明的整体构思,其包括对材料的选择,对高速涂敷时纤维表面液膜的控制,实现了高导电纤维连续的高效率地生产。具体而言,本发明解决了现有高导电纤维生产技术中生产效率和导电性不能同时满足的固有障碍。
优选的,导电粘结剂的成分为:水性聚氨酯与水性丙烯酸树脂中的一种或者两者的组合、纳米炭黑与机械剥离石墨烯中的一种或者两种的组合、消泡剂、润湿剂以及增稠剂;
其中,炭黑含量不高于15%,石墨烯含量不高于0.3%。
优选的,导电粘结剂的成分为:水性聚氨酯70-80份,纳米导电炭黑10-15份,机械剥离石墨烯0.1-0.3份,消泡剂1份,润湿剂1份,增稠剂1份。
关于“导电粘结剂”,具体为带有导电材料的粘结剂:对粘结剂种类以及导电材料并不做具体的限制,此处仅作为一种示例,采用水性聚氨酯与水性丙烯酸树脂;纳米炭黑与机械剥离石墨烯;本领域技术人员可在常规选择上进行配制而得。采用“导电粘结剂”的用意在于:赋予粘结剂以导电性。基于成型材料本身的结构,导电粘结剂形成的粘结层与一维导电纳米材料网络所形成的导电层之间类似于“并联”结构(即实现层间粘结的同时,实现垂直导电通路),提高了导电性。
优选的,一维导电纳米材料浆料的成分为单壁碳纳米管浆料或银纳米线浆料。
优选的,一维导电纳米材料浆料的成分还包括去离子水、乙醇、异丙醇。
优选的,一维导电纳米材料浆料的成分中包括离子型表面活性剂。具体的实施环节,结合以上方案的基础上,在一维导电纳米材料浆料中加入适量的离子型表面活性剂(本领域技术人员可自行选择,如烯基磺酸钠或十二烷基硫酸钠),其量保持在10%-20%之间为最佳;使得一维导电纳米材料浆料具有一定的浸润度,以提高一维导电纳米材料浆料与粘结剂的结合效率,实现在纤维快速牵引的状态下实现导电材料均匀涂敷(0.1-5秒/米),同时保持优良的导电性能以及其他物理性能。
优选的,还包括另外一组胶池,其内盛装有带红外发射纳米颗粒的粘结剂;
和/或;
带有磁性纳米颗粒的粘结剂。
优选的,红外发射纳米颗粒包括金属纳米颗粒、二氧化三铁纳米颗粒以及钨掺杂二氧化钒纳米颗粒中的一种或者几种的组合;
磁性纳米颗粒包括纳米四氧化三铁。
与粘结剂结合不同的功能性颗粒,用于涂覆之用,以赋予最终纤维产物具有不同的功能特性。
优选的,胶池的入口和/或出口处设置有同轴的椎管,椎管的输出端环设有柔性毛细纤毛;纤维在制备阶段从椎管中输入/输出,采用同轴设计,使其穿行通畅,不与锥管壁发生摩擦,避免了表面材料的摩擦损失;采用柔性毛细纤毛便于精准地控制该液滴,并且,采用此方式对纤维进行作业,材料渗透(粘接剂与一维导电材料层)均匀;也适配于纤维高速穿行作业的稳定性特点,提高生产效率。
优选的,椎管的倾角为10°,椎管的输出口直径为2毫米。
从内到外包括有机纤维芯材以及至少包括导电层的复合功能包层,内芯材的直径在30~70微米之间,复合功能包层的厚度在2~4微米之间。
优选的,导电层为多层状结构,单层的厚度不超过50纳米。
优选的,复合功能包层还包括红外发射特性层以及磁性层。
优选的,复合功能包层的总层数8-30层。
有机纤维芯材为PA6、PA66、PET、PE、PP中的任一种的连续长丝,直径在15D1F至60D1F之间。
导电纱,包括上述的一维纳米材料多层涂敷连续高导电有机纤维构成。
导电纤维结构体,包括上述的导电纱。
上述的这些特点和优点将会在下面的附图以及具体实施方式中,更为详细地描述。
附图说明
图1为本发明导电纤维制备步骤的示意图。
图2为本发明柔性毛细管结构示意图。
图3为纤维表面碳纳米管(左)、表面碳管局部放大(右上)、表面银纳米线局部放大(右下)扫描电镜照片;
图4为纤维单丝反复拉伸应力-应变曲线和电阻-应变曲线。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
将熔融纺丝法生产的20D1F锦纶长丝,经过电晕处理后,参照图1,纤维进行初次干燥(干燥温度为110℃)后进入胶池中;
本实施例的胶池共设有12个(按照纤维穿过的顺序分别命名为胶池1--胶池12),且按照其内物质(即涂覆物)的不同分为四组,第一组为胶池1、胶池5、胶池9—胶池12;其内的涂覆物为导电粘结剂,具体成分为:为水性聚氨酯70-80份,纳米导电炭黑10-15份,机械剥离石墨烯0.1-0.3份,消泡剂1份,润湿剂1份,增稠剂1份,机械混合;
第二组为胶池2-胶池4以及胶池6-胶池8,其内的涂覆物为,带有离子型表面活性剂的导电纳米材料浆料,具体成分为:单壁碳纳米管浆料,碳纳米管为中科院成都化学所生产的单壁碳纳米管水性浆料,含离子型表面活性剂,碳纳米管含量为0.2%,蒸发水相浓缩至0.8%。
继续参照图1,在胶池与胶池之间还安装有干燥管进行干燥。
参照图2,胶池入口、出口为柔性毛细锥管,椎管的倾角为10°,椎管的输出口直径为2毫米,椎管的输出端环设有柔性毛细纤毛;如图2所示,入口,出口距离不低于10毫米,入口与出口共轴,胶池中液体通过容积泵循环。
本实施例的采用单壁碳纳米管浆料,加入适量离子型表面活性剂,采用柔性毛细涂覆法,通过控制纤维穿过毛细刷涂尖端液滴直径,使得液滴直径不大于3倍纤维直径条件下,可以使得在一定速度下纤维表面的液层厚度低于Pleteau-Rayleigh失稳厚度,抑制由于液膜失稳产生的不连续液滴及干燥后导电层不均匀,达到在纤维表面均匀涂覆薄导电层,通过反复涂覆,调节层数,可以得到不同导电性的连续纤维。
胶池之间的加热管的干燥温度为110℃-130℃之间,纤维张力不大于0.01牛,速度不大于0.3米/秒;
纤维从最后一个胶池输出之后,通过油刷后上卷,再120℃烘干20分钟,测量纤维单丝导电性,比电阻不高于20千欧姆/厘米;
在其他优选的实施例中,当通过碳纳米管胶池数增加到10个时,比电阻不高于2千欧姆/厘米,总膜厚(即除去纤维芯材的部分)不大于3微米。
实施例2:本实施例中结构与实施例1一致,包括胶池的结构,胶池出入口结构以及干燥管结构以及干燥温度的设定。
不同之处在于对纤维的处理流程上。
具体的,将实施例1中穿过胶池9并干燥后得到的比电阻为20千欧的纤维收卷后,再经如下处理:
按照实施例图1的模式,设置10个胶池,分别是胶池I-胶池X,其中胶池I-胶池III以及胶池V-胶池VI内均盛装有银纳米线浆料;银纳米线为采用多元醇法制备的长纳米线,平均直径低于40纳米,平均长度大于10微米,分散在50%去离子水、20%乙醇、20%异丙醇溶液,溶液中含有10-20%离子型表面活性剂;
胶池IV以及胶池VII-胶池X为导电粘结剂,成分与实施例1中的一致。
纤维通过油刷后上卷,在120℃烘干20分钟,测量纤维单丝导电性,单位长度比电阻不高于100欧姆/厘米,
在本发明另一个优选实施例中,通过银纳米线胶池数增加到10个时,比电阻不高于30欧姆/厘米,总膜厚不大于4微米。
实施例3:
本实施例中结构与实施例1一致,包括胶池的结构,胶池出入口结构以及干燥管结构以及干燥温度的设定。
区别之处在于,对纤维的处理过程;
具体的,将熔融纺丝法生产的15D1F锦纶长丝,经过电晕处理后。依照图1的形式,依次通过加热管以及胶池。
胶池设置有14个,按照纤维穿过的顺序依次为,胶池a-胶池n;其中,胶池a、胶池e以及胶池i内均盛装有导电粘结剂,其成分为:水性丙烯酸树脂70-80份,纳米导电炭黑10-15份,机械剥离石墨烯0.1-0.3份,消泡剂1份,润湿剂1份,增稠剂1份,机械混合。
胶池b-胶池d以及胶池f-胶池h内盛装的均为与实施例1中相同的单壁碳纳米管浆料;
胶池j-胶池m内盛装与实施例2中相同的银纳米线浆料,胶池n中盛装有含有铜、锌纳米颗粒、或二氧化三铁纳米颗粒、或掺钨二氧化钒纳米颗粒的水性丙烯酸树脂粘结剂,该粘结剂成分为:水性丙烯酸树脂60-70份,纳米导电炭黑5-10份,机械剥离石墨烯0.1-0.3份,铜、锌纳米颗粒、或二氧化三铁纳米颗粒、或掺钨二氧化钒纳米颗粒一种或几种组合的总量15-20份,消泡剂1份,润湿剂1份,增稠剂1份,机械混合。
在本实施例中,添加了含有铜、锌纳米颗粒、或二氧化三铁纳米颗粒、或掺钨二氧化钒纳米颗粒的水性丙烯酸树脂粘结剂,其目的加入红外发射纳米颗粒时,纤维具有电流控制红外发射特性调节。
纤维通过所有的胶池后,通过油刷并上卷,在120℃烘干20分钟,测量纤维单丝导电性,比电阻不高于300欧姆/厘米,总膜厚不大于4微米。
实施例4
本实施例中结构与实施例1一致,包括胶池的结构,胶池出入口结构以及干燥管结构以及干燥温度的设定。
区别之处在于,对纤维的处理过程;
将熔融纺丝法生产的15D1F锦纶长丝,经过电晕处理后,依照图1的形式,依次通过加热管以及胶池;
本实施例中设置了14个胶池,本实施例与实施例3的不同之处,是将实施例3中胶池n中的含有铜、锌纳米颗粒、或二氧化三铁纳米颗粒、或掺钨二氧化钒纳米颗粒的水性丙烯酸树脂粘结剂,替换成含有四氧化三铁纳米颗粒的水性聚氨酯与水性丙烯酸树脂混合粘结剂,该粘结剂成分为:水性聚氨酯10-20份,水性丙烯酸树脂40-50份,纳米导电炭黑5-10份,机械剥离石墨烯0.1-0.3份,四氧化三铁纳米颗粒15-20份,消泡剂1份,润湿剂1份,增稠剂1份,机械混合。
本实施例的通过向纤维添加磁性纳米颗粒(即四氧化三铁纳米颗粒,尺寸小于10纳米),以实现纤维的可调磁性;其可调性可通过涂覆的层度来实现。
综上所有实施例,本发明区别于其他涂敷法制备碳纳米管、石墨烯导电纤维的关键是不在碳纳米管或银纳米线浆料中掺入聚合物用于提高导电层粘附性;
参照图3所示,提高导电层粘附性的核心是通过控制液滴厚度,使具有一定导电性和渗透性的粘结层浆料能渗入一维纳米材料网络间隙形成连续粘结层;调节粘结层厚度,使纤维导电性不因粘结层损失过多,整体导电层厚度低于4微米,纤维比电阻通过调节碳纳米管和银纳米线层数在几十欧姆到几千欧姆之间(100~104欧姆/厘米)可设计,降低电阻通过增加导电层厚度和银纳米线层数实现,解决涂敷导电层连续有机导电纤维普遍存在的高导电性、耐磨性、连续化难以同时具备缺点。
另外,为了得到性能可设计的功能化纤维,本发明在纤维表面层中可以加入不同纳米颗粒,加入红外发射纳米颗粒时,纤维具有电流控制红外发射特性调节,加入铁磁纳米颗粒时,纤维具有电流控制铁磁顺磁转变特性。
最终的成品纤维,在有机纤维芯材之外,包覆有导电层,层间组合导电粘结层(主要由导电粘结剂组成)以及表面功能层(如红外发射纳米层以及磁性层)。总层数在8-30层之间,有机纤维芯材是指PA6、PA66、PET、PE、PP中的任一种的连续长丝,直径在15D1F至60D1F之间,其他的皮层厚度在2-4微米之间。其中导电层的单层厚度不超过50纳米。
再参照图4所示,最终的成品纤维,具有耐腐蚀性,在30%盐水中浸泡1000小时,干燥后电阻变化低于5%;具有耐折弯性,折弯曲率1毫米,折弯105次,电阻增加低于10%;具有耐重复拉伸应变性,拉伸30%,100次,电阻增加低于10%。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (9)
1.一维纳米材料多层涂敷连续高导电有机纤维的制备方法,其特征在于:包括如下步骤:
将经过预处理后的有机纤维芯材依次通过若干个胶池,胶池的出口液滴直径φ≤3D,D为有机纤维芯材的直径,胶池供纤维穿行的出口处环设有柔性毛细纤毛,胶池的进口以及出口设置有同轴的椎管,柔性毛细纤毛设置在椎管上;
纤维的牵引速度在0.1米/秒-5米/秒之间;
并且,有机纤维芯材在进入胶池前/后进行干燥工序;
至少包括两组胶池:一组胶池中盛装有导电粘结剂浆料,另一组胶池中盛装有一维导电纳米材料浆料;
最终在有机纤维芯材外形成包括导电层的复合功能包层,复合功能包层的厚度在在2μm-4μm之间。
2.根据权利要求1所述的一维纳米材料多层涂敷连续高导电有机纤维的制备方法,其特征在于:导电粘结剂浆料的成分为:水性聚氨酯与水性丙烯酸树脂中的一种或者两者的组合、纳米炭黑与机械剥离石墨烯、消泡剂、润湿剂以及增稠剂。
3.根据权利要求1所述的一维纳米材料多层涂敷连续高导电有机纤维的制备方法,其特征在于:一维导电纳米材料浆料为单壁碳纳米管浆料或银纳米线水与异丙醇混合溶液。
4.根据权利要求1或3所述的一维纳米材料多层涂敷连续高导电有机纤维的制备方法,其特征在于:一维导电纳米材料浆料的成分中包括离子型表面活性剂。
5.根据权利要求1所述的一维纳米材料多层涂敷连续高导电有机纤维的制备方法,其特征在于:还包括另外一组胶池,其内盛装有带红外发射纳米颗粒的粘结剂;
和/或;
带有磁性纳米颗粒的粘结剂。
6.一维纳米材料多层涂敷连续高导电有机纤维,其特征在于:采用如权利要求1-5任一项所述的制备方法制备而得;
从内到外包括有机纤维芯材以及至少包括导电层的复合功能包层,内芯材的直径在30μm-70μm之间, 复合功能包层的厚度在2μm-4μm之间。
7.根据权利要求6所述的一维纳米材料多层涂敷连续高导电有机纤维,其特征在于:复合功能包层还包括红外发射特性层以及磁性层。
8.导电纱,其特征在于:包括权利要求6或7所述的一维纳米材料多层涂敷连续高导电有机纤维构成。
9.导电纤维结构体,其特征在于:包括权利要求8所述的导电纱。
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