CN111395002B - 纺织电极材料的制备方法及其纺织电极材料 - Google Patents
纺织电极材料的制备方法及其纺织电极材料 Download PDFInfo
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- CN111395002B CN111395002B CN202010189870.3A CN202010189870A CN111395002B CN 111395002 B CN111395002 B CN 111395002B CN 202010189870 A CN202010189870 A CN 202010189870A CN 111395002 B CN111395002 B CN 111395002B
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
本发明公开了一种纺织电极材料的制备方法及其纺织电极材料,所述制备方法包括:首先将预处理的织物浸泡在多巴胺盐酸盐溶液中,得聚多巴胺镀层织物;随后将聚多巴胺镀层织物浸泡在银氨溶液中,一定时间后加入葡萄糖溶液得镀银织物;再将镀银织物通过电化学方法在氯化钠溶液中进行氯化处理,形成银‑氯化银复合镀层织物;最后将银‑氯化银复合镀层织物通过电化学方法在导电聚合物单体溶液中进行修饰,得银‑氯化银‑导电聚合物复合镀层织物。所述的纺织电极材料表面比电阻为0.01‑5Ω,0.9%氯化钠溶液中的极化阻抗为10‑1000Ω,与皮肤界面阻抗为1KΩ‑100MΩ@1Hz,0.5‑50Hz频率范围内相位角变化量为0‑30°。
Description
技术领域
本发明涉及电极材料技术领域,具体涉及一种纺织电极材料的制备方法及其纺织电极材料。
背景技术
纺织电极用于人体心电监测近年受到世界各国研究者的广泛关注。心血管疾病是人类健康的头号杀手,这类疾病具有长期性、累积性、偶发性,常规的健康检查难以及时发现,给患者家庭和整个社会带来沉重的医疗负担,因此对心脏健康状况进行长期监测、早诊断和早治疗显得尤为重要。传统一次性心电测量电极通常为金属-水凝胶电极,但在使用过程中水凝胶会逐渐干涸,影响电极性能;同时水凝胶的导电电解质会对皮肤产生刺激,造成过敏,严重的会导致皮肤发炎或溃烂。纺织电极因其柔软舒适、透气透湿、耐久性、易集成性等优点,非常适合作为穿戴式心电监测传感器。
电极作为传感器是沟通人体内的离子导电和信号采集设备中电子导电的桥梁,电极材料的选择和制备成为纺织电极的关键技术,并且对电极性能有着重要的影响。心电信号属于微弱低频电压信号,人体皮肤表面心电信号强度范围在1-5mV,频率范围在0.01-250Hz,其中能量谱密度主要集中在0.5-40Hz之间,要通过置于皮肤表面的电极进行获得精准的心电信号,电极的基本要求是对信号的强度具有最低的抑制和对波形具有最小的畸变,前者要求心电电极具有较低的界面阻抗,而后者要求电极在心电信号频域范围具有较稳定的相位角。因此,优选材料及对电极界面性能调控显得极为关键。
目前纺织电极材料采用各种导电材料及其复合材料,如:黄金、银、镍和不锈钢等金属,或导电高分子材料,或无机导电材料,在纤维或者织物表面进行这些材料的镀层,亦或普通纤维与导电(镀层)纤维进行混纺或交织。意大利Pisa大学Paradiso R.等人采用不锈钢导电纤维制成的针织物测量静态下的人体心电信号(Paradiso R.et al,A wearablehealth care system based on knitted integrated sensors,IEEE Transactions onInformation Technology in Biomedicine,2005,9(3),pp337-344.);德国亚琛工业大学Becnmann L.等人采用镀银、镀铜纤维制作针织物和机织物的纺织电极(Beckmann L.etal.,Characterization of textile electrodes and conductors using standardizedmeasurementsetups,Physiological Measurement,2010,31(2)pp233-243.);比利时Gent大学Westbroek P.等人使用不锈钢纤维制作的机织物、针织物和非织造布作为纺织电极(Westbroek P.et al.,Quality control of textile electrodes by electrochemicalimpedance spectroscopy,Textile Research Journal,2006,76(2),pp152-159.);瑞典大学等人采用不锈钢纤维、不锈钢纤维/涤纶混纺纱线以及镀银纱线制作机织和针织结构的纺织电极(L.et al.,Electrical characteristics ofconductive yarns and textile electrodes for medical applications,Medical&Biological Engineering&Computing,2007,45(12),pp1251-1257.);美国北卡罗来纳州大学Kang T.等人将导电银漆印刷在非织造布上制作纺织心电电极(Kang T.et al.,Nonwoven fabric active electrodes for bio-potential measurement during normaldaily activity,IEEE Transactions on Biomedical Engineering,2008 55(1),pp188-195.)。以上纺织电极均采用较为传统的导电材料,而且使用的材料较单一,未实现电极材料的可控制备及电极界面性能的调控。申请号201310461096.7公开一种测量心电信号的纺织电极的制备方法,采用两步法制备聚吡咯(PPY)镀层导电织物,先是水浴法制备聚吡咯(PPY)镀层,然后再将其放入吡咯溶液中进行电化学聚合得到聚吡咯(PPY)镀层导电织物的纺织电极;该专利方法的制备的纺织电极阻抗较大,而且导电聚合物耐久性较差,镀层水洗容易脱落。东华大学许鹏俊的博士论文《用于体表心电监测的纺织结构电极与皮肤之间机械作用分析及动态噪音研究》将银镀层纱线改性得到银-氯化银镀层织物作为纺织电极;该方法得到的银-氯化银镀层较脆弱,氯化银颗粒裸露纤维表面,在使用中容易脱落进而影响电极性能。申请号201811357957.6公开一种石墨烯心电电极及其制备方法,将石墨烯、羧甲基纤维素和水混合得石墨烯导电油墨,再将石墨烯导电油墨印刷在织物上,得到柔性织物心电电极;该方法制得的电极阻抗较大,且耐久性差,难以长时间使用。以上方法均未有效的对纺织电极的界面性能的调控,所制得的电极耐久性较差,所测量的心电信号准确性和一致性差,不适合作为心电监测电极长时间使用。
发明内容
本发明旨在提供一种纺织电极材料的制备方法及其纺织电极材料,特别是提供一种银-氯化银-导电聚合物复合镀层织物的纺织电极材料及其制备方法。
本发明的一种纺织电极材料的制备方法,包括如下步骤:
(1)将预处理的织物浸泡在多巴胺盐酸盐溶液中,得聚多巴胺镀层织物;
(2)将聚多巴胺镀层织物浸泡在银氨溶液中,然后加入葡萄糖溶液,反应后得镀银织物;
(3)将镀银织物通过电化学方法在氯化钠溶液中进行表面氯化处理,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;
(4)将银-氯化银复合镀层织物通过电化学方法在导电聚合物单体的水溶液进行修饰,得银-氯化银-导电聚合物复合镀层织物。
进一步地,所述织物的纤维材料类型为天然纤维和/或化学纤维的短纤和/或长丝;所述织物的纤维材料平均直径为1nm-2000um,其中短纤的长径比为10-10000。
进一步地,步骤(1)中,所述的预处理为水洗和/或干洗和/或皂洗和/或煮练和/或漂白和/或碱减量和/或有机溶剂洗涤和/或等离子体处理。
进一步地,步骤(1)中,所述的多巴胺盐酸盐溶液浓度为0.1-100g/L;和/或,
步骤(1)中,所述的多巴胺盐酸盐溶液的pH值为6.8-10;和/或,
步骤(1)中,所述的浸泡,浴比为1:(10-50),时间为1-48h;和/或,
步骤(1)中,所述的浸泡过程中加入多巴胺盐酸盐溶液,时间间隔为0.1-4h,加入量为固液总体积的1-20%;和/或,
步骤(1)中,所述的浸泡过程中进行震荡,震荡频率10-80次/min。
进一步地,步骤(2)中,所述的所述银氨溶液的制备方法为:配置1-50g/L的硝酸银溶液,并逐滴滴加2%的稀氨水),直到溶液产生沉淀并至澄清;和/或,
步骤(2)中,所述的葡萄糖溶液浓度为2-100g/L;和/或,
步骤(2)中,所述的浸泡,时间为15-60min;和/或,
步骤(2)中,所述的反应,时间为30-180min;和/或,
步骤(2)中,所述的溶液进行震荡,震荡频率10-80次/min。
进一步地,步骤(3)中,所述的电化学方法为恒电流和/或恒电位和/或线性扫描伏安法和/或循环伏安法和/或方波伏安法和/或计时库伦法和/或计时安培法和/或阶跃电势法;和/或,
步骤(3)中,所述的氯化钠溶液,浓度为5-40g/L;和/或,
步骤(3)中,所述的氯化钠溶液,浴比为1:(10-50);和/或,
步骤(3)中,所述的氯化钠溶液中加入了十六烷基三甲基溴化铵,用量为10-20g/L;和/或,
步骤(3)中,所述的电化学方法,处理电压为0V-5V和/或电流密度为0.05-5A/dm2,处理时间为15-120sec。
进一步地,步骤(4)中,所述的电化学方法为恒电流和/或恒电位和/或线性扫描伏安法和/或循环伏安法和/或方波伏安法和/或计时库伦法和/或计时安培法和/或阶跃电势法;和/或,
步骤(4)中,所述的导电聚合物单体为3,4-乙烯二氧噻吩(EDOT)和/或吡咯(PY)和/或苯胺;和/或,
步骤(4)中,所述的导电聚合物溶液浓度为0.1-3g/L(3,4-乙烯二氧噻吩)和/或0.1-65g/L(吡咯)和/或0.1-4g/L(苯胺);和/或,
步骤(4)中,所述的导电聚合物单体的水溶液中加入十二烷基苯磺酸,用量为10-20g/L;和/或,
步骤(4)中,所述的导电聚合物单体的水溶液,浴比为1:(10-50);和/或,
步骤(4)中,所述的电化学方法,处理电压为0V-5V和/或电流密度为0.05-5A/dm2,处理时间为15-120sec。
相应地,本发明还提供了由上述纺织电极材料的制备方法所得的纺织电极材料,所述的纺织电极材料的纤维具有“皮芯”结构,银-氯化银-导电聚合物复合镀层均匀地包覆在外层,纤维表面由内而外依次为银层和/或导电聚合物层,氯化银根植于银层、贯穿导电聚合物层并镶嵌于其中形成“枣糕”状微观形态。
进一步地,所述的纺织电极材料的表面颗粒尺度为10nm-3um,银-氯化银-导电聚合物复合镀层织物的接触角为0-90°。
进一步地,所述的纺织电极材料的表面比电阻为0.01-5Ω,在浓度为0.9%氯化钠溶液中极化阻抗为10-1000Ω,与人体皮肤接触的界面阻抗为1KΩ-100MΩ@1Hz,0.5-500Hz频率范围内相位角变化量为0-30°。
与现有技术相比较,本发明具有以下有益效果:
1.本发明采用聚多巴胺对织物进行镀银,多巴胺的氧化自聚合反应在纤维表面生成粘附性极强的聚多巴胺薄膜,再在银氨溶液中利用聚多巴胺薄膜的强粘附性以及葡萄糖的强还原性将银离子还原成银单质而沉积在织物的表面,所制得的镀银层连续、致密、均匀且导电性优良。该法简化了传统化学镀银中的粗化、敏化、活化工艺,避免了传统化学镀银工艺复杂、银与基底结合力差、环境污染等问题。
2.本发明制备的银-氯化银-导电聚合物镀层的纺织电极材料既具有优良的界面性能又有极高的耐腐蚀性。银-氯化银材料体系具有较低的极化阻抗、较低的平衡电势、较高的导电率、较好的生理兼容性;导电聚合物具有离子导电和电子导电的双重特性,作为生物电信号传感器能更有效沟通人体内离子导电和电子设备中的电子导电。本发明的制备方法将两者融合在一起,制得的电极材料具有二者的优点;导电聚合物镀层填充了银-氯化银层的孔隙,既有效地提高了镀银层的耐腐蚀性,又解决了氯化银颗粒易脱落的问题。
3.本发明制备的银-氯化银-导电聚合物复合镀层的纺织电极材料,银-氯化银-导电聚合物复合镀层均匀地包覆在外层,纤维表面由内而外依次为银层和/或导电聚合物层,氯化银根植于银层、贯穿导电聚合物层并镶嵌于其中形成“枣糕”状微观形态,表面颗粒尺度为10nm-3um。这种材料体系本身具有良好的亲水性,表面的微纳结构则更进一步增强表面亲水性。
4.本发明制备的银-氯化银-导电聚合物复合镀层的纺织电极材料时,精确调控银-氯化银-导电聚合物镀层织物的纺织电极的界面性能,既降低电极的界面阻抗,又减小特定频率范围内相位角变化对信号精度的影响。人体的心电频率是在0.01-250Hz之间,而主要能量密度谱集中在0.5-40Hz范围内,在这一区间内电极的阻抗越低、相位角变化越小,就越有利于获取高精度人体心电信号。因此,本发明所制备的纺织电极不仅具有优良且持久的性能,又具有透气透湿、柔软、舒适的优点,在纺织服装、电子信息、医疗健康以及人工智能等领域具有广泛的应用前景。
附图说明
图1显示为实施例6不同摩擦次数处理的镀银织物的电阻;
图2显示为实施例6制备的银(Ag)、银-氯化银(Ag-AgCl)和银-氯化银-聚噻吩(Ag-AgCl-PEDOT)镀层织物电极的电化学阻抗:(a)阻抗随频率变化,(b)相位角随频率变化;
图3显示为不同镀层的扫描电镜图;
图4显示为不同镀层的EDS元素分析图;
图5显示为不同电极测试的心电图;
图6显示为对照例不同镀层的扫描电镜图。
具体实施方式
为详细说明技术方案的技术内容、构造特征、所实现目的及效果,以下结合具体实施例并配合附图详予说明。
实施例1
一种纺织电极材料的制备方法,具体步骤如下:
(1)将棉纤维织物(纤维平均直径为12um,平均长度为32mm,组织结构为平纹机织物,单位面积重量为120g/m2)进行皂洗处理后,在室温下浸泡在浓度为50g/L、pH值为8.6的多巴胺盐酸盐溶液中,浴比为1:40,在浸泡过程中进行震荡,震荡频率45次/min,浸泡时间为24h;且在浸泡过程中每隔2h加入固液总体积的10%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置25g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中40min,在浸泡过程中进行震荡,震荡频率45次/min,然后加入浓度为51g/L葡萄糖溶液,保持震荡反应105min后得镀银织物;
(3)先向浓度为22g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为15g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中进行表面氯化处理,浴比为1:40,处理的电压为2.5V,时间为65sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;其中,所述的电化学方法为恒电压法;
(4)先向浓度为2g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为15g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在导电聚合物单体的水溶液进行修饰,浴比为1:40,处理电压为2.5V,时间为65s,得银-氯化银-导电聚合物复合镀层织物,其中,所述的电化学方法为恒电压法。
上述方法制得的电极材料的表面颗粒尺度为300nm±100nm,接触角为30°±10°,表面比电阻为1.5Ω±0.8Ω,在浓度为0.9%氯化钠溶液中极化阻抗为80Ω±20Ω,与人体皮肤接触的界面阻抗为1.2MΩ±0.2MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为25°。(注:±前为平均数,±后为偏差值)
实施例2
一种纺织电极材料的制备方法,具体步骤如下:
(1)将亚麻纤维织物(纤维平均直径为14um,平均长度为22mm,组织结构为平纹机织物,单位面积重量为160g/m2)进行皂洗处理后,在室温下浸泡在浓度为60g/L、pH值为8.5的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率40次/min,浴比为1:35,浸泡时间为18h;且在浸泡过程中每隔1.5h加入固液总体积的8%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置20g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中45min,在浸泡过程中进行震荡,震荡频率40次/min,然后加入浓度为43g/L葡萄糖溶液,保持震荡反应115min后得镀银织物;
(3)先向浓度为25g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为12g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中采用循环伏安法进行表面氯化处理,浴比为1:35,扫描电压范围为0-2.0V,扫描速率为0.1V/sec,扫描循环数为2,即:处理时间为80sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;
(4)先向浓度为20g/L的吡咯(PY)的水溶液中加入的十二烷基苯磺酸(加入量为16g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在导电聚合物单体的水溶液采用循环伏安法进行修饰,浴比为1:35,扫描电压范围为0-2.0V,扫描速率为0.1V/sec,扫描循环数为2,即:处理时间为80sec,得银-氯化银-导电聚合物复合镀层织物。
上述方法制得的电极材料的表面颗粒尺度为350nm±90nm,接触角为34°±11°,表面比电阻为2Ω±1Ω,在浓度为0.9%氯化钠溶液中极化阻抗为100Ω±25Ω,与人体皮肤接触的界面阻抗为1.4MΩ±0.3MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为22°。
实施例3
一种纺织电极材料的制备方法,具体步骤如下:
(1)将羊毛纤维织物(纤维平均直径为20um,平均长度为55mm,组织结构为平纹机织物,单位面积重量为180g/m2)进行水洗后,在室温下浸泡在浓度为70g/L、pH值为8.0的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率25次/min,浴比为1:45,浸泡时间为15h;且在浸泡过程中每隔1h加入固液总体积的6%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置24g/L的硝酸银溶液,并逐滴滴加2.5%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中35min,在浸泡过程中进行震荡,震荡频率35次/min,然后加入浓度为49g/L葡萄糖溶液,保持震荡反应95min后得镀银织物;
(3)先向浓度为18g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为16g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中采用计时安培法进行表面氯化处理,浴比为1:45,初始电压为0V,最高电压为3.0V,最低电压为0V,脉冲数为25个,每个脉冲电压持续时间为2sec,即:处理时间为50sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;
(4)先向浓度为3g/L的苯胺的水溶液中加入的十二烷基苯磺酸(加入量为18g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在导电聚合物单体的水溶液中采用计时安培法进行表面氯化处理,浴比为1:45,初始电压为0V,最高电压为3.0V,最低电压为0V,脉冲数为25个,每个脉冲电压持续时间为2sec,即:处理时间为50sec,得银-氯化银-导电聚合物复合镀层织物。
上述方法制得的电极材料的表面颗粒尺度为400nm±120nm,接触角为38°±12°,表面比电阻为1Ω±0.5Ω,在浓度为0.9%氯化钠溶液中极化阻抗为90Ω±20Ω,与人体皮肤接触的界面阻抗为1.3MΩ±0.3MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为21°。
实施例4
一种纺织电极材料的制备方法,具体步骤如下:
(1)将桑蚕丝纤维织物(纤维平均直径为10um,组织结构为平纹机织物,单位面积重量为120g/m2)进行皂洗处理后,在室温下浸泡在浓度为75g/L、pH值为7.9的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率28次/min,浴比为1:50,浸泡时间为12h;且在浸泡过程中每隔0.5h加入固液总体积的5%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置26g/L的硝酸银溶液,并逐滴滴加2.5%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中28min,在浸泡过程中进行震荡,震荡频率30次/min,然后加入浓度为55g/L葡萄糖溶液,保持震荡反应90min后得镀银织物;
(3)先向浓度为15g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为10g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中采用线性扫描法进行表面氯化处理,浴比为1:50,初始电压为0V,最终电压为3.0V,扫描速率为0.2V/sec,即:处理时间为15sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;
(4)先向浓度为1g/L3,4-乙烯二氧噻吩(EDOT)溶液中加入的十二烷基苯磺酸(加入量为12/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在导电聚合物单体的水溶液中采用线性扫描法进行表面氯化处理,浴比为1:50,初始电压为0V,最终电压为3.0V,扫描速率为0.2V/sec,即:处理时间为15sec,得银-氯化银-导电聚合物复合镀层织物。
上述方法制得的电极材料的表面颗粒尺度为200nm±50nm,接触角为25°±5°,表面比电阻为0.5Ω±0.3Ω,在浓度为0.9%氯化钠溶液中极化阻抗为75Ω±10Ω,与人体皮肤接触的界面阻抗为1.0MΩ±0.1MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为20°。
实施例5
一种纺织电极材料的制备方法,具体步骤如下:
(1)将涤纶短纤维织物(纤维平均直径为18um,平均长度为44mm,组织结构为平纹机织物,单位面积重量为150g/m2)进行减减量处理后,在室温下浸泡在浓度为35g/L、pH值为8.5的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率56次/min,浴比为1:25,浸泡时间为21h;且在浸泡过程中每隔1.5h加入固液总体积的5%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置21g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中42min,在浸泡过程中进行震荡,震荡频率56次/min,然后加入浓度为43g/L葡萄糖溶液,保持震荡反应135min后得镀银织物;
(3)先向浓度为12g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为10g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中采用恒电流法进行表面氯化处理,浴比为1:25,电流密度为0.3A/dm2,处理时间为30sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;
(4)先向浓度为2g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为15g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在3,4-乙烯二氧噻吩(EDOT)的水溶液采用恒电流法进行修饰,浴比为1:25,电流密度为0.3A/dm2,处理时间为30sec,得银-氯化银-导电聚合物复合镀层织物。
上述方法制得的电极材料的表面颗粒尺度为400nm±130nm,接触角为45°±10°,表面比电阻为1.2Ω±0.4Ω,在浓度为0.9%氯化钠溶液中极化阻抗为65Ω±10Ω,与人体皮肤接触的界面阻抗为1.25MΩ±0.15MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为18°。
实施例6
一种纺织电极材料的制备方法,具体步骤如下:
(1)将涤纶长丝纤维织物(纤维平均直径为15um,组织结构为平纹机织物,单位面积重量为125g/m2)进行丙酮清洗处理后,在室温下浸泡在浓度为50g/L、pH值为8.4的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率45次/min,浴比为1:30,浸泡时间为24h;且在浸泡过程中每隔2h加入固液总体积的10%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置24g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中40min,在浸泡过程中进行震荡,震荡频率50次/min,然后加入浓度为52g/L葡萄糖溶液,保持震荡反应120min后得镀银织物;
(3)先向浓度为19g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为14g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中进行表面氯化处理,浴比为1:30,处理的电压为1.5V,时间为45sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;其中,所述的电化学方法为恒电压法;
(4)先向浓度为2.2g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为15g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在3,4-乙烯二氧噻吩(EDOT)的水溶液进行修饰,浴比为1:30,处理电压为4.0V,时间为45sec,得银-氯化银-导电聚合物复合镀层织物,其中,所述的电化学方法为恒电压法。
上述方法制得的电极材料的表面颗粒尺度为375nm±150nm,接触角为38°±9°,表面比电阻为0.4Ω±0.2Ω,在浓度为0.9%氯化钠溶液中极化阻抗为75Ω±10Ω,与人体皮肤接触的界面阻抗为1.15MΩ±0.1MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为16°。
对本实施例制备方法过程中制备的镀银织物进行耐磨测试,测试结果如图1所示。
实施例7
一种纺织电极材料的制备方法,具体步骤如下:
(1)将锦纶长丝纤维织物(纤维平均直径为14um,组织结构为平纹机织物,单位面积重量为115g/m2)进行超声水洗后,在室温下浸泡在浓度为60g/L、pH值为8.1的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率30次/min,浴比为1:20,浸泡时间为12h;且在浸泡过程中每隔1h加入固液总体积的10%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置30g/L的硝酸银溶液,并逐滴滴加3%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中25min,在浸泡过程中进行震荡,震荡频率30次/min,然后加入浓度为63g/L葡萄糖溶液,保持震荡反应100min后得镀银织物;
(3)先向浓度为30g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为20g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中进行表面氯化处理,浴比为1:20,处理的电压为2.0V,时间为35sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;其中,所述的电化学方法为恒电压法;
(4)先向浓度为1.6g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为12g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在3,4-乙烯二氧噻吩(EDOT)的水溶液进行修饰,浴比为1:20,处理电压为2.0V,时间为35s,得银-氯化银-导电聚合物复合镀层织物,其中,所述的电化学方法为循环伏安法。
上述方法制得的电极材料的表面颗粒尺度为365nm±155nm,接触角为34°±9°,表面比电阻为0.8Ω±0.2Ω,在浓度为0.9%氯化钠溶液中极化阻抗为72Ω±10Ω,与人体皮肤接触的界面阻抗为1.0MΩ±0.3MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为23°。
实施例8
一种纺织电极材料的制备方法,具体步骤如下:
(1)将芳纶长丝纤维织物(纤维平均直径为21um,组织结构为平纹机织物,单位面积重量为115g/m2)进行等离子处理后,在室温下浸泡在浓度为80g/L、pH值为8.3的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率20次/min,浴比为1:15,浸泡时间为9h;且在浸泡过程中每隔0.5h加入固液总体积的10%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置18g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中45min,在浸泡过程中进行震荡,震荡频率20次/min,然后加入浓度为38g/L葡萄糖溶液,保持震荡反应150min后得镀银织物;
(3)先向浓度为35g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为25g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中进行表面氯化处理,浴比为1:15,处理的电压为1.8V,时间为60sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;其中,所述的电化学方法为恒电压法;
(4)先向浓度为2.1g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为15g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在3,4-乙烯二氧噻吩(EDOT)的水溶液进行修饰,浴比为1:15,处理的电压为1.8V,时间为60sec,得银-氯化银-导电聚合物复合镀层织物,其中,所述的电化学方法为循环伏安法。
上述方法制得的电极材料的表面颗粒尺度为455nm±165nm,接触角为42°±10°,表面比电阻为0.7Ω±0.2Ω,在浓度为0.9%氯化钠溶液中极化阻抗为68Ω±9Ω,与人体皮肤接触的界面阻抗为1.4MΩ±0.4MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为25°。
实施例9
一种纺织电极材料的制备方法,具体步骤如下:
(1)将聚丙烯腈(PAN)纳米纤维膜(纤维平均直径为380nm,薄膜厚度为0.1mm,薄膜微观结构呈非织造布形态,单位面积重量为15g/m2)固定在塑料网孔支架上,在室温下整体浸泡在浓度为55g/L、pH值为7.4的多巴胺盐酸盐溶液中,在浸泡过程中进行震荡,震荡频率35次/min,浴比为1:15,浸泡时间为18h;且在浸泡过程中每隔2h加入固液总体积的10%的多巴胺盐酸盐溶液,得聚多巴胺镀层织物;
(2)配置19g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清,将聚多巴胺镀层织物室温下浸泡在银氨溶液中32min,在浸泡过程中进行震荡,震荡频率15次/min,然后加入浓度为40g/L葡萄糖溶液,保持震荡反应75min后得镀银织物;
(3)先向浓度为19g/L氯化钠溶液中加入了十六烷基三甲基溴化铵(加入量为15g/L),然后将镀银织物通过电化学方法室温下在氯化钠溶液中进行表面氯化处理,浴比为1:15,处理的电压为2.0V,时间为25sec,形成氯化银包覆银(即:银-氯化银)的复合镀层织物;其中,所述的电化学方法为循环伏安法;
(4)先向浓度为2.3g/L的3,4-乙烯二氧噻吩(EDOT)的水溶液中加入的十二烷基苯磺酸(加入量为20g/L),然后将银-氯化银复合镀层织物通过电化学方法室温下在3,4-乙烯二氧噻吩(EDOT)的水溶液进行修饰,浴比为1:15,处理电压为2.0V,时间为25sec,得银-氯化银-导电聚合物复合镀层织物,其中,所述的电化学方法为循环伏安法。
上述方法制得的电极材料的表面颗粒尺度为225nm±105nm,接触角为22°±10°,表面比电阻为0.9Ω±0.2Ω,在浓度为0.9%氯化钠溶液中极化阻抗为72Ω±6Ω,与人体皮肤接触的界面阻抗为1.1MΩ±0.4MΩ@1Hz,0.5-50Hz频率范围内相位角变化量的绝对值为18°。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者终端设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者终端设备所固有的要素。在没有更多限制的情况下,由语句“包括……”或“包含……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者终端设备中还存在另外的要素。此外,在本文中,“大于”、“小于”、“超过”等理解为不包括本数;“以上”、“以下”、“以内”等理解为包括本数。
尽管已经对上述各实施例进行了描述,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例做出另外的变更和修改,所以以上所述仅为本发明的实施例,并非因此限制本发明的专利保护范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围之内。
Claims (10)
1.一种纺织电极材料的制备方法,其特征在于,包括如下步骤:
(1)将预处理的织物浸泡在多巴胺盐酸盐溶液中,得聚多巴胺镀层织物;
(2)将聚多巴胺镀层织物浸泡在银氨溶液中,一定时间后加入葡萄糖溶液,反应后得镀银织物;
(3)将镀银织物通过电化学方法在氯化钠溶液中进行表面氯化处理,形成氯化银包覆银复合镀层织物;所述的氯化钠溶液中加入了十六烷基三甲基溴化铵,用量为10-20g/L;
(4)将银-氯化银复合镀层织物通过电化学方法在导电聚合物单体的水溶液进行修饰,所述的导电聚合物单体为3,4-乙烯二氧噻吩和/或吡咯和/或苯胺;所述的导电聚合物单体的水溶液中加入十二烷基苯磺酸,用量为10-20g/L;得银-氯化银-导电聚合物复合镀层织物。
2.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于,所述织物的纤维材料类型为天然纤维和/或化学纤维的短纤和/或长丝;所述织物的纤维材料平均直径为1nm-2000um,其中短纤的长径比为10-100000。
3.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于:步骤(1)中,所述的预处理为水洗和/或皂洗和/或煮练和/或漂白和/或碱减量和/或有机溶剂洗涤和/或等离子体处理。
4.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于:步骤(1)中,所述的多巴胺盐酸盐溶液浓度为0.1-100 g/L;和/或,
步骤(1)中,所述的多巴胺盐酸盐溶液的pH值为6.8-10;和/或,
步骤(1)中,所述的浸泡,浴比为1:(10-50),时间为1-48h;和/或,
步骤(1)中,所述的浸泡过程中加入多巴胺盐酸盐溶液,时间间隔为0.1-4h,加入量为固液总体积的1-20%;和/或,
步骤(1)中,所述的浸泡过程中进行震荡,震荡频率10-80次/min。
5.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于:步骤(2)中,所述银氨溶液的制备方法为:配置1-50g/L的硝酸银溶液,并逐滴滴加2%的稀氨水,直到溶液产生沉淀并至澄清;和/或,
步骤(2)中,所述的葡萄糖溶液浓度为2-100g/L;和/或,
步骤(2)中,所述的浸泡,时间为15-60min;和/或,
步骤(2)中,所述的反应,时间为30-180min;和/或,
步骤(2)中,所述的溶液进行震荡,震荡频率10-80次/min。
6.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于:步骤(3)中,所述的电化学方法为恒电流和/或恒电位和/或线性扫描伏安法和/或循环伏安法和/或计时库伦法和/或计时安培法;和/或,
步骤(3)中,所述的氯化钠溶液,浓度为5-40g/L;和/或,
步骤(3)中,所述的氯化钠溶液,浴比为1:(10-50);和/或,
步骤(3)中,所述的电化学方法,处理电压为0V-5V和/或电流密度为0.05-5A/dm2,处理时间为15-120sec。
7.根据权利要求1所述的一种纺织电极材料的制备方法,其特征在于:步骤(4)中,所述的电化学方法为线性扫描伏安法和/或循环伏安法和/或恒电压和/或方波伏安法和/或计时库伦法和/或计时安培法;和/或,
步骤(4)中,所述的导电聚合物溶液浓度为0.1-3g/L和/或0.1-65g/L吡咯和/或0.1-4g/L苯胺;和/或,
步骤(4)中,所述的导电聚合物单体的水溶液,浴比为1:(10-50);和/或,
步骤(4)中,所述的电化学方法,处理电压为0-5V和/或电流密度为0.05-5A/dm2,处理时间为15-120sec。
8.根据权利要求1所述的一种纺织电极材料的制备方法所得的纺织电极材料,其特征是:所述的纺织电极材料的纤维具有“皮芯”结构,银-氯化银-导电聚合物复合镀层均匀地包覆在外层,纤维表面由内而外依次为银层、氯化银、导电聚合物层,并且氯化银根植于银层、贯穿导电聚合物层并镶嵌于其中形成“枣糕”状微观形态。
9.根据权利要求8中所述的纺织电极材料,其特征在于,所述的纺织电极材料的表面颗粒尺度为10nm-3um,银-氯化银-导电聚合物复合镀层织物的接触角为0-90°。
10.根据权利要求8中所述的纺织电极材料,其特征在于,所述的纺织电极材料的表面比电阻为0.01-5Ω,在浓度为0.9%氯化钠溶液中极化阻抗为10-1000Ω,与人体皮肤接触的界面阻抗为1KΩ-100MΩ@1Hz,0.5-50Hz频率范围内相位角变化量为0-30°。
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