CN105484015A - 一种层状复合屏蔽织物的制备方法 - Google Patents
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Abstract
本发明属于电子材料领域,涉及一种层状复合屏蔽织物的制备方法。本发明提出的制备方法是以亚麻为基体,在其表面依次沉积聚吡咯层和金属镍层,具体工艺包括亚麻碱减量处理、聚吡咯原位化学聚合、硅烷偶联剂自组装改性、钯纳米溶胶活化以及化学镀镍等。本发明制备的层状复合屏蔽织物,将反射形式与吸收形式结合,拓宽了屏蔽材料可应用的电磁波频率范围,提升了其电磁屏蔽效应。本发明制备的层状复合屏蔽织物可用于医疗保健、电磁屏蔽工作服、智能纺织品等高新技术产品,市场前景广阔。
Description
技术领域
本发明属于电子材料技术领域,具体涉及一种层状复合屏蔽织物的制备方法。
背景技术
如今越来越多的电子产品及电器进入人类的生活中,如移动电话、计算机、电热毯、微波炉等。在正常的情况下,人体的器官和组织都存在着稳定有序的微弱电磁场,而这些电子电器产品在工作时会产生各种不同波长和频率的电磁波。在这些外界电磁场的干扰下,人体内处于平衡状态的微弱电磁场将遭到破坏,从而改变人体中的血液、淋巴液和细胞原生质,不但影响人体的神经系统、循环、免疫、生殖和代谢功能,严重的时候甚至可导致胎儿畸形或孕妇自然流产,给人体带来严重危害。因此,随着人们对健康越来越重视以及对生活质量的要求越来越高,研究和开发各种具有防电磁辐射面料已成为新型纺织品研究和发展的热点领域之一。电磁波传播至屏蔽材料表面时,有三种不同的衰减机理,一是在入射表面的反射衰减,是由空气与屏蔽材料之间的错配阻抗引起,为富含电子或空穴的屏蔽材料的主要衰减形式。二是未被反射而进入屏蔽体的电磁波被吸收衰减,是一种能量耗散,这是本征导电高分子(聚吡咯、聚苯胺、聚乙炔、聚聚塞吩)的主要衰减形式。三是屏蔽体内部多重反射衰减,占衰减总量的很小比例,只在屏蔽效应小于15dB时才有考虑意义。目前大部分防电磁辐射面料都只是以单种衰减形式(反射或吸收)为主导,如导电高分子复合织物、金属化织物、碳基复合织物等,而将两种衰减机理结合起来用作电磁屏蔽的产品在市面上还很少见。理论上,在织物表面构建金属/导电高分子复合层,得到的防电磁辐射面料可以实现反射与吸收两种衰减机理的强势结合,从而达到相互增强的效果,解决屏蔽效应低、屏蔽性能不稳定等难题。
发明内容
本发明的目的在于提供一种层状复合屏蔽织物的制备方法。
本发明提出的层状复合屏蔽织物的制备方法,以亚麻为基体,在其表面依次沉积聚吡咯层和金属镍层,具体工艺包括亚麻碱减量处理、聚吡咯原位化学聚合、硅烷偶联剂自组装改性、钯纳米溶胶活化以及化学镀镍等,具体步骤如下:
(1)亚麻碱减量处理:将亚麻布置于60~80℃碱溶液中,碱减量处理10~30分钟,取出、烘干;
(2)聚吡咯原位化学聚合:将碱减量处理后的亚麻布置于吡咯—乙醇溶液中5~20分钟,取出再立即放入氧化剂溶液中5~20分钟,取出、洗净,上述过程循环3~5次,烘干;
(3)硅烷偶联剂自组装改性:将步聚(2)处理过的亚麻布浸入硅烷偶联剂溶液中5~10分钟,取出,于100~120
℃烘干,浸泡与烘干循环3~5次;
(4)钯纳米溶胶活化:将步聚(3)处理过的亚麻布置于钯纳米溶胶溶液中3~5小时,取出、洗净;
(5)化学镀镍:将步聚(4)处理过的亚麻布浸泡在镍化学镀液中,于30~60 ℃化学镀0.5~2小时,取出洗净,烘干,制得层状复合屏蔽织物。
本发明中,碱溶液的配方是溶剂为去离子水,溶液中各种溶质为:氢氧化钠的浓度为 2~4 g/L,磷酸钠的浓度为4~8 g/L,碳酸钠的浓度为2~4 g/L。
本发明中,吡咯—乙醇溶液的溶质为吡咯单体,溶剂为无水乙醇,吡咯溶液的摩尔浓度为0.5~1.0 mol/L。
本发明中,氧化剂溶液的溶剂为去离子水,溶液中各种溶质为氯化铁的浓度为 5~20 g/L,对甲苯磺酸钠的浓度为 2~5 g/L。.
本发明中,硅烷偶联剂溶液的溶质为3-氨基丙基三甲氧基硅烷,溶剂为丙酮,改性溶液的质量浓度为0.1%~1%。
本发明中,钯纳米溶胶溶液的配方溶剂为去离子水,溶液中各种溶质为氯化钯的浓度为 3~5 g/L,酒石酸钾钠的浓度为 10~15 g/L,盐酸的浓度为3~5
g/L,硼氢化钠的浓度为3~5 g/L。
本发明中,镍化学镀液的配方是溶剂为去离子水,溶液中各种溶质为硫酸镍的浓度为15~25 g/L,焦磷酸钠的浓度15~25 g/L,氨水的浓度为5~15 g/L,多聚磷酸的浓度为3~5 g/L,二甲氨基硼烷的浓度为3~5 g/L。
本发明制备的层状复合屏蔽织物具有以下优点:(1)亚麻是天然纤维,属可再生资源,绿色环保。(2)经碱减量处理后的亚麻布为多孔清洁基体,吡咯单体可渗入孔内并在孔内聚合,得到的聚吡咯层与亚麻基体相互铆合,结合力增强。(3)亚麻布主要成份为纤维素,表面具有较多羟基(>C-OH),可以与聚吡咯中的(-N-H)形成氢键,结合力增强。(4)硅烷偶联剂可以充当桥梁,联接内层聚吡咯层与外层金属镍,使彼此结合力增强,提升材料可靠性。(5)外层的金属镍以反射电磁波形式为主,内层聚吡咯导电高分子以吸收电磁波形式为主,本发明制备的层状复合屏蔽织物,将反射形式与吸收形式结合,拓宽了屏蔽材料可应用的电磁波频率范围,提升了其电磁屏蔽效应。本发明制备的层状复合屏蔽织物可用于医疗保健、电磁屏蔽工作服、智能纺织品等高新技术产品,市场前景广阔。
本发明的有益效果在于:(1)以亚麻作为屏蔽材料的基材,原料来源丰富,降低工艺成本。(2)亚麻布进行碱减量处理,不仅可以去除亚麻布上原有的杂质以及化学残留,还可以提升得到的聚吡咯层与亚麻基体之间的结合力,提高产品的质量。(3)硅烷偶联剂可充当聚吡咯层与金属层的分子桥梁,提高产品的可靠性。(4)本发明采用导电高分子化学聚合和化学镀相结合,克服了单独高分子聚合或化学镀所制备的屏蔽材料低电磁屏蔽问题。(5)工艺过程维护简便,对仪器设备的依赖度低可进行连续化生产,适合大规模生产,能满足市场需求。
附图说明
图1为层状复合屏蔽织物的制备流程示意图;
图2为层状复合屏蔽织物的扫描电镜照片。
具体实施方式
下面通过实例进一步描述本发明。
实施例
1
将2g氢氧化钠,4g磷酸钠,2g碳酸钠溶于500mL去离子水中,溶解完毕,得碱溶液。
将亚麻布置于含有500 mL上述碱溶液的烧杯中,60 ℃水浴加热处理10分钟,取出淋洗直至洗出液呈中性,烘干。
将1g氯化铁,0.4g对甲苯磺酸钠溶于200mL去离子水中,溶解完毕,得到氧化剂溶液。
将碱处理后的亚麻布置于浓度为0.5mol/L的200mL吡咯—乙醇溶液10分钟。取出再立即放入上述氧化剂溶液中10分钟,取出、洗净,上述过程循环3次,烘干,得到表面沉积有聚吡咯的亚麻布。
将聚吡咯/亚麻布置于浓度为0.1%的3-氨基丙基三甲氧基硅烷丙酮溶液,浸泡5分钟,取出,然后在100 ℃烘干,浸泡与烘干循环3次。
将3g氯化钯,15g酒石酸钾钠,3g盐酸,3g硼氢化钠溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得钯纳米溶胶溶液。
将改性后的聚吡咯/亚麻布置于上述溶液中,放置3小时,取出,洗净,得表面活化的聚吡咯/亚麻布。
将15g硫酸镍,15g焦磷酸钠,5g氨水,3g多聚磷酸,3g二甲氨基硼烷溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得化学镀镍溶液。
将表面活化的聚吡咯/亚麻布置于上述镀镍液中,于40℃化学镀1小时,取出,用水洗净,烘干,得层状复合屏蔽织物,聚吡咯含量为24.52%,磁性镍含量为5.16%,表面方阻为0.97Ω/□,饱和磁化强度为7.56 emu/g,屏蔽效能为43.52 dB,剥离强度能通过3M公司思高®胶带的测试。
实施例
2
将3g氢氧化钠,5g磷酸钠,2.5g碳酸钠溶于500mL去离子水中,溶解完毕,得碱溶液。
将亚麻布置于含有500 mL上述碱溶液的烧杯中,70 ℃水浴加热处理12分钟,取出淋洗直至洗出液呈中性,烘干。
将1.5g氯化铁,0.5g对甲苯磺酸钠溶于200mL去离子水中,溶解完毕,得到氧化剂溶液。
将碱处理后的亚麻布置于浓度为0.6mol/L的200mL吡咯—乙醇溶液12分钟。取出再立即放入上述氧化剂溶液中12分钟,取出、洗净,上述过程循环4次,烘干,得到表面沉积有聚吡咯的亚麻布。
将聚吡咯/亚麻布置于浓度为0.5%的3-氨基丙基三甲氧基硅烷丙酮溶液,浸泡8分钟,取出,然后在120 ℃烘干,浸泡与烘干循环3次。
将5g氯化钯,25g酒石酸钾钠,4g盐酸,4g硼氢化钠溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得钯纳米溶胶溶液。
将改性后的聚吡咯/亚麻布置于上述溶液中,放置5小时,取出,洗净,得表面活化的聚吡咯/亚麻布。
将25g硫酸镍,25g焦磷酸钠,14g氨水,5g多聚磷酸,4g二甲氨基硼烷溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得化学镀镍溶液。
将表面活化的聚吡咯/亚麻布置于上述镀镍液中,于45℃化学镀1.5小时,取出,用水洗净,烘干,得层状复合屏蔽织物,聚吡咯含量为25.61%,磁性镍含量为6.16%,表面方阻为0.82Ω/□,饱和磁化强度为8.56 emu/g,屏蔽效能为46.32 dB,剥离强度能通过3M公司思高®胶带的测试。
实施例
3
将4g氢氧化钠,7.5g磷酸钠,4g碳酸钠溶于500mL去离子水中,溶解完毕,得碱溶液。
将亚麻布置于含有500 mL上述碱溶液的烧杯中,65 ℃水浴加热处理15分钟,取出淋洗直至洗出液呈中性,烘干。
将2.5g氯化铁,0.8g对甲苯磺酸钠溶于200mL去离子水中,溶解完毕,得到氧化剂溶液。
将碱处理后的亚麻布置于浓度为0.6mol/L的200mL吡咯—乙醇溶液20分钟。取出再立即放入上述氧化剂溶液中15分钟,取出、洗净,上述过程循环3次,烘干,得到表面沉积有聚吡咯的亚麻布。
将聚吡咯/亚麻布置于浓度为0.7%的3-氨基丙基三甲氧基硅烷丙酮溶液,浸泡5分钟,取出,然后在120 ℃烘干,浸泡与烘干循环3次。
将4g氯化钯,20g酒石酸钾钠,4g盐酸,4g硼氢化钠溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得钯纳米溶胶溶液。
将改性后的聚吡咯/亚麻布置于上述溶液中,放置4小时,取出,洗净,得表面活化的聚吡咯/亚麻布。
将20g硫酸镍,20g焦磷酸钠,10g氨水,4g多聚磷酸,4g二甲氨基硼烷溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得化学镀镍溶液。
将表面活化的聚吡咯/亚麻布置于上述镀镍液中,于50℃化学镀1.5小时,取出,用水洗净,烘干,得层状复合屏蔽织物,聚吡咯含量为25.24%,磁性镍含量为6.76%,表面方阻为0.85Ω/□,饱和磁化强度为8.14 emu/g,屏蔽效能为44.38 dB,剥离强度能通过3M公司思高®胶带的测试。
实施例
4
将2g氢氧化钠,4g磷酸钠,2g碳酸钠溶于500mL去离子水中,溶解完毕,得碱溶液。
将亚麻布置于含有500 mL上述碱溶液的烧杯中,60 ℃水浴加热处理10分钟,取出淋洗直至洗出液呈中性,烘干。
将1g氯化铁,0.4g对甲苯磺酸钠溶于200mL去离子水中,溶解完毕,得到氧化剂溶液。
将碱处理后的亚麻布置于浓度为0.5mol/L的200mL吡咯—乙醇溶液10分钟。取出再立即放入上述氧化剂溶液中10分钟,取出、洗净,上述过程循环3次,烘干,得到表面沉积有聚吡咯的亚麻布。
将聚吡咯/亚麻布置于浓度为0.3%的3-氨基丙基三甲氧基硅烷丙酮溶液,浸泡5分钟,取出,然后在115 ℃烘干,浸泡与烘干循环3次。
将3.5g氯化钯,22g酒石酸钾钠,4g盐酸,3g硼氢化钠溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得钯纳米溶胶溶液。
将改性后的聚吡咯/亚麻布置于上述溶液中,放置3.5小时,取出,洗净,得表面活化的聚吡咯/亚麻布。
将20g硫酸镍,15g焦磷酸钠,8g氨水,4g多聚磷酸,3g二甲氨基硼烷溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得化学镀镍溶液。
将表面活化的聚吡咯/亚麻布置于上述镀镍液中,于55℃化学镀1.5小时,取出,用水洗净,烘干,得层状复合屏蔽织物,聚吡咯含量为26.53%,磁性镍含量为6.88%,表面方阻为0.92Ω/□,饱和磁化强度为8.53 emu/g,屏蔽效能为44.31 dB,剥离强度能通过3M公司思高®胶带的测试。
实施例
5
将4g氢氧化钠,8g磷酸钠,3g碳酸钠溶于500mL去离子水中,溶解完毕,得碱溶液。
将亚麻布置于含有500 mL上述碱溶液的烧杯中,80 ℃水浴加热处理15分钟,取出淋洗直至洗出液呈中性,烘干。
将3.5g氯化铁,1g对甲苯磺酸钠溶于200mL去离子水中,溶解完毕,得到氧化剂溶液。
将碱处理后的亚麻布置于浓度为0.5mol/L的200mL吡咯—乙醇溶液15分钟。取出再立即放入上述氧化剂溶液中8分钟,取出、洗净,上述过程循环4次,烘干,得到表面沉积有聚吡咯的亚麻布。
将聚吡咯/亚麻布置于浓度为0.8%的3-氨基丙基三甲氧基硅烷丙酮溶液,浸泡5分钟,取出,然后在110 ℃烘干,浸泡与烘干循环3次。
将4.5g氯化钯,20.5g酒石酸钾钠,3.5g盐酸,4.5g硼氢化钠溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得钯纳米溶胶溶液。
将改性后的聚吡咯/亚麻布置于上述溶液中,放置4.5小时,取出,洗净,得表面活化的聚吡咯/亚麻布。
将21g硫酸镍,23g焦磷酸钠,12g氨水,3.5g多聚磷酸,4g二甲氨基硼烷溶于500mL去离子水中,溶解完毕,添加去离子水,至溶液体积为1L,得化学镀镍溶液。
将表面活化的聚吡咯/亚麻布置于上述镀镍液中,于60℃化学镀2小时,取出,用水洗净,烘干,得层状复合屏蔽织物,聚吡咯含量为27.52%,磁性镍含量为9.21%,表面方阻为0.66Ω/□,饱和磁化强度为9.03 emu/g,屏蔽效能为50.05 dB,剥离强度能通过3M公司思高®胶带的测试。
Claims (7)
1.一种层状复合屏蔽织物的制备方法,其特征在于具体步骤如下:
(1)亚麻碱减量处理:将亚麻布放入碱溶液中碱减量处理、烘干;
(2)聚吡咯原位化学聚合:将碱减量处理后的亚麻布置于吡咯—乙醇溶液中5~20分钟,取出再立即放入氧化剂溶液中5~20分钟,循环处理3~5次,取出、洗净、烘干;
(3)硅烷偶联剂自组装改性:将聚吡咯原位化学聚合处理过的亚麻布浸入硅烷偶联剂溶液中5~10分钟,取出于100~120℃烘干,浸泡与烘干循环3~5次;
(4)钯纳米溶胶活化:将硅烷偶联剂自组装改性处理过的亚麻布置于钯纳米溶胶溶液中3~5小时,取出、洗净;
(5)化学镀镍:将钯纳米溶胶活化处理过的亚麻布浸泡在镍化学镀液中,于30~60 ℃化学镀1~2小时,取出洗净,烘干,制得磁性亚麻基层状复合屏蔽材料。
2.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(1)中所述碱溶液的配方是溶剂为去离子水,溶液中各种溶质为:氢氧化钠的浓度为 2~4 g/L,磷酸钠的浓度为4~8 g/L,碳酸钠的浓度为2~4 g/L。
3.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(2)中所述的吡咯—乙醇溶液的溶质为吡咯单体,溶剂为无水乙醇,吡咯溶液的摩尔浓度为0.5~1.0 mol/L。
4.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(2)中所述的氧化剂溶液的溶剂为去离子水,溶液中各种溶质为氯化铁的浓度为 5~20 g/L,对甲苯磺酸钠的浓度为 2~5 g/L。
5.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(3)中所述的硅烷偶联剂溶液的溶质为3-氨基丙基三甲氧基硅烷,溶剂为丙酮,改性溶液的质量浓度为0.1%~1%。
6.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(4)中所述的钯纳米溶胶溶液的配方溶剂为去离子水,溶液中各种溶质为氯化钯的浓度为 3~5 g/L,酒石酸钾钠的浓度为 10~15 g/L,盐酸的浓度为3~5 g/L,硼氢化钠的浓度为3~5 g/L。
7.根据权利要求1所述的层状复合屏蔽织物的制备方法,其特征在于步骤(5)中所述的镍化学镀液的配方是溶剂为去离子水,溶液中各种溶质分别为:硫酸镍的浓度为15~25 g/L;焦磷酸钠的浓度15~25 g/L;氨水的浓度为5~15 g/L;多聚磷酸的浓度为3~5 g/L;二甲氨基硼烷的浓度为3~5 g/L。
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