CN106087400A - 铥锰镍合金/维纶电子导线的制备方法 - Google Patents

铥锰镍合金/维纶电子导线的制备方法 Download PDF

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CN106087400A
CN106087400A CN201610475040.0A CN201610475040A CN106087400A CN 106087400 A CN106087400 A CN 106087400A CN 201610475040 A CN201610475040 A CN 201610475040A CN 106087400 A CN106087400 A CN 106087400A
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蓝碧健
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Taicang Biqi New Material Research Development Co Ltd
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Abstract

本发明属于可穿戴电子技术领域，涉及一种铥锰镍合金/维纶电子导线的制备方法。该电子导线的制备方法的包括维纶纤维清洗、表面改性，催化活化及化学镀铥锰镍合金。本发明制备方法的优点是：经180天模拟人体体液腐蚀测试，金属离子溢出率小于1ppm，即该材料具有极高的生物环境可靠性；电子导线的电导率高于铜，达到8×107 S/m以上。铥锰镍合金/维纶电子导线可用于智能服装，应用前景明朗，市场潜力巨大。

Description

铥锰镍合金/维纶电子导线的制备方法
技术领域
本发明属于可穿戴电子技术领域，涉及一种铥锰镍合金/维纶电子导线的制备方法。
背景技术
电子织物(e-textile)是当前可穿戴计算领域的主要研究方向之一，基于织物可穿戴传感和电子技术追求光电性能(精度、EMC、稳定性)与机械性能(柔性、伸展性、强度)俱佳的织物化传感、电路和驱动单元(或装置)，它们可以任意弯曲和扭褶，可通过特殊连接技术“编织”成具有普通衣物形态和舒适度的智能衣物，其上分布式地融入了光、电、声学性能并同时具备柔韧性。然而，就目前的技术水平而言，如光电性能好，则做到柔性化和弹性化就相对困难，也更缺乏可洗性能，反之亦然。当前主要有三种典型的可穿戴电子织物设计与制作方法，第一种是柔性丝网印刷法，将导电和传感材料直接印刷在织物基底上。第二种是编织、针织或刺绣，即将导电、传感和绝缘纤维或丝线通过编织等方法直接制成传感器。第三种是缝制，利用导电纱线等将现成的电路板或传感器缝合在衣物上。
维纶是聚乙烯醇缩醛纤维的商品名称，也叫维尼纶。其性能接近棉花，有“合成棉花”之称，是现有合成纤维中吸湿性最大的品种。维纶的柔软及保暖性好，它的相对密度比棉花要小，因此与棉花相同重量的维纶能织出更多的衣料。它的热传导率低，因而保暖性好。维纶的耐磨性和强度也比棉花要好，因此维纶在很多方面可以与棉混纺以节省棉花。维纶主要用于制作外衣、棉毛衫裤、运动衫等针织物，还可用于帆布、渔网、外科手术缝线、自行车轮胎帘子线、过滤材料等。
用于可穿戴服装的电子导线，由于与身体长时间接触，安全问题一直存在风险，特别是含金属电子导电的应用，在人体汗液环境中，电子导线金属离子的溢出，对人体不利。本发明是在维纶表面被覆一层铥锰镍合金层，核心工艺是在铜锌复合催化活化下，在化学镀溶液中，稀土元素铥进入锰镍合金的晶格中，形成更加致密稳定的合金层，经180天模拟人体体液腐蚀测试，铥锰镍合金/维纶电子导线的金属离子溢出率小于百万分之一(1ppm)，说明该材料具有极高的生物环境可靠性；铥锰镍合金/维纶电子导线的电导率高于铜，达到8×107S/m以上，是目前所有导电维纶复合材料中最好的。综上所述，本发明提出的铥锰镍合金/维纶电子导线的制备方法具有突出的实质性特点和显著的进步，即具备创造性。
发明内容
本发明属于可穿戴电子领域，涉及一种铥锰镍合金/维纶电子导线的制备方法。该制备方法的步骤如下：
1)将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干；
2)将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维；其中改性剂溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：3-巯基丙基三乙氧基硅烷浓度3～6g/L，甲基丙烯酸甲酯浓度9～12g/L，过氧化叔丁醇浓度1～3g/L，丙酮浓度100～200g/L。
3)将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维；其中活化剂溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：硫酸锌浓度20～30g/L，硫酸铜浓度20～30g/L，十二烷基硫酸钠浓度20～30g/L。
4)将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。其中铥锰镍化学镀溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：硝酸铥浓度20～30g/L；硫酸镍浓度20～30g/L；硝酸锰浓度40～60g/L；碳酸氢钠浓度30～60g/L；十二烷基硫酸钠浓度60～90g/L；二甲氨基硼烷浓度3～6g/L；丁二酸浓度6～9g/L。
5)铥锰镍合金/维纶电子导线测试表征。将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率；以四探针测试仪测试电子导线的电导率。其中模拟人体体液各成分含量：NaCl 8g/L，KCl 0.4g/L，NaHCO3 0.35g/L，CaCl2 0.14g/L，Na2HPO4 0.06g/L，KH2PO4 0.06g/L，MgSO4.7H2O 0.2g/L,葡萄糖1g/L。
铥锰镍合金/维纶电子导线可用于可穿戴服装，应用前景明朗，市场潜力巨大。
具体实施方式
下面通过实施例进一步描述本发明
实施例1
将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将3.5g 3-巯基丙基三乙氧基硅烷，9.5g甲基丙烯酸甲酯，2.5g过氧化叔丁醇溶于165g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维。
将29.5g硫酸锌，21.5g硫酸铜，25.5g十二烷基硫酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维。
将24.5g硝酸铥，25.5g硫酸镍，46.5g硝酸锰，57.5g碳酸氢钠，78.5g十二烷基硫酸钠，4.5g二甲氨基硼烷，8.5g丁二酸溶于500mL去离子水中，再稀释成体积为1L的铥锰镍化学镀溶液。
将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
将8g NaCl，0.4g KCl，0.35g NaHCO3，0.14g CaCl2，0.06g Na2HPO4，0.06g KH2PO4，0.2g MgSO4.7H2O，1g葡萄糖溶于500mL去离子水中，再稀释成体积为1L的模拟人体体液。
将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率分别为0.35ppm、0.25ppm、0.15ppm；以四探针测试仪测试电子导线的电导率为8.5×107S/m。
实施例2
将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将4.4g 3-巯基丙基三乙氧基硅烷，10.3g甲基丙烯酸甲酯，2.2g过氧化叔丁醇溶于151g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维。
将21.5g硫酸锌，22.7g硫酸铜，22.9g十二烷基硫酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维。
将23.8g硝酸铥，24.9g硫酸镍，56.4g硝酸锰，58.2g碳酸氢钠，81.6g十二烷基硫酸钠，4.1g二甲氨基硼烷，6.9g丁二酸溶于500mL去离子水中，再稀释成体积为1L的铥锰镍化学镀溶液。
将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
将8g NaCl，0.4g KCl，0.35g NaHCO3，0.14g CaCl2，0.06g Na2HPO4，0.06g KH2PO4，0.2g MgSO4.7H2O，1g葡萄糖溶于500mL去离子水中，再稀释成体积为1L的模拟人体体液。
将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率分别为0.13ppm、0.11ppm、0.31ppm；以四探针测试仪测试电子导线的电导率为8.3×107S/m。
实施例3
将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将6g 3-巯基丙基三乙氧基硅烷，12g甲基丙烯酸甲酯，3g过氧化叔丁醇溶于200g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维。
将30g硫酸锌，30g硫酸铜，30g十二烷基硫酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维。
将30g硝酸铥，30g硫酸镍，60g硝酸锰，60g碳酸氢钠，90g十二烷基硫酸钠，6g二甲氨基硼烷，9g丁二酸溶于500mL去离子水中，再稀释成体积为1L的铥锰镍化学镀溶液。
将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
将8g NaCl，0.4g KCl，0.35g NaHCO3，0.14g CaCl2，0.06g Na2HPO4，0.06g KH2PO4，0.2g MgSO4.7H2O，1g葡萄糖溶于500mL去离子水中，再稀释成体积为1L的模拟人体体液。
将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率分别为0.22ppm、0.31ppm、0.21ppm；以四探针测试仪测试电子导线的电导率为8.5×107S/m。
实施例4
将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将3.4g 3-巯基丙基三乙氧基硅烷，10.5g甲基丙烯酸甲酯，2.6g过氧化叔丁醇溶于172g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维。
将25.2g硫酸锌，23.8g硫酸铜，22.2g十二烷基硫酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维。
将21.1g硝酸铥，23.3g硫酸镍，45.5g硝酸锰，56.7g碳酸氢钠，71.9g十二烷基硫酸钠，5.1g二甲氨基硼烷，7.3g丁二酸溶于500mL去离子水中，再稀释成体积为1L的铥锰镍化学镀溶液。
将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
将8g NaCl，0.4g KCl，0.35g NaHCO3，0.14g CaCl2，0.06g Na2HPO4，0.06g KH2PO4，0.2g MgSO4.7H2O，1g葡萄糖溶于500mL去离子水中，再稀释成体积为1L的模拟人体体液。
将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率分别为0.32ppm、0.11ppm、0.21ppm；以四探针测试仪测试电子导线的电导率为8.1×107S/m。。
实施例5
将维纶纤维依次用重量百分比浓度为10％的碳酸钾水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将3g 3-巯基丙基三乙氧基硅烷，9g甲基丙烯酸甲酯，1g过氧化叔丁醇溶于100g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维。
将20g硫酸锌，20g硫酸铜，20g十二烷基硫酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5％的硼氢化钾水溶液中10分钟，取出，洗净，得活化维纶纤维。
将20g硝酸铥，20g硫酸镍，40g硝酸锰，30g碳酸氢钠，60g十二烷基硫酸钠，3g二甲氨基硼烷，6g丁二酸溶于500mL去离子水中，再稀释成体积为1L的铥锰镍化学镀溶液。
将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
将8g NaCl，0.4g KCl，0.35g NaHCO3，0.14g CaCl2，0.06g Na2HPO4，0.06g KH2PO4，0.2g MgSO4.7H2O，1g葡萄糖溶于500mL去离子水中，再稀释成体积为1L的模拟人体体液。
将铥锰镍合金/维纶电子导线置于模拟人体体液中，于37℃放置180天，取出，以能量弥散X射线探测器(EDX)测试电子导线的元素含量，计算铥、锰、镍离子的溢出率分别为0.42ppm、0.11ppm、0.16ppm；以四探针测试仪测试电子导线的电导率为8.2×107S/m。

Claims (4)

1.一种铥锰镍合金/维纶电子导线的制备方法，其特征在于：
1）将维纶纤维依次用重量百分比浓度为10%的碳酸钾水溶液、5% 的双氧水溶液、去离子水洗净、烘干；
2）将洗净的维纶纤维置于改性剂溶液中30分钟，取出，置于烘箱中于60℃干燥3小时，冷却至室温，得改性维纶纤维；
3）将改性维纶纤维置于活化剂溶液中30分钟，取出，用去离子水洗净，烘干，再置于重量百分比浓度为5%的硼氢化钾水溶液中10分钟，取出，用去离子水洗净，得活化维纶纤维；
4）将活化维纶纤维置于铥锰镍化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得铥锰镍合金/维纶电子导线。
2.如权利要求1所述的铥锰镍合金/维纶电子导线的制备方法，其特征在于所述的改性剂溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：
3-巯基丙基三乙氧基硅烷浓度 3~6 g/L；
甲基丙烯酸甲酯浓度9~12 g/L；
过氧化叔丁醇浓度1~3 g/L；
丙酮浓度100~200 g/L。
3.如权利要求1所述的铥锰镍合金/维纶电子导线的制备方法，其特征在于所述的活化剂溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：
硫酸锌浓度 20~30g/L；
硫酸铜浓度 20~30g/L；
十二烷基硫酸钠浓度20~30g/L。
4.如权利要求1所述的铥锰镍合金/维纶电子导线的制备方法，其特征在于所述的铥锰镍化学镀溶液的配方是溶剂为去离子水，溶液中各种溶质浓度分别为：
硝酸铥浓度 20~30g/L；
硫酸镍浓度 20~30g/L；
硝酸锰浓度 40~60g/L；
碳酸氢钠浓度 30~60g/L；
十二烷基硫酸钠浓度60~90g/L；
二甲氨基硼烷浓度 3~6g/L；
丁二酸浓度6~9g/L。
CN201610475040.0A 2016-06-27 2016-06-27 铥锰镍合金/维纶电子导线的制备方法 Pending CN106087400A (zh)

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