CN106120311A - 镱锰铜合金/腈纶电子导线的制备方法 - Google Patents

镱锰铜合金/腈纶电子导线的制备方法 Download PDF

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CN106120311A
CN106120311A CN201610474574.1A CN201610474574A CN106120311A CN 106120311 A CN106120311 A CN 106120311A CN 201610474574 A CN201610474574 A CN 201610474574A CN 106120311 A CN106120311 A CN 106120311A
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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，涉及一种镱锰铜合金/腈纶电子导线的制备方法。该电子导线的制备方法的包括腈纶纤维清洗、表面改性，催化活化及化学镀镱锰铜合金。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。镱锰铜合金/腈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

镱锰铜合金/腈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，涉及一种镱锰铜合金/腈纶电子导线的制备方法。
背景技术
近年来，随着科学技术的发展，特别是航空、航天技术的飞速发展，对材料的要求越来越来高，传统材料一旦制成成品，就不可能在使用过程中对其性能实施动态监控，并且材料只能被动地受环境的影响，不能针对环境的变化做出适当的反应。对于这些不足。在上世纪70年代末80年代初，受自然界生物具备的某些能力的启发，美国军方为提高行器的性能，首先提出了“可穿戴材料”的概念。分为三类：①.消极可穿戴材料，仅具有对外界环境和刺激感知的能力；②.积极可穿戴材料，具有对外界环境和刺激感知且反应的能力；③.高级可穿戴材料，不仅具有对外界环境和刺激感知和反应的能力，还表现出动态的自适应性。
腈纶是聚丙烯腈或丙烯腈含量大于85％(质量百分比)的丙烯腈共聚物制成的合成纤维。常用的第二单体为非离子型单体，如丙烯酸甲酯、甲基丙烯酸甲酯等，第三单体为离子型单体如丙烯磺酸钠和2-亚甲基-1，4-丁二酸等。聚丙烯腈纤维的性能极似羊毛，弹性较好，伸长20％时回弹率仍可保持65％，蓬松卷曲而柔软，保暖性比羊毛高15％，有合成羊毛之称。强度22.1～48.5cN/dtex，比羊毛高1～2.5倍。耐晒性能优良，露天曝晒一年，强度仅下降20％，可做成窗帘、幕布、篷布、炮衣等。腈纶在内部大分结构上很独特，呈不规则的螺旋形构象，且没有严格的结晶区，但有高序排列与低序排列之分。
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。本发明是在腈纶表面被覆一层镱锰铜合金层，核心工艺是在镍铝复合催化活化下，在化学镀溶液中，稀土元素镱进入锰铜合金的晶格中，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，镱锰铜合金/腈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；镱锰铜合金/腈纶电子导线的电导率高于铜，达到8×107S/m以上，是目前所有导电腈纶复合材料中最好的。综上所述，本发明提出的镱锰铜合金/腈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，涉及一种镱锰铜合金/腈纶电子导线的制备方法。该制备方法的步骤如下：
1)将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、5％的双氧水溶液、去离子水洗净、烘干；
2)将洗净的腈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，得改性腈纶纤维；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，氰基丙烯酸乙酯浓度9～12g/L，过氧化苯甲酰浓度1～3g/L，丙酮浓度100～200g/L。
3)将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维；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：硫酸铝浓度20～30g/L，硫酸镍浓度20～30g/L，酒石酸钠浓度20～30g/L。
4)将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。其中镱锰铜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：硝酸镱浓度20～30g/L；硫酸铜浓度20～30g/L；硝酸锰浓度40～60g/L；碳酸氢钠浓度30～60g/L；酒石酸钠浓度60～90g/L；二甲氨基硼烷浓度3～6g/L；草酸铵浓度6～9g/L。
5)镱锰铜合金/腈纶电子导线测试表征。将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率；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。
镱锰铜合金/腈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
将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将3.3g 3-巯基丙基三乙氧基硅烷，9.4g氰基丙烯酸乙酯，2.5g过氧化苯甲酰溶于166g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的腈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，得改性腈纶纤维。
将29.1g硫酸铝，21.2g硫酸镍，25.3g酒石酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维。
将24.8g硝酸镱，25.8g硫酸铜，46.8g硝酸锰，57.8g碳酸氢钠，78.1g酒石酸钠，4.9g二甲氨基硼烷，8.1g草酸铵溶于500mL去离子水中，再稀释成体积为1L的镱锰铜化学镀溶液。
将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
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。
将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率分别为0.21ppm、0.21ppm、0.23ppm；以四探针测试仪测试电子导线的电导率为8.4×107S/m。
实施例2
将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将4.1g 3-巯基丙基三乙氧基硅烷，10.3g氰基丙烯酸乙酯，2.5g过氧化苯甲酰溶于152g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的腈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，得改性腈纶纤维。
将27.5g硫酸铝，29.7g硫酸镍，23.9g酒石酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维。
将21.8g硝酸镱，23.9g硫酸铜，55.4g硝酸锰，57.2g碳酸氢钠，89.6g酒石酸钠，4.2g二甲氨基硼烷，6.4g草酸铵溶于500mL去离子水中，再稀释成体积为1L的镱锰铜化学镀溶液。
将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
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。
将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率分别为0.23ppm、0.41ppm、0.11ppm；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3
将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、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氰基丙烯酸乙酯，3g过氧化苯甲酰溶于200g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的腈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，得改性腈纶纤维。
将30g硫酸铝，30g硫酸镍，30g酒石酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维。
将30g硝酸镱，30g硫酸铜，60g硝酸锰，60g碳酸氢钠，90g酒石酸钠，6g二甲氨基硼烷，9g草酸铵溶于500mL去离子水中，再稀释成体积为1L的镱锰铜化学镀溶液。
将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
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。
将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率分别为0.32ppm、0.21ppm、0.11ppm；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4
将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、5％的双氧水溶液、去离子水洗净、烘干。
将3.1g 3-巯基丙基三乙氧基硅烷，10.4g氰基丙烯酸乙酯，2.7g过氧化苯甲酰溶于162g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的腈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，得改性腈纶纤维。
将22.2g硫酸铝，24.8g硫酸镍，26.2g酒石酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维。
将26.1g硝酸镱，28.3g硫酸铜，42.5g硝酸锰，54.7g碳酸氢钠，73.9g酒石酸钠，5.6g二甲氨基硼烷，7.1g草酸铵溶于500mL去离子水中，再稀释成体积为1L的镱锰铜化学镀溶液。
将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
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。
将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率分别为0.12ppm、0.18ppm、0.28ppm；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5
将腈纶纤维依次用重量百分比浓度为10％的草酸水溶液、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氰基丙烯酸乙酯，1g过氧化苯甲酰溶于100g丙酮中，添加去离子水，配成体积为1L的改性剂溶液。
将洗净的腈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，得改性腈纶纤维。
将20g硫酸铝，20g硫酸镍，20g酒石酸钠溶于500mL去离子水中，再稀释成体积为1L的活化剂溶液。
将改性腈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3％的硼氢化钠水溶液中10分钟，取出，洗净，得活化腈纶纤维。
将20g硝酸镱，20g硫酸铜，40g硝酸锰，30g碳酸氢钠，60g酒石酸钠，3g二甲氨基硼烷，6g草酸铵溶于500mL去离子水中，再稀释成体积为1L的镱锰铜化学镀溶液。
将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
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。
将镱锰铜合金/腈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，计算镱、锰、铜离子的溢出率分别为0.12ppm、0.21ppm、0.36ppm；以四探针测试仪测试电子导线的电导率为8.6×107S/m。

Claims (4)

1.一种镱锰铜合金/腈纶电子导线的制备方法，其特征在于：
1）将腈纶纤维依次用重量百分比浓度为10%的草酸水溶液、5% 的双氧水溶液、去离子水洗净、烘干；
2）将洗净的腈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，得改性腈纶纤维；
3）将改性腈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3%的硼氢化钠水溶液中10分钟，取出，用去离子水洗净，得活化腈纶纤维；
4）将活化腈纶纤维置于镱锰铜化学镀溶液中，于25℃化学镀3小时，取出洗净，烘干，得镱锰铜合金/腈纶电子导线。
2.如权利要求1所述的镱锰铜合金/腈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；
氰基丙烯酸乙酯浓度9~12 g/L；
过氧化苯甲酰浓度1~3 g/L；
丙酮浓度100~200 g/L。
3.如权利要求1所述的镱锰铜合金/腈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：
硫酸铝浓度 20~30g/L；
硫酸镍浓度 20~30g/L；
酒石酸钠浓度20~30g/L。
4.如权利要求1所述的镱锰铜合金/腈纶电子导线的制备方法，其特征在于所述的镱锰铜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：
硝酸镱浓度 20~30g/L；
硫酸铜浓度 20~30g/L；
硝酸锰浓度 40~60g/L；
碳酸氢钠浓度 30~60g/L；
酒石酸钠浓度60~90g/L；
二甲氨基硼烷浓度 3~6g/L；
草酸铵浓度6~9g/L。
CN201610474574.1A 2016-06-27 2016-06-27 镱锰铜合金/腈纶电子导线的制备方法 Pending CN106120311A (zh)

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