CN114075352A - 一种柔性传感器用导电橡胶及其制备方法 - Google Patents
一种柔性传感器用导电橡胶及其制备方法 Download PDFInfo
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- CN114075352A CN114075352A CN202010804540.0A CN202010804540A CN114075352A CN 114075352 A CN114075352 A CN 114075352A CN 202010804540 A CN202010804540 A CN 202010804540A CN 114075352 A CN114075352 A CN 114075352A
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- latex
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Abstract
本发明公开了一种柔性传感器用导电橡胶及其制备方法，其采用湿法混炼工艺将制备所得的导电剂水性分散液和液态胶乳混合，实现导电剂和胶乳在纳米尺度上的有效混合，且经过烘干脱水形成橡胶生胶；该方法避免了传统导电橡胶采用干法混炼时对橡胶分子产生破坏的情况，且导电剂采用了两种及两种以上不同微观形态，利用不同微观形态的导电剂之间的协同效应，使不同维度之间的导电剂可以在橡胶基体中搭建更加完善的导电网络，从而提高了导电橡胶的导电性能。
Description
技术领域
本发明涉及一种导电橡胶及其制备方法，尤其涉及一种柔性传感器用导电橡胶及其制备方法，属于柔性传感器用功能材料技术领域。
背景技术
随着智能化水平的不断提升，传感器作为物联世界的重要神经触角变得越来越重要。面对越来越多的特殊信号和特殊环境，传感器需要具有透明、柔韧、延展、可自由弯曲甚至折叠、便于携带、可穿戴等特点，传统脆性硅半导体传感器很难满足这些新的需求，而基于橡胶等弹性体材料的柔性传感器能够有效的解决这些问题。
目前柔性传感器通常采用导电橡胶作为感应材料，其原理是利用导电橡胶在不同应变状态下电学性能的变化制备形成传感器。但是目前现有的这类导电橡胶通常是采用炭黑等导电剂通过密炼或者开炼的方式加入到固态橡胶基体中制备所得的，这种加工方法不仅能耗高、扬尘严重，而且粉状的导电剂在固态橡胶基体中需要长时间的高速剪切才能良好分散；同时为了在橡胶基体中形成有效的导电网络，通常需要填充较高比例的导电剂，而导电剂填充比例的增加会对橡胶的硬度、弹性及其他性能造成影响，且橡胶基体也会因为长时间的高温高速剪切而性能下降，从而难以制备高性能的导电橡胶材料。
因此本领域技术人员急需一种可以有效保证橡胶性能的柔性传感器用导电橡胶及其制备方法。
发明内容
为克服橡胶基体因长时间高温高速剪切而出现的性能下降，以及导电剂在橡胶基体中因分散不均而出现电阻过高等问题，本发明提供了一种柔性传感器用导电橡胶及其制备方法，由该制备方法制备所得的导电橡胶在保证具有良好有效的橡胶性能基础上具有优异的导电性，适用于柔性传感器中。
本发明的技术方案是：
一种柔性传感器用导电橡胶，由主要包括下述按重量份计的各组分原料制备而成：固含量为60wt.％的橡胶胶乳100份、活化剂0.1-30份、促进剂0.1-10份、硫磺0.1-10份、导电剂0.1-90份、防老化剂0.1-10份、离子型高分子分散剂0.1-10份；其中所述导电剂由至少两种具有不同微观形态的导电剂组成。
其进一步的技术方案是：
所述橡胶胶乳为天然橡胶胶乳、人工聚合形成的胶乳和通过物理溶解分散方法制备形成的人造胶乳中的至少一种。
其进一步的技术方案是：
所述人工聚合形成的胶乳包括丁苯橡胶乳液、丁腈橡胶乳液、氯丁橡胶乳液、丁二烯胶乳、聚硫胶乳、氟橡胶胶乳、硅橡胶胶乳、均聚醋酸乙烯酯胶乳、共聚醋酸乙烯酯胶乳、丙烯酸酯乳液、聚氯乙烯胶乳、偏氯乙烯胶乳和苯丙胶乳中的至少一种；所述通过物理溶解分散方法制备形成的人造胶乳包括丁基胶乳、聚异戊二烯胶乳、乙丙胶乳、聚氨酯胶乳、聚乙烯胶乳和环氧树脂胶乳中的至少一种。
其进一步的技术方案是：
所述导电剂由导电炭黑、石墨、导电碳纤维、碳纳米管、导电晶须、石墨烯、富勒烯和金属基导电颗粒中的至少两种具有不同微观形态的导电剂混合组成。
其进一步的技术方案是：
所述导电炭黑包括导电槽黑炭黑(CC)、导电炉法炭黑(CF)、超导电炉法炭黑(SCF)、特导电炉法炭黑(XCF)和乙炔炭黑(ACEF)中的至少一种；所述石墨包括鳞片石墨、膨胀石墨、膨胀石墨微粉和蠕虫状石墨中的至少一种；所述金属基导电颗粒包括银粉、铜粉、镀银玻璃微珠和镀银镍粉中的至少一种。
其进一步的技术方案是：
所述活化剂为普通氧化锌、活性氧化锌、碳酸锌、氧化镁、氧化钙、一氧化铅、四氧化铅、碳酸镁、碱式碳酸铅、碱式硅酸铝、氯化亚锡、氧化镉、氢氧化钙、硬脂酸、硬脂酸锌、硬脂酸铅、油酸、月桂酸、三乙醇胺、二甘醇、聚对二亚硝基苯、四氯苯醌和三甲基丙烯酸三羟甲基丙烷酯中的至少一种。
其进一步的技术方案是：
所述促进剂为二硫代甲酸盐类促进剂、黄原酸类促进剂、秋兰姆类促进剂、噻唑类促进剂、次磺酰胺类促进剂、胍类促进剂、硫脲类促进剂、醛胺类促进剂和胺类促进剂中的至少一种。
其进一步的技术方案是：
所述防老化剂为防老剂4010、防老剂A、防老剂D、防老剂IPPD、防老剂6PPD、防老剂7PPD、防老剂DTPD、防老剂H、防老剂DNP、防老剂TPPD、防老剂OPPD、防老剂4030和防老剂8PPD中的至少一种。
其进一步的技术方案是：
所述离子型高分子分散剂为聚丙烯酸及其盐、聚甲基丙烯酸及其盐、苯乙烯丙烯酸共聚物及其盐、乙烯丙烯酸共聚物及其盐、羧基纤维素及其盐、藻酸及其盐、聚马来酸及其盐、马来酸酐共聚物及其盐、聚酰胺、苯磺酸共聚物、直链烷基苯磺酸钠(LAS)、脂肪醇聚氧乙烯醚硫酸钠(AES)、脂肪醇聚氧乙烯醚硫酸铵(AESA)、木质素磺酸盐、重烷基苯磺酸盐和烷基磺酸盐(石油磺酸盐)中的至少一种。
本发明还公开了一种上述柔性传感器用导电橡胶的制备方法，该制备方法主要包括下述步骤：
S1，称取各组分原料：固含量为60wt.％的橡胶胶乳100份、活化剂0.1-30份、促进剂0.1-10份、硫磺0.1-10份、导电剂0.1-90份、防老化剂0.1-10份和离子型高分子分散剂0.1-10份；
S2，导电剂水性分散液的制备：将离子型高分子分散剂加入到水中充分搅拌溶解后，再加入导电剂、硫磺、活化剂、促进剂和防老化剂进行初步搅拌分散成浆料后，将该浆料通入研磨机中研磨0.5-24h，形成稳定均一的导电剂水性分散液；
S3，制备乳胶混合液：将步骤S2中所得导电剂水性分散液加入橡胶胶乳中，并于常温下搅拌15-60min形成胶乳混合液；
S4，涂布烘干脱水：将步骤S3中所得胶乳混合液采用涂布方式涂布后烘干脱水或采用直接导入模具后烘干脱水，形成片状混炼胶；
S5，硫化成型：将步骤S4中所得经烘干后的片状混炼胶按需裁剪、拼接成所需形状后，经过硫化可得所述柔性传感器用导电橡胶。
本发明的有益技术效果是：本发明采用湿法混炼工艺进行柔性传感器用导电橡胶的制备，其先制备导电剂水性分散液，然后将该导电剂水性分散液和液态胶乳进行混合，该方法能够实现导电剂和胶乳在纳米尺度上的有效混合，且经过烘干脱水形成橡胶生胶，避免了传统导电橡胶采用干法混炼时对橡胶分子产生破坏的情况；此外，本发明中的导电剂采用了两种及两种以上不同微观形态，如采用链球状导电炭黑和片状石墨，或采用纤维状碳纳米管和片状石墨烯等，上述不同形貌的导电剂之间存在协同效应，如零维颗粒状的炭黑可以堆积成导电团簇，一维的碳纤维、碳纳米管、导电晶须可以形成长的导电链，二维的片状石墨和石墨烯可以形成平面状的导电片层，一维和二维的导电剂可以在零维的颗粒状导电剂之间起到桥梁作用，完善导电橡胶的导电网络，从而提高导电橡胶的导电性能。
具体实施方式
为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，下面结合具体实施例，对本发明的具体实施方式作进一步详细描述，以下实施例用于说明本发明，但不用来限制本发明的范围。
具体实施例1
组分原料为：天然胶乳(固含量60wt.％)为100份；普通氧化锌为3.0份；促进剂ZDMC为1.5份；硫磺为2.0份；导电炭黑SP为3.0份；石墨KS6为10份；防老化剂4010为1.0份；藻酸钠为1.0份。
制备方法：按上述组分原料用量称取各组分；将藻酸钠加入到水中搅拌15min进行充分溶解后，再加入氧化锌、促进剂ZDMC、硫磺、导电炭黑SP、石墨KS6和防老化剂4010进行初步搅拌分散成浆料后，将该浆料通过研磨机中在常温下研磨5h，形成稳定均一的导电剂水性分散液；然后将该导电剂水性分散液加入到天然胶乳中，并于常温下搅拌30min形成胶乳混合液；将该胶乳混合物倒入平板模具中烘干脱水，形成片状混炼胶，将该片状混炼胶在130℃下模压加热20min得到柔性传感器用导电橡胶。
具体实施例2
组分原料为：天然胶乳(固含量60wt.％)为100份；活性氧化锌为5.0份；促进剂ZDMC为2.0份；硫磺为3.0份；导电炭黑SP为5.0份；石墨KS6为13份；防老化剂6PPD为1.5份；聚甲基丙烯酸钠为2.0份。
制备方法：按上述组分原料用量称取各组分；将聚甲基丙烯酸钠加入到水中搅拌15min进行充分溶解后，再加入活性氧化锌、促进剂ZDMC、硫磺、导电炭黑SP、石墨KS6和防老化剂6PPD进行初步搅拌分散成浆料后，将该浆料通过研磨机中在常温下研磨5h，形成稳定均一的导电剂水性分散液；然后将该导电剂水性分散液加入到天然胶乳中，并于常温下搅拌30min形成胶乳混合液；将该胶乳混合物倒入平板模具中烘干脱水，形成片状混炼胶，将该片状混炼胶在130℃下模压加热20min得到柔性传感器用导电橡胶。
具体实施例3
组分原料为：丁苯橡胶乳液(固含量60wt.％)为100份；活性氧化锌为5.0份；促进剂ZDMC为3.0份；硫磺为2.0份；导电炭黑SP为5.0份；石墨KS6为15份；镀银镍粉5.0份；防老化剂DNP为2.0份；脂肪醇聚氧乙烯醚硫酸钠为5.0份。
制备方法：按上述组分原料用量称取各组分；将脂肪醇聚氧乙烯醚硫酸钠加入到水中搅拌15min进行充分溶解后，再加入活性氧化锌、促进剂ZDMC、硫磺、导电炭黑SP、石墨KS6、镀银镍粉和防老化剂DNP进行初步搅拌分散成浆料后，将该浆料通过研磨机中在常温下研磨5h，形成稳定均一的导电剂水性分散液；然后将该导电剂水性分散液加入到天然胶乳中，并于常温下搅拌30min形成胶乳混合液；将该胶乳混合物倒入平板模具中烘干脱水，形成片状混炼胶，将该片状混炼胶在130℃下模压加热20min得到柔性传感器用导电橡胶。
将上述具体实施例1-3制备所得的柔性传感器用导电橡胶，按照表1中所示测试项目和测试标准进行性能测试，测试结果参见表1所示。
表1具体实施例1-3性能测试结果
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。
Claims (10)
1.一种柔性传感器用导电橡胶，其特征在于，由主要包括下述按重量份计的各组分原料制备而成：固含量为60wt.％的橡胶胶乳100份、活化剂0.1-30份、促进剂0.1-10份、硫磺0.1-10份、导电剂0.1-90份、防老化剂0.1-10份、离子型高分子分散剂0.1-10份；其中所述导电剂由至少两种具有不同微观形态的导电剂组成。
2.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述橡胶胶乳为天然橡胶胶乳、人工聚合形成的胶乳和通过物理溶解分散方法制备形成的人造胶乳中的至少一种。
3.根据权利要求2所述的柔性传感器用导电橡胶，其特征在于，所述人工聚合形成的胶乳包括丁苯橡胶乳液、丁腈橡胶乳液、氯丁橡胶乳液、丁二烯胶乳、聚硫胶乳、氟橡胶胶乳、硅橡胶胶乳、均聚醋酸乙烯酯胶乳、共聚醋酸乙烯酯胶乳、丙烯酸酯乳液、聚氯乙烯胶乳、偏氯乙烯胶乳和苯丙胶乳中的至少一种；所述通过物理溶解分散方法制备形成的人造胶乳包括丁基胶乳、聚异戊二烯胶乳、乙丙胶乳、聚氨酯胶乳、聚乙烯胶乳和环氧树脂胶乳中的至少一种。
4.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述导电剂由导电炭黑、石墨、导电碳纤维、碳纳米管、导电晶须、石墨烯、富勒烯和金属基导电颗粒中的至少两种具有不同微观形态的导电剂混合组成。
5.根据权利要求4所述的柔性传感器用导电橡胶，其特征在于，所述导电炭黑包括导电槽黑炭黑、导电炉法炭黑、超导电炉法炭黑、特导电炉法炭黑和乙炔炭黑中的至少一种；所述石墨包括鳞片石墨、膨胀石墨、膨胀石墨微粉和蠕虫状石墨中的至少一种；所述金属基导电颗粒包括银粉、铜粉、镀银玻璃微珠和镀银镍粉中的至少一种。
6.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述活化剂为普通氧化锌、活性氧化锌、碳酸锌、氧化镁、氧化钙、一氧化铅、四氧化铅、碳酸镁、碱式碳酸铅、碱式硅酸铝、氯化亚锡、氧化镉、氢氧化钙、硬脂酸、硬脂酸锌、硬脂酸铅、油酸、月桂酸、三乙醇胺、二甘醇、聚对二亚硝基苯、四氯苯醌和三甲基丙烯酸三羟甲基丙烷酯中的至少一种。
7.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述促进剂为二硫代甲酸盐类促进剂、黄原酸类促进剂、秋兰姆类促进剂、噻唑类促进剂、次磺酰胺类促进剂、胍类促进剂、硫脲类促进剂、醛胺类促进剂和胺类促进剂中的至少一种。
8.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述防老化剂为防老剂4010、防老剂A、防老剂D、防老剂IPPD、防老剂6PPD、防老剂7PPD、防老剂DTPD、防老剂H、防老剂DNP、防老剂TPPD、防老剂OPPD、防老剂4030和防老剂8PPD中的至少一种。
9.根据权利要求1所述的柔性传感器用导电橡胶，其特征在于，所述离子型高分子分散剂为聚丙烯酸及其盐、聚甲基丙烯酸及其盐、苯乙烯丙烯酸共聚物及其盐、乙烯丙烯酸共聚物及其盐、羧基纤维素及其盐、藻酸及其盐、聚马来酸及其盐、马来酸酐共聚物及其盐、聚酰胺、苯磺酸共聚物、直链烷基苯磺酸钠、脂肪醇聚氧乙烯醚硫酸钠、脂肪醇聚氧乙烯醚硫酸铵、木质素磺酸盐、重烷基苯磺酸盐和烷基磺酸盐中的至少一种。
10.根据权利要求1至9中任一权利要求所述柔性传感器用导电橡胶的制备方法，其特征在于，主要包括下述步骤：
S1，称取各组分原料：固含量为60wt.％的橡胶胶乳100份、活化剂0.1-30份、促进剂0.1-10份、硫磺0.1-10份、导电剂0.1-90份、防老化剂0.1-10份和离子型高分子分散剂0.1-10份；
S2，导电剂水性分散液的制备：将离子型高分子分散剂加入到水中充分搅拌溶解后，再加入导电剂、硫磺、活化剂、促进剂和防老化剂进行初步搅拌分散成浆料后，将该浆料通入研磨机中研磨0.5-24h，形成稳定均一的导电剂水性分散液；
S3，制备乳胶混合液：将步骤S2中所得导电剂水性分散液加入橡胶胶乳中，并于常温下搅拌15-60min形成胶乳混合液；
S4，涂布烘干脱水：将步骤S3中所得胶乳混合液采用涂布方式涂布后烘干脱水或采用直接导入模具后烘干脱水，形成片状混炼胶；
S5，硫化成型：将步骤S4中所得经烘干后的片状混炼胶按需裁剪、拼接成所需形状后，经过硫化可得所述柔性传感器用导电橡胶。
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