CN115538163B - 一种纤维神经电极及其制备方法 - Google Patents
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Abstract
本发明属于神经电极领域,具体为一种纤维神经电极及其制备方法。本发明通过湿法纺丝将导电高分子制备成为纳米级纤维网络,并将人工液体基质填充于纳米纤维网络形成导电高分子纤维电极,通过调节液体基质的溶度参数得到模量为50‑1000kPa的纤维神经电极。制备步骤包括纺丝液的制备、湿法纺丝形成初级纤维电极、初级纤维电极再浸润、纤维电极绝缘处理。本发明制备的纤维神经电极具有优异的力学性能和电学性能,其可以在麻醉至剧烈运动状态下稳定记录神经信号。
Description
技术领域
本发明属于神经电极领域,具体涉及一种适用于麻醉至剧烈运动的纤维神经电极及其制备方法。
背景技术
随着对大脑不断深入研究,研究人员认为,了解人类认知的神经基础是神经科学的普遍目标,其对于脑部疾病的诊疗和干预有重要意义。
植入式神经电极是检测大脑电生理信号的重要手段。为此,研究者们开发了一系列神经电极,包括金属、硅基、聚合物和碳材料等,为可靠地解释与分析大脑功能提供了诸多可能性。然而,目前已开发的神经电极材料的模量处于吉帕级别,与模量为千帕级别的脑组织之间存在机械不匹配,无法建立稳定的电极/组织界面,在植入后容易引起严重的免疫反应,并在长期的自由活动过程中丢失信号记录。目前,尚未开发出能在剧烈运动下稳定记录的神经电极。因此,制备出与脑组织模量匹配、具有优秀电化学性能的神经电极,实现在麻醉至剧烈运动情况下长期稳定记录电生理信号是亟待解决的技术性难题。
发明内容
本发明所要解决的技术问题在于,针对当前神经电极与脑组织之间模量不匹配、无法在剧烈运动下稳定工作的问题,提供一种低模量(kPa级别)、低阻抗(<1000kΩ·μm2)和高电导(>100S/cm)的纤维神经电极及其制备方法,其可在麻醉至剧烈运动情况下实现电生理信号稳定监测。
本本发明所要解决的技术问题采用以下的技术方案来实现:
一种适用于麻醉至剧烈运动的纤维神经电极及其制备方法,以导电高分子构建纳米级纤维网络,使用生物安全性液体基质填充网络,形成模量为50-1000kPa的纤维神经电极。具体步骤如下:
(1)制备低浓度、分散稳定的导电高分子分散液,然后将导电高分子分散液加热浓缩至固体含量为2-15%,加入小分子调节剂,调节导电高分子的链端舒展性。使用过滤器去掉杂质和气泡,再进一步使用真空烘箱除气泡。
(2)通过湿法纺丝技术对步骤(1)制备的导电高分子分散液进行连续化纺丝,然后使用去离子水清洗掉残留的凝固浴成分,晾干后得到具有纳米网络的初级纤维。
(3)将不同根初级纤维进行加捻,得到不同直径的导电纤维。
(4)将步骤(3)制备的导电纤维浸泡于生物相容性的液体基质中,使液体基质填充到导电纤维的纳米网络中,得到低模量、低阻抗和高电导率的柔性纤维电极。
(5)使用易挥发溶剂配置氟橡胶溶液,对步骤(4)制备的纤维电极进行绝缘处理,得到纤维神经电极。溶剂选用有机系,并且与步骤(4)使用的液体基质不相溶。
进一步地,所述步骤(1)中导电高分子为聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)聚合物。所述溶解导电高分子的溶剂为水,质量分数为85-98%。
进一步地,所述步骤(1)中小分子调节剂为二甲亚砜,浓度为2-5%。
进一步地,所述步骤(2)中凝固浴为异丙醇和二甲亚砜,所述体积比为9:1。
进一步地,所述步骤(4)中液体基质为水和甘油混合液,水和甘油混合液比例1:20-20:1。改变水和甘油的摩尔比例,可以获得模量从几十千帕到几兆帕的纤维电极。
进一步地,所述步骤(4)中纤维电极在液体基质中浸泡时间为1-4小时。导电纤维模量可以通过改变液体基质和纳米纤维网络中所用高分子的溶度参数之差来调控。
进一步地,所述步骤(5)中溶解氟橡胶的溶剂为4-甲基-2-戊酮,所述氟橡胶溶液的质量分数为10-20%。
进一步地,所述步骤(5)中纤维电极进行绝缘过程为:将导电纤维置于四氟乙烯支架上,浸没于氟橡胶溶液中,然后缓慢匀速拉出,控制纤维表面不产生挂珠现象。
进一步地,将一根或多根融合的导电纤维和氟橡胶绝缘层可以组成任意通道数的纤维神经电极。
本发明制备的纤维神经电极可以在电声理中应用,包括刺激和记录,将其运用于动物体内,在麻醉至剧烈运动情况下可以实现稳定电信号记录。
本发明有益效果是:
(1)本发明制备的纤维神经电极模量在50-1000kPa范围内可调,模量和特征阻抗均处于领先水平。在循环拉伸10000次后电化学阻抗保持稳定,在37摄氏度液体环境保存5个月电化学性能保持稳定。
(2)在剧烈运动时纤维神经电极保持高质量的电生理信号记录,实现长达5个月多通道电信号稳定记录。
附图说明
图1为湿法纺丝流程示意图;
图2为纤维神经电极内纳米纤维网络图;
图3为涂覆绝缘层后的纤维电极图;
图4为实施例1纤维神经电极循环拉伸10000次后电化学阻抗的曲线图;
图5为实施例1纤维神经电极在37摄氏度液体环境保存5个月电化学性能曲线图。
具体实施方式
下面结合实施例和附图对本发明的具体实施方式做进一步的详细描述。以下实施例和附图用于说明本发明,但不用来限制本发明的范围。
实施例1纤维状神经电极的制备
(1)纺丝悬浮液的制备。将4克聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)水溶液(分散液)放入玻璃瓶中,放置于50摄氏度热台上加热蒸发水分,每隔5分钟摇晃玻璃瓶一次直至溶液浓缩为固含量2%。在浓缩溶液中加入2%的二甲亚砜,放置于磁力搅拌台上搅拌1小时,用0.45微米的水系过滤器过滤搅拌后的溶液,过滤后在室温下使用真空烘箱除去气泡得到纺丝悬浮液。
(2)湿法纺丝制备初级导电纤维。将450毫升异丙醇与50毫升二甲亚砜混合制备凝固浴。将0.5克纺丝悬浮液吸入1毫升注射器中,注射器针头连接硅胶软管,硅胶软管另一头连接16G点胶针,点胶针针头没入凝固浴液面。1毫升注射器固定于注射泵上,以100微升/分钟的流量进行湿法纺丝。湿法纺丝得到的纤维转移至去离子水中浸泡1小时后,以一定张力搭接在架子上室温下晾干4小时,得到初级电极。
(3)初级导电纤维填充液体基质。60克去离子水和18克甘油混合,经磁力搅拌12小时,得到满足不同模量需求的的液体基质。将一根初级电极浸泡于液体基质1小时后取出,在室温下晾干4小时后得到一根模量约为1000kPa的纤维状神经电极。
(4)纤维电极绝缘处理,制备纤维神经电极。将5克氟橡胶溶解于45克4-甲基-2-戊酮溶剂中,在50摄氏度下搅拌12小时,得到质量分数为10%的透明粘性溶液,将一根神经电极浸入粘性溶液中匀速拉拔而出,在通风橱内晾干12小时,得到外围包覆氟橡胶绝缘层的纤维电极。
(4)电极可用于外周神经及肠道神经等的在体长期检测。
实施例2多根融合的纤维状神经电极的制备
(1)纺丝悬浮液的制备。将10克聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)水溶液(分散液)放入玻璃瓶中,放置于90摄氏度热台上加热蒸发水分,每隔10分钟摇晃玻璃瓶一次直至溶液浓缩为固含量15%。在浓缩溶液中加入5%的二甲亚砜,放置于磁力搅拌台上搅拌5小时,用0.45微米的水系过滤器过滤搅拌后的溶液,过滤后在室温下使用真空烘箱除去气泡得到纺丝悬浮液。
(2)湿法纺丝制备初级导电纤维。将450毫升异丙醇与50毫升二甲亚砜混合制备凝固浴。将1克纺丝悬浮液吸入1毫升注射器中,注射器针头连接硅胶软管,硅胶软管另一头连接32G点胶针,点胶针针头没入凝固浴液面。1毫升注射器固定于注射泵上,以600微升/分钟的流量进行湿法纺丝。湿法纺丝得到的纤维转移至去离子水中浸泡5小时后,以一定张力搭接在架子上室温下晾干10小时,得到初级电极。
(3)初级导电纤维填充液体基质。80克去离子水和83克甘油混合,经磁力搅拌12小时,得到满足不同模量需求的的液体基质。将多根初级电极加捻后浸泡于渗透溶液中,4小时后取出,在室温下晾干10小时后得到多根融合为一根模量约为300kPa的整体的纤维状神经电极。
(4)纤维电极绝缘处理,制备纤维神经电极。将20克氟橡胶溶解于80克4-甲基-2-戊酮溶剂中,在80摄氏度下搅拌12小时,得到质量分数为20%的透明粘性溶液,将一根神经电极浸入粘性溶液中匀速拉拔而出,在通风橱内晾干12小时,得到外围包覆氟橡胶绝缘层的纤维电极。
实施例3多通道纤维状神经电极的制备:
(1)纺丝悬浮液的制备。将7克聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)水溶液(分散液)放入玻璃瓶中,放置于90摄氏度热台上加热蒸发水分,每隔10分钟摇晃玻璃瓶一次直至溶液浓缩为固含量8%。在浓缩溶液中加入5%的二甲亚砜,放置于磁力搅拌台上搅拌3小时,用0.45微米的水系过滤器过滤搅拌后的溶液,过滤后在室温下使用真空烘箱除去气泡得到纺丝悬浮液。
(2)湿法纺丝制备初级导电纤维。将450毫升异丙醇与50毫升二甲亚砜混合制备凝固浴。将1克纺丝悬浮液吸入1毫升注射器中,注射器针头连接硅胶软管,硅胶软管另一头连接23G点胶针,点胶针针头没入凝固浴液面。1毫升注射器固定于注射泵上,以300微升/分钟的流量进行湿法纺丝。湿法纺丝得到的纤维转移至去离子水中浸泡3小时后,以一定张力搭接在架子上室温下晾干7小时,得到初级电极。
(3)初级导电纤维填充液体基质。40克去离子水和80克甘油混合,经磁力搅拌12小时,得到满足不同模量需求的的液体基质。在室温下晾干7小时得到模量约为50KPa的纤维电极。
(4)纤维电极绝缘处理,制备纤维神经电极。将9克氟橡胶溶解于51克4-甲基-2-戊酮溶剂中,在60摄氏度下搅拌12小时,得到质量分数为15%的透明粘性溶液,将一根神经电极浸入粘性溶液中匀速拉拔而出,在通风橱内晾干12小时,得到外围包覆氟橡胶绝缘层的纤维电极。
(5)将多根(4)中所述电极加捻或者平行排列在一起,组成多通道神经电极,用刚性探针辅助植入体内。
(6)在小鼠脑内植入后,使用牙科水泥固定。在恢复一段时间后进行在体测试,除了能在麻醉、头部固定和自由活动时稳定记录神经信号,例如单神经元的跟踪,还能实现在剧烈运动时同样稳定追踪单神经元信号。对照组(刚性电极如金属丝电极)不能在剧烈运动时实现稳定记录。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (6)
1.一种纤维神经电极的制备方法,其特征在于,所述纤维神经电极具体制备方法如下:
(1)制备分散稳定的导电高分子分散液,然后将导电高分子分散液加热浓缩至固体含量为2-15%,加入小分子调节剂,调节导电高分子的链端舒展性;
步骤(1)中所述导电高分子分散液由导电高分子和溶剂混合而成,所述导电高分子分散液中导电高分子质量分数为80-96%;其中导电高分子为聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)聚合物,溶剂为水;
步骤(1)中所述小分子调节剂为二甲亚砜,浓度为 2-5%;
(2)通过湿法纺丝技术对步骤(1)制备的导电高分子分散液进行连续化纺丝,然后清洗掉残留的凝固浴成分,干燥后得到具有纳米网络的初级纤维;
(3)将不同根初级纤维进行加捻,得到不同直径的导电纤维;
(4)将步骤(3)制备的导电纤维浸泡于生物相容性的液体基质中,使液体基质填充到导电纤维的纳米网络中,得到柔性纤维电极;
步骤(4)中所述液体基质为水和甘油混合液,水和甘油混合液比例为1:20-20:1;
(5)使用易挥发溶剂配置氟橡胶溶液,对步骤(4)制备的柔性纤维电极进行绝缘处理,得到纤维神经电极;
步骤(5)中溶解氟橡胶的溶剂为4-甲基-2-戊酮,所述氟橡胶溶液中氟橡胶的质量分数为10-20%;
步骤(5)中所述纤维电极进行绝缘的过程为:将导电纤维置于四氟乙烯支架上,浸没于氟橡胶溶液中,然后缓慢匀速拉出,控制纤维表面不产生挂珠现象。
2.根据权利要求1所述纤维神经电极的制备方法,其特征在于,步骤(2)中所述凝固浴为异丙醇和二甲亚砜,体积比为9:1。
3.根据权利要求1所述纤维神经电极的制备方法,其特征在于,步骤(4)中纤维电极在液体基质中浸泡时间为1-4小时。
4.如权利要求1所述的制备方法得到的纤维神经电极,经过组装形成任意通道数的纤维神经电极。
5.如权利要求4所述的纤维神经电极,其特征在于,所述纤维神经电极在电声理中的应用,包括刺激和记录。
6.如权利要求5所述的纤维神经电极,其特征在于,所述纤维神经电极适用于在麻醉至剧烈运动状态下动物体内电生理信号监测。
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