CN112121237A - 具备生物活性的脑深部植入复合导电涂层电极及制备方法 - Google Patents
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Abstract
本申请公开了具备生物活性的脑深部植入复合导电涂层电极及其制备方法,包括:植入电极本体,所述植入电极本体的下端为自由端,所述植入电极本体的上端连接导线,所述植入电极本体自由端设置若干个电刺激区域,其余区域为绝缘区域,所述电刺激区域表面制备有具备生物活性的复合导电涂层;所述具备生物活性的复合导电涂层由内及表依次是:金属基底、聚吡咯导电层和聚多巴胺生物纳米层;其中,所述金属基底表面制备亲水性表面微织构;所述聚吡咯导电层内部掺杂纳米氧化锌颗粒。
Description
技术领域
本申请涉及脑科学及电极技术领域,特别是涉及具备生物活性的脑深部植入复合导电涂层电极及制备方法。
背景技术
本部分的陈述仅仅是提到了与本申请相关的背景技术,并不必然构成现有技术。
自1990年国外首次报道脑深部植入电极电刺激(DBS)对神经退行性疾病的治疗以来,DBS手术为神经退行性疾病的治疗提供了新的思路。然而,由于电极材料与脑组织力学失配、细菌感染以及其与神经细胞相容性较差等原因,导致植入组织发生感染且植入脑内的电极逐渐被小胶质细胞和星型胶质细胞所包裹。随着时间增长,形成胶质包膜,致使电极电阻增大,失去电刺激治疗效果。这减少了脑深部植入电极使用寿命,增加二次手术概率。
发明内容
为了解决现有技术的不足,本申请提供了具备生物活性的脑深部植入复合导电涂层电极及制备方法;
第一方面,本申请提供了具备生物活性的脑深部植入复合导电涂层电极;
具备生物活性的脑深部植入复合导电涂层电极,包括:
植入电极本体,所述植入电极本体的下端为自由端,所述植入电极本体的上端连接导线,导线用于与外部电源连接;所述植入电极本体自由端设置若干个电刺激区域,所述植入电极本体的非电刺激区域即为绝缘区域,所述电刺激区域表面制备具有生物活性的复合导电涂层;
所述具备生物活性的复合导电涂层由内及表依次为:金属基底、聚吡咯(Ppy)导电层和聚多巴胺(PDA)生物纳米层;其中,所述金属基底表面制备亲水性表面微织构;所述聚吡咯(Ppy)导电层内部掺杂纳米氧化锌(Nano-ZnO)颗粒。
第二方面,本申请提供了具备生物活性的脑深部植入复合导电涂层电极的制备方法;
具备生物活性的脑深部植入复合导电涂层电极的制备方法,包括:
采用紫外激光镭射方式,在植入电极本体的金属基底表面制备亲水性微织构;
利用超声震荡分散方式,将抗菌纳米氧化锌粒子均匀分散于电解液;通过电化学法,在植入电极本体的表面微织构上沉积掺杂纳米氧化锌的聚吡咯导电层;
采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层。
与现有技术相比,本申请的有益效果是:
(1)在生物医用金属基底上制备具有良好抗菌性、生物活性和导电性的复合涂层。基底表面亲水微织构的引入在保证涂层结构、形貌的同时,增大了膜-基结合面积,对提升膜-基结合强度有重要作用。复合涂层的设计改善了植入手术感染、植入电极与脑组织生物相容性差等问题。
(2)基底表面亲水性微织构的设计解决了复合生物活性导电涂层因残余应力大、亲润性差引起的膜-基结合强度低等问题;
(3)复合涂层中三组分相互协同作用,提升脑深部植入电极的整体性能:聚吡咯在提升基底金属导电性的同时降低了其力学特性,从而缓解脑组织因力学适配引起的炎性反应;
(4)掺杂在聚吡咯涂层内的纳米氧化锌缓释锌离子不但起到杀菌作用还协同表层聚多巴胺纳米层促进神经细胞增殖,而纳米级聚多巴胺层在不降低电极电导率的同时提升电极的生物活性;
(5)复合生物活性导电层成分均对人体无害。金属质脑深部植入电极与脑组织力学性差异大,术后易对脑组织造成物理损伤,引起组织炎性反应,久而久之生成胶质包膜、神经细胞退化以及植入电极失效的问题,达到了本申请的目的。
(6)本申请结合激光镭射与电化学沉积技术在金属基表面制备出生物活性导电复合涂层,具有结合强度高、抗菌性强、导电性好以及生物相容性优异等系列优点,有效解决脑深部植入手术的术中感染、术后组织损伤以及胶质瘢痕等系列问题,提高了脑深部植入电极性能与寿命。
附图说明
构成本申请的一部分的说明书附图用来提供对本申请的进一步理解,本申请的示意性实施例及其说明用于解释本申请,并不构成对本申请的不当限定。
图1为本申请的脑深部植入电极的结构示意图。
图2为本申请的脑深部植入电极的结构剖面图。
图3为本申请的脑深部植入电极表面生物活性复合导电涂层的结构示意图。
图4为本申请的金属基底表面微织构的结构示意图。
具体实施方式
应该指出,以下详细说明都是示例性的,旨在对本申请提供进一步的说明。除非另有指明,本文使用的所有技术和科学术语具有与本申请所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是,这里所使用的术语仅是为了描述具体实施方式,而非意图限制根据本申请的示例性实施方式。如在这里所使用的,除非上下文另外明确指出,否则单数形式也意图包括复数形式,此外,还应当理解的是,术语“包括”和“具有”以及他们的任何变形,意图在于覆盖不排他的包含,例如,包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元,而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备固有的其它步骤或单元。
在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。
本申请的目的是提供一种具有膜基结合强度高、抗菌能力强、生物相容性好的具备生物活性的脑深部植入复合导电涂层电极及其制备方法,以解决纯金属脑深部植入电极与周围脑组织力学性能失配、术后感染以及生物相容性差引起的胶质瘢痕的问题。
实施例一
本实施例提供了具备生物活性的脑深部植入复合导电涂层电极;
如图1、图2、图3和图4所示,具备生物活性的脑深部植入复合导电涂层电极,包括:
植入电极本体,所述植入电极本体的下端为自由端,所述植入电极本体的上端连接导线,所述植入电极本体自由端一侧设置若干个电刺激区域,所述植入电极本体的非电刺激区域即为绝缘区域,所述电刺激区域表面制备具有生物活性的复合导电涂层;
所述具备生物活性的复合导电涂层由内及表依次为:金属基底、聚吡咯(Ppy)导电层和聚多巴胺(PDA)生物纳米层;其中,所述金属基底表面制备亲水性表面微织构;所述聚吡咯(Ppy)导电层内部掺杂纳米氧化锌(Nano-ZnO)颗粒。
示例性的,所述电刺激区域设置在电极端部及以上1/3~2/3的几个放电部位,减少放电部位与脑组织之间的应力失配。
进一步地,所述导电涂层整体厚度为:1μm~5μm。
进一步地,所述聚吡咯(Ppy)导电层的厚度为:1μm~4.95μm。
进一步地,所述掺杂纳米氧化锌(Nano-ZnO)颗粒的粒径为40nm~70nm。
进一步地,所述掺杂纳米氧化锌(Nano-ZnO)颗粒的质量分数为:0.1%~3%。
进一步地,所述聚多巴胺(PDA)纳米层的厚度为:10nm~50nm。
进一步地,所述植入电极整体的金属材料为铂、铱、铂铱合金或钨中的一种。
实施例二
本实施例提供了具备生物活性的脑深部植入复合导电涂层电极的制备方法;
具备生物活性的脑深部植入复合导电涂层电极的制备方法,包括:
S101:采用紫外激光镭射方式,在植入电极本体的每个电刺激区域的金属基底表面制备亲水性微织构;
S102:利用超声震荡分散方式,将抗菌纳米氧化锌ZnO粒子均匀分散于电解液;通过电化学法,在植入电极本体的表面微织构上沉积制备掺杂纳米氧化锌的聚吡咯导电层;
S103:采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层。
进一步地,所述S101:采用激光镭射方式,在植入电极本体的金属基底表面制备表面微织构;步骤之前,还包括:
S100:基体预处理:用600目、800目、1000目和1500目砂纸依次打磨植入电极本体的金属基体,后采用研磨膏将其表面研磨至金属基底表面粗糙度Ra=0.04~0.10μm,依次采用丙酮和无水乙醇去离子水超声清洗15min,烘干备用。
进一步地,所述S101:采用紫外激光镭射方式,在植入电极本体的金属基底表面制备亲水性表面微织构;具体步骤包括:
采用紫外激光镭射工艺在植入电极本体的金属基底表面制备网格状微织构,工艺参数:镭射功率范围5W~15W,织构间距50~200μm,宽度20~30μm,深度0.5~1.5μm;
将植入电极本体放入质量分数为10%盐酸溶液酸洗活化处理10min后,再将植入电极本体依次放入丙酮、无水乙醇和去离子水中超声清洗15min,烘干备用。
进一步地,所述S102中,通过电化学法,在植入电极本体的表面微织构上沉积制备掺杂纳米氧化锌的聚吡咯导电层;具体步骤包括:
在纳米氧化锌分散液中,通过三电极体系恒电压法,在植入电极本体的亲水性表面微织构上沉积制备掺杂纳米氧化锌的聚吡咯导电层。
进一步地,所述S102中,通过电化学法,在植入电极本体的亲水性表面微织构上沉积制备掺杂纳米氧化锌的聚吡咯导电层;详细步骤包括:
在纳米氧化锌分散液中,采用三电极体系恒电压法制备聚合导电层,其中基底金属为工作电极,铂丝为对电极,Ag-AgCl为参比电极,沉积电压为0.6V~0.85V,沉积时间200s~1000s。取出试样,去离子水冲洗15min,60℃真空干燥12h。
进一步地,所述纳米氧化锌分散液的配置步骤包括:
称取纳米氧化锌,使电解液中纳米氧化锌浓度保持在0.1g/L~3g/L范围;
将纳米氧化锌和表面活性剂十二烷基苯磺酸钠磁力搅拌10min,超声震荡分散20min;其中,十二烷基苯磺酸钠浓度为0.01M;
称量、配制对甲苯磺酸钠电解质溶液,再次磁力搅拌10min,超声震荡分散20min;其中,对甲苯磺酸钠浓度为0.1M~0.3M;
加入吡咯单体依次搅拌、超声震荡分散5min形成最终电解质;其中,吡咯单体浓度为0.05M~0.3M。
进一步地,所述S103:采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;具体步骤包括:
在碱性缓冲液环境中,采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层。
进一步地,所述S103:采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;具体步骤包括:
配制Tris-HCl缓冲溶液,采用盐酸调至pH=8.5,称量多巴胺粉末,加入Tris-HCl缓冲溶液,使多巴胺浓度为2g/L;放入试样,使其在室温条件下静置24h。
进一步地,所述S103:采用氧化自聚方式,在植入电极本体的聚吡咯导电层沉积聚多巴胺纳米生物活性层;步骤之后,还包括:
涂层后处理:取出试样,分别用无水乙醇、去离子水超声清洗15min,放入真空干燥箱65℃保温12h,后随着干燥箱自然冷却至室温。
本申请所制备的功能复合涂层具有良好的抗菌性、生物相容性和膜-基结合强度。聚吡咯导电层在降低金属基底材料力学性能的同时,提升金属电极导电性,同时,缓释锌离子达到杀菌作用。表层纳米聚多巴胺涂层结合微量锌元素可改善聚吡咯导电层生物活性,促进神经细胞在电极表面及周围的增殖生长。本申请对减少脑深部植入的术中手术感染、术后胶质包膜形成以及延长脑深部植入电极工作寿命具有积极意义。
铂、铱、铂铱合金、钨等惰性金属是常用脑深部刺激电极材料,以该种金属为基底,沉积制备具有生物活性的脑深部植入纳米复合导电涂层电极。
聚吡咯作为一种导电聚合材料,具有制备简单、化学性质稳定、机械性能良好等特点,且随着不同阴离子的掺杂,其电导率可调节范围广泛。因此,其在生物医学领域具备广阔的应用价值。
锌是人体不可或缺的微量元素,对大脑的生长发育具有重要促进作用,且锌离子具备广谱抗菌性,同时,纳米氧化锌颗粒尺寸微小,其表面电子结构和晶体结构发生变化,使其具备宏观颗粒不具备的表面效应、体积效应及量子尺寸效应,这使其广泛应用于生物医学领域。
多巴胺是大脑中含量最丰富的儿茶酚胺类神经递质,也是神经发育的必备物质。多巴胺的缺失易造成神经细胞发育迟缓,脑老化等系列神经退行性疾病,而提升多巴胺含量有助于改善帕金森、多动症等系列神经退行性疾病的症状。这使得聚多巴胺膜在生物医学领域的应用十分广泛。
目前,用于制备聚吡咯的方法主要有化学氧化聚合法和电化学聚合法。化学氧化聚合成本低、工艺简单适合大批量生产,但该法制备的产物多为聚吡咯粉末,难以成膜,不易进一步加工。电化学聚合是在电场作用下,采用电极电位作为聚合反应所需要的能量,经过一段时间的反应,会在电极表面沉积一层共轭高分子聚合膜,但电解液种类、吡咯单体浓度、溶剂以及聚合电压等因素对薄膜的表面形貌、力学、电学性能有着直接影响。多巴胺的聚合反应较为简单,有溶液氧化聚合法和酶氧化聚合法。由于溶液氧化聚合条件简单,成本低廉,应用更为广泛。多巴胺(多巴胺盐酸盐)在避光有氧碱性条件即可发生聚合反应,将基体材料放入反应容器,静置一定时间,其表面即可形成聚多巴胺生物活性膜。研究表明,聚多巴胺薄膜最大沉积厚度为50nm。当达到一定厚度,随着沉积时间增长,薄膜不再增厚。
以上所述仅为本申请的优选实施例而已,并不用于限制本申请,对于本领域的技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。
Claims (10)
1.具备生物活性的脑深部植入复合导电涂层电极,其特征是,包括:
植入电极本体,所述植入电极本体的下端为自由端,所述植入电极本体的上端连接导线,导线用于与外部电源连接;所述植入电极本体自由端设置若干个电刺激区域,所述植入电极本体的非电刺激区域即为绝缘区域,所述电刺激区域表面制备具有生物活性的复合导电涂层;
所述具备生物活性的复合导电涂层由内及表依次为:金属基底、聚吡咯导电层和聚多巴胺生物纳米层;其中,所述金属基底表面制备亲水性表面微织构;所述聚吡咯导电层内部掺杂纳米氧化锌颗粒。
2.如权利要求1所述的电极,其特征是,所述导电涂层整体厚度为:1μm~5μm;所述聚吡咯导电层的厚度为:1μm~4.95μm;所述掺杂纳米氧化锌颗粒的粒径为40nm~70nm;所述掺杂纳米氧化锌颗粒的质量分数为:0.1%~3%;所述聚多巴胺纳米层的厚度为:10nm~50nm。
3.具备生物活性的脑深部植入复合导电涂层电极的制备方法,其特征是,包括:
采用紫外激光镭射方式,在植入电极本体的金属基底表面制备亲水性微织构;
利用超声震荡分散方式,将抗菌纳米氧化锌粒子均匀分散于电解液;通过电化学法,在植入电极本体的微织构表面沉积制备掺杂纳米氧化锌的聚吡咯导电层;
采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层。
4.如权利要求3所述的方法,其特征是,采用紫外激光镭射方式,在植入电极本体的金属基底表面制备表面微织构;步骤之前,还包括:
基体预处理:用600目、800目、1000目和1500目砂纸依次打磨植入电极本体的金属基体,后采用研磨膏将其表面研磨至金属基底表面粗糙度Ra=0.04~0.10μm,依次采用丙酮和无水乙醇去离子水超声清洗15min,烘干备用。
5.如权利要求3所述的方法,其特征是,采用紫外激光镭射方式,在植入电极本体的金属基底表面制备表面亲水性微织构;具体步骤包括:
采用紫外激光镭射工艺在植入电极本体的金属基底表面制备网格状微织构,工艺参数:镭射功率范围为5W~15W,织构间距50~200μm,宽度20~30μm,深度0.5~1.5μm;
将植入电极本体放入质量分数为10%盐酸溶液酸洗活化处理10min后,再将植入电极本体依次放入丙酮、无水乙醇和去离子水中超声清洗15min,烘干备用。
6.如权利要求3所述的方法,其特征是,通过电化学法,在植入电极本体的亲水性微织构表面沉积制备掺杂纳米氧化锌的聚吡咯导电层;具体步骤包括:
在纳米氧化锌分散液中,通过三电极体系恒电压法,在植入电极本体的亲水性微织构表面沉积制备掺杂纳米氧化锌的聚吡咯导电层。
7.如权利要求3所述的方法,其特征是,通过电化学法,在植入电极本体的亲水性微织构表面沉积制备掺杂纳米氧化锌的聚吡咯导电层;详细步骤包括:
在纳米氧化锌分散液中,采用三电极体系恒电压法制备聚合导电层,其中基底金属为工作电极,铂丝为对电极,Ag-AgCl为参比电极,沉积电压为0.6V~0.85V,沉积时间200s~1000s;取出试样,去离子水冲洗15min,60℃真空干燥12h。
8.如权利要求6或7所述的方法,其特征是,所述纳米氧化锌分散液的配置步骤包括:
称取纳米氧化锌,使电解液中纳米氧化锌浓度保持在0.1g/L~3g/L范围;
将纳米氧化锌和表面活性剂十二烷基苯磺酸钠磁力搅拌10min,超声震荡分散20min;其中,十二烷基苯磺酸钠浓度为0.01M;
称量、配制对甲苯磺酸钠电解质溶液,再次磁力搅拌10min,超声震荡分散20min;其中,对甲苯磺酸钠浓度为0.1M~0.3M;
加入吡咯单体依次搅拌、超声震荡分散5min形成最终电解液;其中,吡咯单体浓度为0.05M~0.3M。
9.如权利要求3所述的方法,其特征是,采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;具体步骤包括:
在碱性缓冲液环境中,采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;
或者,
采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;具体步骤包括:
配制Tris-HCl缓冲溶液,采用盐酸调至pH=8.5,称量多巴胺,加入设定量的Tris-HCl缓冲溶液,使多巴胺浓度为2g/L;放入试样,使其在室温条件下静置24h。
10.如权利要求3所述的方法,其特征是,采用氧化自聚方式,在植入电极本体的聚吡咯导电层表面沉积聚多巴胺纳米生物活性层;步骤之后,还包括:
涂层后处理:取出试样,分别用无水乙醇、去离子水超声清洗15min,放入真空干燥箱65℃保温12h,后随着干燥箱自然冷却至室温。
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