CN115128140A - 一种针状同轴多电极装置及其构建方法 - Google Patents
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Abstract
本发明公开了一种针状同轴多电极装置及其构建方法,包括针状导电体,所述针状导电体经过多次旋转溅射和化学处理,其表面依次镀有第一绝缘层、铂电极层、第二绝缘层、银/氯化银电极层;所述第一绝缘层、第二绝缘层采用二氧化硅或三氧化二铝绝缘层。本发明有效解决多根电极对生物体组织的损伤和生物体不同位置生物化学环境不同带来的干扰问题,且低成本、易于操作、高度集成化。
Description
技术领域
本发明涉及电化学测试领域,具体涉及一种针状同轴多电极装置及其构建方法。
背景技术
作为电化学测试最常用的测试体系,三电极体系通常包括工作电极,对电极和参比电极。所谓的三电极体系,是为了排除电极电势因极化电流而产生的较大误差而设计的;它在普通的两电极体系(工作电极与对电极)的基础上引入了用以稳定工作电极的参比电极。
尽管三电极测试体系在溶液电化学中被广泛应用,但是对于生物活体组织或病变组织的小范围分析仍然面临挑战。首先,多根电极分析势必需要对活体组织导入三根不同电极,对组织伤害较大;与此同时,三根电极插入组织的位置对分析结果影响较大,难以保证三根电极在完全一样的生物体环境中。因此,开发一种低成本、易于操作、高度集成化的单根三电极体系是非常迫切的。
发明内容
发明目的:本发明的第一目的在于提供一种针状同轴多电极装置,该装置低成本、易于操作、高度集成化,有效解决多根电极对生物体组织的损伤和生物体不同位置生物化学环境不同带来的干扰问题;本发明的第二目的在于提供一种针状同轴多电极装置的构建方法,该方法工艺简单、可重复性强,适用于生物组织的微创、原位电化学分析。
技术方案:本发明的针状同轴多电极装置,包括针状导电体,所述针状导电体经过多次旋转溅射和化学处理,其表面依次镀有第一绝缘层,铂电极层,第二绝缘层,银/氯化银电极层;所述第一绝缘层、第二绝缘层采用二氧化硅或三氧化二铝绝缘层。
所述针状导电体采用不锈钢针、银针、金针、激光拉制的石英毛细管中的一种。
所述第二绝缘层和银/氯化银电极层之间设置金电极层和第三绝缘层;所述第三绝缘层采用二氧化硅或三氧化二铝绝缘层。此时可以形成铂-金-银/氯化银三电极体系或不锈钢-金-银--银/氯化银三电极体系或更多的组合方式,可以适应更多不同的电化学检测手段和方法。
所述绝缘层、铂电极层、绝缘层、银/氯化银电极层的厚度为50-300nm,层厚尤其是绝缘层厚度低于50nm时,容易在外加测试电压的方法下被击穿,导致短路。层厚超过300nm时,则整体电极过粗,容易对生物组织产生过大伤害。
所述针状导电体的长度为2~6cm,长度低于2cm时,引出电极设计空间较小,工艺精度要求太高,长度超过6cm时则容易超过溅射仪器均匀溅射的范围,容易导致中间厚,两端薄的结果。
本发明还包括一种针状同轴多电极装置的构建方法,包括以下步骤:
S1、在磁控溅射仪中安装水平旋转的电机;
S2:将针状导电体两端用保护套罩住,水平安装至电机上;
S3:开启电机使针状导电体在水平方向连续旋转,抽真空,溅射具有厚度的硅或金属铝,形成硅层或铝层;对溅射完成的针状导电体进行加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S4:将步骤S3中镀上绝缘层的针状导电体两端用保护套罩住,两端各向内移动,水平安装到至电机上;开启电机使针状导电体在水平方向连续旋转,抽真空,溅射具有厚度的铂,形成铂电极层;
S5:将步骤S4中镀上铂电极层的针状导电体两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体在水平方向连续旋转,抽真空,溅射具有厚度的硅或金属铝,形成硅层或铝层,对溅射完成的电极加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S6:将步骤S5中镀上绝缘层的针状导电体两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体在水平方向连续旋转,抽真空,溅射具有厚度的金属银,将针状导电体在次氯酸钠溶液中静置用超纯水清洗,烘干得到银/氯化银电极层。
有益效果:本发明的技术方案与现有技术相比,其有益效果在于:(1)该装置低成本、易于操作、高度集成化,有效解决多根电极对生物体组织的损伤和生物体不同位置生物化学环境不同带来的干扰问题;(2)该方法利用溅射仪,通过连续旋转,在针状导电体表面均匀地溅射镀膜,工艺简单、可程序化、可重复性强,适用于各种材质的针表面镀多层膜。
附图说明
图1为本发明所述针状同轴多电极装置的结构示意图;
图2为本发明所述同轴多电极装置的剖视图;
图3为本发明中安装了旋转马达的磁控溅射仪示意图;
图4为将针状导电体安装于磁控溅射仪时的安装示意图;
图5为本发明实施例5中所述针状同轴多电极装置的结构示意图;
图6为截面扫描电子显微镜图像,单层厚度测量值为99.82nm。
具体实施方式
下面结合具体实施方式和说明书附图对本发明的技术方案进行详细描述。
如图1至4所示,本发明的针状同轴多电极装置包括针状导电体1,所述针状导电体1表面依次镀有第一绝缘层2,铂电极层3,第二绝缘层4、银/氯化银电极层5;针状导电体1采用不锈钢针、银针、金针、激光拉制的石英毛细管中的一种。针状导电体1的长度为2~6cm,本实施中,直径为8mm,长度为5cm。如图6所示,第一绝缘层2、铂电极层3、第二绝缘层4、银/氯化银电极层5的厚度为50-300nm。第一绝缘层2、第二绝缘层4采用二氧化硅或三氧化二铝绝缘层。
使用时,将针状同轴多电极装置插入待分析的生物组织或感兴趣区域,利用导线从尾部连接到电化学工作站即可对生物组织进行电化学分析。
本发明还包括一种针状同轴多电极装置的构建方法,包括以下步骤:
S1:如图3所示,在磁控溅射仪中按照水平旋转的电机;
S2:如图4所示,将针状导电体两端用保护套罩住,水平安装到步骤S1的电机上;
S3:开启电机使针状导电体在水平方向连续旋转,抽真空,溅射100nm厚度的硅或金属铝,形成硅层或铝层,将溅射完成的针状导电体在马弗炉中加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S4:将步骤S3中镀上绝缘层的针状导电体两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体在水平方向连续旋转,抽真空,溅射100nm厚度的铂,形成铂电极层;
S5:将步骤S4中镀上铂电极层的不锈钢针两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使钢针在水平方向连续旋转,抽真空,溅射100nm厚度的硅或金属铝,形成硅层或铝层,将溅射完成的电极在马弗炉中加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S6:将步骤S5中镀上铂电极层的不锈钢针两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体在水平方向连续旋转,抽真空,溅射100nm厚度的金属银,将针状导电体在次氯酸钠溶液中静置,然后用超纯水清洗,烘干得到银/氯化银层。
下面结合实施例对以上方案详细介绍。
实施例1不锈钢-铂-银/氯化银同轴三电极的制备。
在不锈钢针两端套上保护套,放入溅射仪旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射100nm厚度的铂,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的银,并氯化成银/氯化银层,单层截面厚度测量如图6所示。
实施例2:毛细管基底上金-铂-银/氯化银同轴三电极的制备
在激光拉制备的毛细管两端套上保护套,放入溅射仪旋转溅射厚度为100nm的金,保护套两端向内推进,旋转溅射100nm厚度的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的铂,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的银,并氯化成银/氯化银层。
实施例3:银/氯化银-铂-金同轴三电极的制备
在银针两端套上保护套,放入溅射仪旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的铂,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的金,最后将暴露的银针针尖氯化成银/氯化银电极。
实施例4:金-铂-银/氯化银同轴三电极的制备
在金针两端套上保护套,放入溅射仪旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的铂,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的银,并氯化成银/氯化银电极。
实施例5:不锈钢-铂-金-银/氯化银同轴四电极的制备
如图5所示,在不锈钢针两端套上保护套,放入溅射仪旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射100nm厚度的铂,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,保护套两端向内推进,旋转溅射厚度为100nm的金,形成金电极层7,保护套两端向内推进,旋转溅射厚度为100nm的硅或金属铝,并氧化成二氧化硅或三氧化二铝绝缘层绝缘层,该绝缘层为第三绝缘层6,保护套两端向内推进,旋转溅射厚度为100nm的银,并氯化成银/氯化银层。
Claims (6)
1.一种针状同轴多电极装置,其特征在于:包括针状导电体(1),所述针状导电体(1)经过多次旋转溅射和化学处理,其表面依次镀有第一绝缘层(2)、铂电极层(3)、第二绝缘层(4)、银/氯化银电极层(5);所述第一绝缘层(2)、第二绝缘层(4)采用二氧化硅或三氧化二铝绝缘层。
2.根据权利要求1所述的针状同轴多电极装置,其特征在于:所述针状导电体(1)采用不锈钢针、银针、金针、激光拉制的石英毛细管中的一种。
3.根据权利要求1所述的针状同轴多电极装置,其特征在于:所述第二绝缘层(4)和银/氯化银电极层(5)之间设置金电极层(7)和第三绝缘层(6);所述第三绝缘层(6)采用二氧化硅或三氧化二铝绝缘层。
4.根据权利要求1所述的针状同轴多电极装置,其特征在于:所述第一绝缘层(2)、铂电极层(3)、第二绝缘层(4)、银/氯化银电极层(5)的厚度为50-300nm。
5.根据权利要求1所述的针状同轴多电极装置,其特征在于:所述针状导电体(1)的长度为2~6cm。
6.一种关于权利要求1所述针状同轴多电极装置的构建方法,其特征在于,包括以下步骤:
S1:在磁控溅射仪中安装水平旋转的电机;
S2:将针状导电体(1)两端用保护套罩住,水平安装至电机上;
S3:开启电机使针状导电体(1)在水平方向连续旋转,抽真空,溅射具有厚度的硅或金属铝,形成硅层或铝层;对溅射完成的针状导电体(1)进行加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S4:将步骤S3中镀上绝缘层的针状导电体(1)两端用保护套罩住,两端各向内移动,水平安装到至电机上;开启电机使针状导电体(1)在水平方向连续旋转,抽真空,溅射具有厚度的铂,形成铂电极层(3);
S5:将步骤S4中镀上铂电极层的针状导电体(1)两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体(1)在水平方向连续旋转,抽真空,溅射具有厚度的硅或金属铝,形成硅层或铝层,对溅射完成的电极加热氧化处理,形成二氧化硅或三氧化二铝绝缘层;
S6:将步骤S5中镀上绝缘层的针状导电体(1)两端用保护套罩住,两端各向内移动,水平安装到电机上;开启电机使针状导电体(1)在水平方向连续旋转,抽真空,溅射具有厚度的金属银,将针状导电体(1)在次氯酸钠溶液中静置用超纯水清洗,烘干得到银/氯化银电极层(5)。
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