CN1445540A - 电化学电池 - Google Patents

电化学电池 Download PDF

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CN1445540A
CN1445540A CN03103571A CN03103571A CN1445540A CN 1445540 A CN1445540 A CN 1445540A CN 03103571 A CN03103571 A CN 03103571A CN 03103571 A CN03103571 A CN 03103571A CN 1445540 A CN1445540 A CN 1445540A
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阿拉思泰·麦金德·霍杰斯
托马斯·威廉姆·伯克
奥德瓦·约翰森
伊恩·安德鲁·马克思沃尔
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Abstract

一种制造薄层电化学电池(图12、14)的方法，包括如下步骤：形成一个穿过一阻电材料薄板(1)的孔(11)，所述孔限定电池的侧壁；在所述薄板的一侧设置一第一薄电极层(13)，在孔隙(11)上方延伸，从而限定电池的第一端壁；在所述薄板的另一侧设置一第二薄电极层(13)，在孔隙(11)上方延伸，从而限定电池的第二端壁，该第二端壁与第一电极基本重叠对准；以及提供使液体进入所述电池中的装置(16)。

Description

电化学电池
本申请是申请日为1996年11月15日的中国专利申请96199077.5的分案申请。
发明领域
本发明涉及一种用于测定载体中分析物浓度的电化学电池。
背景技术
此处描述的发明是对我们共同未决的申请PCT/AU96/00365中所述的发明的改进或修改，其内容在此引入以供参考。
此处将特别结合一种用以测量血液中葡萄糖浓度的生物传感器对本发明进行描述，但是应当理解本发明并不限于这种特定应用，也可以用于其它分析测量中。
为测量含水液体样品中的待分析成分的浓度，公知方法是通过将样品置于电化学电池的反应区进行测量，其中电化学电池具有两个电极，其间具有使它们适于电流测量的阻抗。允许待分析成分直接或间接与氧化还原剂反应，从而形成一种可氧化的(或可还原的)物质，其总量与待分析成分的浓度相对应。然后通过电化学方法测量存在的可氧化(或可还原的)物质的分量。这种方法通常需要使电极充分分离，以使测量期间一个电极的电解产物不会到达另一电极而影响另一电极的反应过程。
在我们共同未决的申请中，我们描述了一种用于测定在具有一个工作电极和一个与该工作电极隔开一定距离的反电极(或反/参考电极)的电化学电池中还原(或氧化)形态的氧化还原物质的浓度的新方法。该方法包括如下步骤，在电极之间施加电位差，选择工作电极的电位使得还原形态的物质的电解氧化(或氧化形态物质的电解还原)速率受扩散控制。工作电极与反电极之间的间距选择为使得反应产物从反电极到达工作电极。通过在施加电压之后并且在达到稳态电流之前测定作为时间函数的电流，然后估算稳态电流的强度，前述方法使得能够测定还原(或氧化)形态物质的扩散系数和/或浓度。
在我们共同未决的申请中，结合使用了采用GOD/氰亚铁酸盐系统的“薄层电化学电池”对该方法进行了举例说明。这里所用的术语“薄层电化学电池”是指具有小间距的电极从而使反应产物可由反电极到达工作电极的电池。实际上，用于测量血液中葡萄糖浓度的这种电池中电极的间隔小于500微米，并且最好小于200微米。
例示的电化学电池中所用的化学过程如下：
                              反应1
                      反应2
其中GOD为葡萄糖氧化酶，GOD*为‘活化’酶。氰铁酸盐([Fe(CN)6]3)为使GOD*返回其催化状态的‘介体’。反应过程中只要存在过量介体，催化酶GOD就不会消耗。氰亚铁酸盐([Fe(CN)6]4)为整个反应的产物。理论上开始时没有氰亚铁酸盐，但实际中常有少量。在反应完成后，氰亚铁酸盐的浓度(以电化学方法测量)表示葡萄糖的初始浓度。整个反应过程是反应1和2之和： 反应3
“葡萄糖”具体指β-D-葡萄糖。
已有技术具有诸多缺点。首先，所需样品尺寸大于所希望尺寸。通常希望能对较小体积的样品进行测量，因为这反过来使得能够在获取样品时采用较少侵入的方法。
其次，通常希望提高测量精度并且消除或减少由于例如电池不对称或者在批量生产微电池时引入的其它因素所导致的偏差。而且，也希望能够降低电极的“边缘”效应。
再者，由于该电池是一次性使用的，所以希望能够以较低成本大量生产。
发明概述
根据一个方面，本发明包括一种制造电化学电池的方法，其包括如下步骤：形成一个穿过一阻电材料薄板的孔，所述孔限定该电池的侧壁；在上述薄板的一侧设置一第一薄电极层，在所述孔的上方延伸，从而限定电池的第一端壁；在上述薄板的另一侧设置一第二薄电极层，在所述孔的上方延伸，从而限定电池的第二端壁，其与第一电极基本重叠对准；以及提供使液体进入所述侧壁和所述端壁之间限定的电池中的装置。
第一和第二电极层可以是导体或半导体，并且可以是相同的或不同的。优选贵金属电极层。
在本发明最佳实施例中，所述孔具有圆形截面，从而其侧壁是圆柱状的，而且第一和第二电极覆盖所述孔。
根据本发明的一种生物传感器，用于确定水成液样品中成分的浓度，该生物传感器包括：(a)电化学电池，该电化学电池包括第一阻电衬底，它具有在第一面上的第一导电材料的第一薄层，第二阻电衬底，它具有在第二面上的第二导电材料的第二薄层，这些衬底布置成第一导电材料面对第二导电材料并被包括一个孔的板分开，该孔的壁与导电材料相配合以确定一个电池壁，并且其中该孔在电池中限定了一个工作电极，该电池还包括样品引入口，由此该水成液样品可被引入电池中；以及(b)测量电路。
根据本发明的另一种生物传感器，用于确定水成液样品中成分的浓度，该生物传感器包括：(a)薄层电化学电池，该电化学电池包括：(i)阻电薄板，它包括一个孔，其中该孔在电池中限定了一个工作电极；(ii)第一电极层，覆盖该薄板的第一侧上的孔；(iii)第二电极层，覆盖该薄板的第二侧上的孔；和(iv)通道，用于允许该水成液样品进入该孔；以及(b)测量电路。
根据本发明的一种用于确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置，该装置包括：(a)中空的电化学电池，具有一个工作电极和一个反电极或反/参考电极，其中工作电极与反电极或反/参考电极相隔小于500μm；(b)用于在电极之间施加电势差的装置；和(c)用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置。
根据本发明的一种用于确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的方法，该方法包括：(a)提供中空的电化学电池，该电化学电池具有一个工作电极和一个反电极或反/参考电极，其中工作电极与反电极或反/参考电极相隔小于500μm；(b)在电极之间施加电势差；和(c)以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度。
最佳实施例的描述
下面仅以示例方式并且参照附图对本发明进行更详细的说明，附图中：
图1表示制造步骤2制造的产品的平面图。
图2表示图1中产品的侧视图。
图3表示图1中产品的端面图。
图4表示制造步骤3制造的产品的平面图。
图5表示图4中产品沿直线5-5的剖视图。
图6表示制造步骤5制造的产品的平面图。
图7表示图6中产品的侧视图。
图8表示图6中产品的端面图。
图9表示制造步骤7制造的产品的平面图。
图10为沿图9中直线10-10的剖视图。
图11表示图9中产品的端面图。
图12表示根据本发明的电池的平面图。
图13表示图12中电池的侧视图。
图14表示图12中电池的端面图。
图15表示本发明第二实施例的一小部分的放大剖面图。
下面以改进的制造方法作为示例说明薄层电化学电池的构造。
步骤1：将一大约13cm×13cm且100微米厚的Melinex_(化学惰性的阻电的聚对苯二甲酸乙二醇酯[“PET”])薄板1平放在一张脱模纸2上，并且使用2号MYAR棒以水基热活性粘合剂3(采用催化剂：粘合剂的ICI Novacoat系统)对其进行涂覆，使之潮湿厚度12微米(干燥后大约2-5微米)。然后通过热空气干燥器将水蒸发，产生一个压合式粘合剂表面。随后在一脱模纸上将所述薄板翻转，其反面也类似地涂以相同粘合剂4，进行干燥，并且向其裸露的粘合剂表面施加一层保护性脱模纸5。修剪其边缘以获得一张薄板，其两面都均匀涂覆有未干的压合式粘合剂，并以脱模纸加以保护。
步骤2：将此带有保护性脱模纸的薄板切成板条7，每个大约18mm×210mm(图1-3)。
步骤3：将由步骤2得到的相应两侧带有脱模纸2、5的涂有粘合剂的PET板条7置于一冲模组件(未画出)中加以压合。该冲模组件用于在板条上每一端打出定位孔10，并且在沿定位孔10之间的直线上打出例如37个直径均为3.4mm的圆孔11，其中心间距相等，都为5mm。每个孔11的面积约为9平方毫米。
步骤4：将一张大约21cm见方且135微米厚的Mylar_PET薄板置于溅镀室中以便镀覆钯镀层13。溅镀在4至6毫巴的真空和氩气氛中进行。在PET上镀覆厚100-1000埃的钯。从而制得具有钯溅射镀层13的薄板14。
步骤5：然后将从步骤4制成的钯溅射镀覆薄板14切成板条14及15，并在每一板条上利用冲模打两个定位孔16在每一端(图6，7和8)。板条14和15的区别仅在于板条14尺寸为25mm×210mm，板条15为23mm×210mm。
步骤6：接着将在步骤3制得的间隔板条7置于一夹具(未画出)中，该夹具具有两个定位销(各对应于板条7的定位孔10)，并且去掉上层脱模纸2。接着将步骤5制得的镀钯PET板条14置于粘合剂层之上，其钯表面朝下，利用夹具的定位销使定位孔16与其下的PET板条7对准。随后使该组合物通过一个层合机，该层合机具有一组压轮，其中之一用于对带有镀钯PET板条14的一侧进行加热。使板条7相反一侧的压轮冷却。以此方式，仅激活了钯板条14和PET板条7之间的粘合剂。
步骤7：接着将PET板条7翻转，将其置于夹具中，使其脱模涂层在最上面。揭去其脱模涂层，并使第二镀钯板条15镀钯侧朝下置于裸露的粘合剂表面上，利用定位销对准板条，该组件现在再次通过步骤6中的层合机，这一次使加热辊接触在步骤7中加入的镀钯Mylar_，以便激活中间粘合剂(图9、10和11)。
步骤8：由步骤7制得的组件返回至冲模组件，并且定位打穿凹口17，以使其延伸于前面在Melinex_PET上打出的圆孔11和板条边缘17之间。凹口16延伸使得其贯穿每个圆形腔室的圆周。然后将该板条截断，产生37个单个的“传感器条”，每条大约5mm宽，各具有一个薄层腔电池(图12、13和14)。
因而制得了一个电池，如图12、13和14所示。该电池包括：一个由PET层12构成的第一电极，一钯镀层13，一粘合剂层3，一PET板1，一第二粘合剂层4，一个由钯镀层13构成的第二电极，和一PET层12。板1限定一个柱状腔室11，其在电池纵向的厚度对应于Melinex_PET板层1的厚度加上粘合剂层3和4的厚度。此电池具有圆形钯端壁。在电池侧边的凹口16与腔室11相交处，提供有电池的入口。
在本发明最佳实施例中，待分析样品通过毛细作用引入电池中。使样品置于与凹口16接触，通过毛细作用自发吸入电池中，电池中被取代的空气由相反凹口16排出。在毛细缝隙可以加入表面活性剂以助于吸入样品。
对这些传感器配以连接装置，例如印刷板插头座，从而将传感器加入测量电路中。在一最佳实施例中，通过使间隔板1短于钯支承板14、15，并且使一张板15的长度短于另一张板14，可以实现此目的。这就形成了一个插座区域20，其接触表面21、22分别与工作电极和反电极电连接。因而可以采用具有相应啮合导电表面的简单舌形插头用于电连接。也可以采用其它形式的连接器。
电池中采用的化学品可以由电池的电极或壁支承，可以由电池中含有的独立支承物支承，或者可以是自支承的。
在一个实施例中，电池中采用的化学品在步骤1之后立刻印刷至电极的钯表面上，在步骤1中，刚沉积的钯更加亲水。例如，可以将含有0.2摩尔氰铁酸钾和1％重量的葡萄糖氧化酶脱氢酶的溶液印刷至钯表面上。所希望的是，将化学品仅印刷在将要形成电池壁的区域，最好通过喷墨打印机将化学品印在表面上。以此方式，可以精确控制化学品的沉积量。如果需要，希望隔离直到需要使用时的化学品可以分别印刷至第一和第二电极上。例如，可以将GOD/氰亚铁酸盐混合物印刷至一个电极上和另一电极的缓冲区上。尽管在组件置于电池中之前将化学品施加至电极上是很理想的，但是也可以在步骤6或步骤8之后用传统方法以吸液管将化学品注入电池中，随后通过蒸发或干燥将溶剂去除。化学品不是必须要印刷至电池壁或电极上，也可以浸渍在电池中含有的或填充的纱布、薄膜、无纺布等之中(例如在步骤6或7之前置入腔室11中)。在另一实施例中，化学品制成多孔物质，作为小球丸或小颗粒加入电池中。或者，化学品可以作为凝胶加入。
在本发明第二实施例中，首先由步骤5中获得的板条14制得一层压件21，粘合在步骤3中获得的两个板条7之间。层压件20替代步骤5中的薄板1，并且在步骤6和7中与电极组装在一起。
从而制得一个电池，如图15所示，它与图9至11中的电池区别之处在于，该电池具有一环形电极，位于第一和第二电极之间。该电极例如可以用作参考电极。
应当理解，在批量生产该电池时，其部件可以组装为连续线的层压件。例如，可以首先对一张连续的PET薄板1冲孔，然后通过印刷向保留薄板连续施加粘合剂。可以直接将电极(以化学溶液预印刷并干燥)作为层压件施加于涂有粘合剂的一侧。然后将粘合剂施加于冲孔芯板的另一侧，随后将电极作为层压件施加于第二侧。
粘合剂可以作为热熔交替膜施加。或者，芯板可以首先涂覆粘合剂，然后冲孔。
通过在胶合步骤之前使各电极上的化学品干燥，可以防止电极表面沾污。
尽管结合Mylar_和Melinex_PET描述了此电池，但是也可以采用其它化学惰性的阻电材料，并且可以选择其它尺寸。用作间隔薄板1的材料以及用于支承参考电极和反电极的材料可以是相同的，也可以彼此不同。尽管本发明是参照钯电极说明的，但是也可以采用其它金属，如铂、银、金、铜等，并且银可以与氯化物反应以形成一个银/氯化银电极，或者与其它卤化物反应。电极不必是相同金属制成的。
尽管描述了热活性粘合剂的使用，但是其部件也可以利用热熔粘合剂、易熔层压件和其它方法加以组装。
传感器尺寸可以根据需要方便地加以改变。
虽然电极覆盖电池的端部开口是极为理想的，但在其它实施例中(未详述)，其电极没有全部覆盖电池的端部开口。在此情况下，需要电极基本重叠对准。
电极覆盖腔室11孔的本发明优选形式，具有电极面积仅由冲孔11精确限定的优点。另外，如此设置的电极相互平行、重叠，具有基本相同的面积，并且基本或全部没有“边缘”效应。
尽管所述实施例中各传感器具有一个电池腔，但是传感器可以设有两个或更多的腔。例如，可以设置一个具有既定量分析物的第二腔，可用作参考电池。
本领域技术人员由本文所含教导会很清楚，此处所述一个实施例的特征可以与此处所述其它实施例的特征或者与我们共同未决的申请中所述的其它实施例进行结合。尽管此传感器是参照钯电极和GOD/氰亚铁酸盐化学品加以说明的，但是本领域技术人员清楚，可以采用其它的化学品以及其它材料的结构，而不偏离此处所述的原理。

Claims (32)

1.一种生物传感器，用于确定水成液样品中成分的浓度，该生物传感器包括：
(a)电化学电池，该电化学电池包括第一阻电衬底，它具有在第一面上的第一导电材料的第一薄层，第二阻电衬底，它具有在第二面上的第二导电材料的第二薄层，这些衬底布置成第一导电材料面对第二导电材料并被包括一个孔的板分开，该孔的壁与导电材料相配合以确定一个电池壁，并且其中该孔在电池中限定了一个工作电极，该电池还包括样品引入口，由此该水成液样品可被引入电池中；以及
(b)测量电路。
2.根据权利要求1的生物传感器，其中电化学电池还包括一个插座区域，该插座区域具有与第一导电材料的第一薄层电连通的第一接触区，和与第二导电材料的第二薄层电连通的第二接触区，由此，该电化学电池可以与测量电路电连接。
3.根据权利要求1的生物传感器，其中测量电路包括舌形插头。
4.根据权利要求1的生物传感器，其中第一导电材料和第二导电材料至少之一包括金属。
5.根据权利要求4的生物传感器，其中金属包括溅涂的金属。
6.根据权利要求1的生物传感器，其中水成液样品包括血液。
7.根据权利要求1的生物传感器，其中所述成分包括葡萄糖。
8.根据权利要求1的生物传感器，其中测量电路包括自动仪器，用于检测来自电化学电池的电信号，并将该电信号与水成液样品中成分的浓度相关联。
9.根据权利要求1的生物传感器，其中电化学电池包括具有一个厚度的基本上平坦的板条，该板条至少具有两个横向边缘，其中样品引入口包括在横向边缘至少之一中的通过该板条的整个厚度的凹口。
10.一种生物传感器，用于确定水成液样品中成分的浓度，该生物传感器包括：
(a)薄层电化学电池，该电化学电池包括：
(i)阻电薄板，它包括一个孔，其中该孔在电池中限定了一个工作电极；
(ii)第一电极层，覆盖该薄板的第一侧上的孔；
(iii)第二电极层，覆盖该薄板的第二侧上的孔；和
(iv)通道，用于允许该水成液样品进入该孔；和
(b)测量电路。
11.根据权利要求10的生物传感器，其中电化学电池还包括一个插座区域，该插座区域具有与第一电极层电连通的第一接触区，和与第二电极层电连通的第二接触区，由此，该电化学电池可以与测量电路电连接。
12.根据权利要求10的生物传感器，其中测量电路包括舌形插头。
13.根据权利要求10的生物传感器，其中水成液样品包括血液。
14.根据权利要求10的生物传感器，其中所述成分包括葡萄糖。
15.根据权利要求10的生物传感器，其中测量电路包括自动仪器，用于检测来自电化学电池的电信号，并将该电信号与水成液样品中成分的浓度相关联。
16.根据权利要求10的生物传感器，其中电化学电池包括具有一个厚度的基本上平坦的板条，该板条至少具有两个横向边缘，其中用于允许进入该孔的通道包括在横向边缘至少之一中的通过该板条的整个厚度的凹口。
17.一种用于确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置，该装置包括：
(a)中空的电化学电池，具有一个工作电极和一个反电极或反/参考电极，其中工作电极与反电极或反/参考电极相隔小于500μm；
(b)用于在电极之间施加电势差的装置；和
(c)用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置。
18.根据权利要求17的装置，其中用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置包括：
(i)用于确定在施加电势差之后和取得稳定状态电流之前电流随时间的变化的装置；
(ii)用于估算稳定状态电流的幅度的装置；和
(iii)用于从电流随时间的变化和稳定状态电流的幅度获得指示氧化还原物质的还原形式或氧化形式的浓度的装置。
19.根据权利要求17的装置，其中该电池还包括一个插座区域，该插座区域具有与工作电极电连通的第一接触区，和与反电极或反/参考电极电连通的第二接触区，由此，该电池可以与用于在电极之间施加电势差的装置和用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置中的至少一个电连接。
20.根据权利要求17的装置，其中用于在电极之间施加电势差的装置和用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置中的至少一个包括舌形插头。
21.根据权利要求17的装置，其中用于在电极之间施加电势差的装置和用于以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的装置中的至少一个包括自动仪器，用于检测来自电化学电池的电信号，并将该电信号与水成液样品中氧化还原物质的还原形式或氧化形式的浓度相关联。
22.根据权利要求17的装置，其中该电池包括具有一个厚度的基本上平坦的板条，该板条至少具有两个横向边缘，其中一个凹口延伸通过电化学电池的壁，并且在横向边缘至少之一中通过该板条的整个厚度，由此，该液体样品可被引入电池。
23.根据权利要求17的装置，其中液体样品包括血液。
24.根据权利要求17的装置，其中氧化还原物质包括葡萄糖。
25.一种用于确定液体样品中氧化还原物质的还原形式或氧化形式的浓度的方法，该方法包括：
(a)提供中空的电化学电池，该电化学电池具有一个工作电极和一个反电极或反/参考电极，其中工作电极与反电极或反/参考电极相隔小于500μm；
(b)在电极之间施加电势差；和
(c)以电化学方式确定液体样品中氧化还原物质的还原形式或氧化形式的浓度。
26.根据权利要求25的方法，其中步骤(c)包括：
(i)确定在施加电势差之后和取得稳定状态电流之前电流随时间的变化；
(ii)估算稳定状态电流的幅度；和
(iii)从电流随时间的变化和稳定状态电流的幅度获得指示氧化还原物质的还原形式或氧化形式的浓度。
27.根据权利要求25的方法，其中该电池还包括一个插座区域，该插座区域具有与工作电极电连通的第一接触区，和与反电极或反/参考电极电连通的第二接触区。
28.根据权利要求25的方法，其中步骤(b)还包括步骤：
(i)提供自动仪器，用于在电极之间施加电势差。
29.根据权利要求25的方法，其中步骤(c)还包括步骤：
(i)提供自动仪器，用于检测来自电化学电池的电信号；和
(ii)将该电信号与液体样品中氧化还原物质的还原形式或氧化形式的浓度相关联。
30.根据权利要求25的方法，其中该电池包括具有一个厚度的基本上平坦的板条，该板条至少具有两个横向边缘，其中一个凹口延伸通过电化学电池的壁，并且在横向边缘至少之一中通过该板条的整个厚度，由此，该液体样品可被引入电池。
31.根据权利要求25的方法，其中液体样品包括血液。
32.根据权利要求25的方法，其中氧化还原物质包括葡萄糖。
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CN103954668B (zh) * 2004-05-21 2016-11-23 埃葛梅崔克斯股份有限公司 电化学电池和生产电化学电池的方法

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