CN1288436C - Preparation method of reference electrode compatible with micro electromechanical system technology - Google Patents

Preparation method of reference electrode compatible with micro electromechanical system technology Download PDF

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CN1288436C
CN1288436C CN 02160271 CN02160271A CN1288436C CN 1288436 C CN1288436 C CN 1288436C CN 02160271 CN02160271 CN 02160271 CN 02160271 A CN02160271 A CN 02160271A CN 1288436 C CN1288436 C CN 1288436C
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electrode
preparation
micro
mems
technology
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CN1514234A (en
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李华清
蔡新霞
郭增军
崔大付
饶能高
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Institute of Electronics of CAS
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Institute of Electronics of CAS
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Abstract

The present invention relates to a preparation method for reference electrodes, which is compatible to the technology of micro-electromechanical systems (MEMS). Firstly, a designed territory is formed into a mask plate by a microelectronic technology, and a phokto etching method is used for forming a required micro-electrode or an electrode array for composing an electrochemical test system. The present invention uses noble metal aurum Au and platinum Pt as electrode materials, and the preparation method for reference electrodes, which is compatible to the technology of micro-electromechanical systems (MEMS) and application thereof can be realized by adopting the technology of micro-electromechanical systems to make a super-micro-thin membrane electrode array which is applied to biochemical sensors for an embodiment. The present invention has the advantages of convenient and simple technological processes, rapidness, good repeatability, easy realization of high-accuracy replication and scale production, and is especially suitable for manufacturing micro-system biological enzyme sensor arrays. The present invention is suitable for preparing reference electrodes of various electrochemical two-electrode devices, or three-electrode devices or array chips, and can be widely used in the fields of the research and the development of biochemical sensors, biological chips and micro-system integrated chips.

Description

Preparation method with the contrast electrode of MEMS (micro electro mechanical system) process compatible
Technical field
The present invention relates to electrochemical measuring technique, MEMS (micro electro mechanical system) (MEMS) process technology and sensing technology, particularly a kind of preparation method and application thereof of contrast electrode of and MEMS (micro electro mechanical system) (MEMS) process compatible.
Background technology
Various forms of electrochemical electrodes are used widely at aspects such as biochemical analysis, biochip, health quarantine, environmental monitoring, food inspection, industrial fermentation production monitorings.The contrast electrode of standard is in the electro-chemical test system, and its current potential does not change substantially.The most frequently used contrast electrode is the electrode system of saturated calomel electrode or silver and difficulty soluble salt silver chloride composition thereof.
Rely on the manufacturing technology and integrated circuit (IC) manufacturing technology of screen printing technique, MEMS (micro electro mechanical system) (MEMS) at present, electrode device directly can be integrated on the substrate.Adopt the electrode device of this method preparation to help producing in batches, and have that cost is low, volume is little, characteristics such as in light weight, stable performance.More and more MEMS (micro electro mechanical system) (MEMS) technologies that adopt of a lot of Electrochemical Detection devices; adopting the contrast electrode of MEMS (micro electro mechanical system) (MEMS) technology preparation at present all is solid-state Ag/AgCl electrode; its method is to adopt MEMS (micro electro mechanical system) (MEMS) technology earlier after preparing silver electrode on the substrate; utilize chemical method to make the argent chlorination on surface again; therefore; this contrast electrode can not be compatible fully with MEMS technology; certain limitation is particularly arranged when making microelectrode or ultramicroelectrode; as make consuming time, complex process, be unfavorable for large-scale production etc.Therefore, seeking a kind of contrast electrode compatible fully with MEMS (micro electro mechanical system) (MEMS) technology, is indispensable gordian technique in its research application and development.
Summary of the invention
Purpose of the present invention just provides a kind of preparation method of effective, easy contrast electrode, this method can be widely used in the preparation of the contrast electrode of film/thick film microelectrode and other electrochemical electrode and electrode array chip, and technologies such as this method and MEMS (micro electro mechanical system) (MEMS) and integrated circuit (IC) manufacturing technology are fully compatible and be applied in the actual Electrochemical Detection.
For achieving the above object, solution of the present invention provides a kind of preparation method of contrast electrode of and MEMS (micro electro mechanical system) process compatible, and this method may further comprise the steps:
At first the electrode system domain that designs is utilized microelectronic technique to make the mask plate, dry again the spin coating photoresist after substrate cleans and promptly can use mask board to explosure, development in cleaning fluid, passing through the identical noble metal electrode material of sputter on the substrate that develops then, the back cleaning of coming unstuck promptly can prepare needed working electrode and contrast electrode and form two electrodes or three-electrode electro Chemical device.
The preparation method of described contrast electrode, its described electrode patterns is galvanochemistry two electrodes shape of the same race, various sizes, three electrode devices or array chip.
The preparation method of described contrast electrode, its described two electrodes, three electrode electrode shape comprise circle, square, bar shaped.
The preparation method of described contrast electrode, its described working electrode and contrast electrode are film/thick film ultramicroelectrode.
The preparation method of described contrast electrode, its described electrochemical device, the thick film device or the array chip of also useful silk-screen printing technique preparation.
The preparation method of described contrast electrode, the experimental technique of its described contrast electrode, be applicable to two electrodes, three electrode devices and the array chip thereof that use inert electrode such as noble metal etc. to form as material, contrast electrode and working electrode are the various electrochemical methods of the detection architecture that membrane electrode constituted of same material.
Working electrode and contrast electrode with the present invention's preparation are formed two electrodes or three-electrode electro Chemical device, and this contrast electrode can be used for the undemanding detection architecture of electrode potential requirement, as are used for biology enzyme sensor ampere method detection substrate.
Description of drawings
Fig. 1 is to use the present invention to prepare the process flow diagram of electrode;
Fig. 2 is galvanochemistry contrast electrode of the present invention and electrode system synoptic diagram;
Fig. 3 is to use the cyclic voltammogram of multi-form contrast electrode of the present invention to compare;
Fig. 4 is to use the cyclic voltammogram of different materials contrast electrode of the present invention to compare.
Embodiment
Describe implementation of the present invention in detail in conjunction with example with reference to the accompanying drawings below.
As shown in Figure 1, the preparation method of the contrast electrode of of the present invention and MEMS (micro electro mechanical system) (MEMS) process compatible may further comprise the steps:
At first the electrode system domain that designs is utilized microelectronic technique to make mask plate 1, dry again the substrate 2 that the spin coating photoresist obtains having photoresist after substrate cleans and use mask board to explosure, development again in cleaning fluid.
Passing through the identical noble metal electrode material 4 of sputter on the substrate 3 after the development then, the back of coming unstuck is cleaned and promptly can be prepared needed working electrode and contrast electrode 5;
Simultaneously, as required working electrode and contrast electrode are formed two electrodes or three-electrode electro Chemical device.
Embodiment 1:
Fig. 2 represents the design of the electrochemical electrode system of the embodiment of the invention, mainly comprises with the lower part: reaction raceway groove 1, contrast electrode 2, working electrode 3, insulation course 4, contact conductor 5 compositions such as grade.Electrode is made and is adopted MEMS (micro electro mechanical system) (MEMS) technology, and wherein working electrode adopts identical Precious Metals-Gold or platinum to sputter on the glass matrix with contrast electrode.This device promptly can be used for three-electrode system or two electrode systems.Wherein the A sensor is that square-shaped electrode is that with the difference of B sensor reaction chamber is different among the figure, and B is circular reaction chamber.C is a disk electrode, and D is a strip electrode.
Embodiment 2:
Fig. 3, that Fig. 4 is to use respectively that the present invention carries out is multi-form, the comparison of the contrast electrode cyclic voltammogram of different materials, wherein dotted line representative is D sensor in Fig. 1, the solid line representative be C type sensor in Fig. 1, the dotted line representative be A type sensor in Fig. 1.Among the figure as can be seen, the detection system of three kinds of multi-form contrast electrode compositions can obtain typical cyclic voltammetry curve, the redox peak that symmetry occurs, and the ratio of negative electrode peak and anodic peak current is 1: 1, spike potential is not with the feature of reversible reaction systems such as sweep velocity change, the dotted line representative is the gold electrode material among Fig. 4, and what realize representative is the platinum electrode material.
The test fluid of the cyclic voltammogram among the embodiment 2 is 1mM potassium ferricyanate and 250mMKCl, and base is the 10mM phosphate buffer of pH7.4 mutually; Sweep velocity is 100mV/sec.

Claims (3)

1, with the preparation method of the contrast electrode of MEMS (micro electro mechanical system) process compatible, it is characterized in that this method may further comprise the steps:
At first the electrode system domain that designs is utilized microelectronic technique to make the mask plate, dry again the spin coating photoresist after substrate cleans and promptly can use mask board to explosure, development in cleaning fluid, passing through the identical noble metal electrode material of sputter on the substrate that develops then, the back cleaning of coming unstuck promptly can prepare needed working electrode and contrast electrode and form two electrodes or three-electrode electro Chemical device; Described electrode patterns is galvanochemistry two electrodes shape of the same race, various sizes, three electrode devices or array chip; Described two electrodes, three electrode electrode shape comprise circle, square, bar shaped.
2, the preparation method of contrast electrode as claimed in claim 1 is characterized in that, described working electrode and contrast electrode are film/thick film ultramicroelectrode.
3, the preparation method of contrast electrode as claimed in claim 1 is characterized in that, described electrochemical device, the thick film device or the array chip of also useful silk-screen printing technique preparation.
CN 02160271 2002-12-31 2002-12-31 Preparation method of reference electrode compatible with micro electromechanical system technology Expired - Lifetime CN1288436C (en)

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Application Number Priority Date Filing Date Title
CN 02160271 CN1288436C (en) 2002-12-31 2002-12-31 Preparation method of reference electrode compatible with micro electromechanical system technology

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CN1288436C true CN1288436C (en) 2006-12-06

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Publication number Priority date Publication date Assignee Title
DE102007026243A1 (en) * 2007-06-04 2008-12-11 Endress + Hauser Gmbh + Co. Kg Capacitive pressure sensor
CN102249181A (en) * 2011-03-28 2011-11-23 大连理工大学 Manufacturing method of SU-8 photoresist micro-force sensor
CN102320559B (en) * 2011-09-14 2014-06-18 上海交通大学 Preparation method of hollow-structured micro-array electrode
CN103031246B (en) * 2011-10-10 2014-11-05 中国科学院电子学研究所 Microelectrode array chip for multi-parameter detection of nerve cells and preparation method thereof
CN103043597B (en) * 2011-10-13 2015-05-20 聊城大学 Method for preparing metal micro-nano array electrode by using ZnO crystal as template
CN103956320B (en) * 2014-04-16 2016-08-31 苏州大学 Method for transferring electrode pattern on arbitrary substrate and constructing electronic device
CN105628757A (en) * 2015-12-30 2016-06-01 中国科学院电子学研究所 ORP sensing chip based on MEMS and manufacturing method of ORP sensing chip
CN105891192A (en) * 2016-06-24 2016-08-24 大连理工大学 Electrochemical and electrochemical luminescence detection method based on integrated three-electrode system microchip
CN106769833A (en) * 2017-01-03 2017-05-31 北京科技大学 For the device and method of the high-flux electric chemical characterization of combined material chip

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