CN100395545C - Method for preparing integrated multiple ultramicro microdisc electrode - Google Patents
Method for preparing integrated multiple ultramicro microdisc electrode Download PDFInfo
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- CN100395545C CN100395545C CNB2006100189714A CN200610018971A CN100395545C CN 100395545 C CN100395545 C CN 100395545C CN B2006100189714 A CNB2006100189714 A CN B2006100189714A CN 200610018971 A CN200610018971 A CN 200610018971A CN 100395545 C CN100395545 C CN 100395545C
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Abstract
The present invention relates to a method for preparing an integrated multiple ultra micro-micro disc electrode. A plurality of electrode fibrils (>/=2) respectively connected with an electronic conducting line are bonded together after the fibrils are insulated by high molecular insulation materials, and integration microelectrode team is obtained. The integration microelectrode team is penetrated in a glass pipe and is sealed by epoxy resin, after the epoxy resin is solidified, the end surface of an electrode is polished, and the integrated multiple ultra micro-micro disc electrode is obtained. Compared with the traditional double ultra micro-micro disc electrode, the integrated multiple ultra micro-micro disc electrode prepared by the method for preparing an integrated multiple ultra micro-micro disc electrode has the advantages of low price, simple preparation, no need of an auxiliary instrument apparatus, small electrode gap, unlimited micro disc electrode number, etc. The integrated multiple ultra micro-micro disc electrode can be used for the fields of electrochemistry, analytical chemistry, electric analytical chemistry and bioelectricity analytical chemistry, and the integrated multiple ultra micro-micro disc electrode quantitatively detects and analyzes substances with different electrochemistry activities.
Description
Technical field
The present invention relates to a kind of preparation method of integrated multiple ultramicro microdisc electrode.
Background technology
Many ultramicroelectrodes be owing to can carry out check and analysis to the different material of electrochemical activity simultaneously, thereby are used widely in Electroanalytical Chemistry and life science.For example, two ultramicroelectrodes and liquid chromatography coupling can improve the selectivity of liquid chromatography/electrochemical system, thereby reach purpose (Roston, the D.A. of the electro-active species in the analyzing and testing complex biological sample; Kissinger, P.T.Analytical Chemistry (1981), 53 (11), 1695-1699.); Two ultramicroelectrodes and Capillary Electrophoresis coupling can improve the sensitivity and the selectivity of Capillary Electrophoresis/electrochemical system, to the research of electroactive living things system very effective (Zhong, M.; Zhou, J.; Lunte, S.M.; Zhao, G.; Giolando, D.M.; Kirchhoff, J.R.Analytical Chemistry (1996), 68 (1), 203-207.).Many ultramicroelectrodes mainly contain two kinds of many ultra micros post electrode and multiple ultramicro microdisc electrodes.Wherein, multiple ultramicro microdisc electrode is used for detection by quantitative science, accurate more.Following two kinds of methods are often used in the preparation of traditional multiple ultramicro microdisc electrode: a kind of is at microscopically many wire electrodes to be arranged in parallel, and uses an end of epoxy resin fixed electorde silk then, and the other end of wire electrode is connected (Peng, W. with elargol with electronic wire; Li, P.; Zhou X.Y.J.Electroanal.Chem. (1993), 347,1-14.); Another kind is to penetrate a wire electrode respectively in two pipes with the θ glass tube, uses front end (Whited, the B.L. of epoxy sealing wire electrode then; Motsegood, P.N.; Baur, J.E.J.Chromatography A. (1997), 771,89-98.).The first method complicated operation, and the spacing of carbon fiber is difficult to adjust to a smaller value (spacing of two carbon fiber electrodes is more little, and the data of on-the-spot synchronous detection are scientific and reasonable more); Second method is simple, yet the θ glass tube is an external product, for domestic researcher, be difficult for obtaining and price comparatively expensive; This method can not prepare number of electrodes and surpass 2 multiple ultramicro microdisc electrode in addition.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of simple, cheap, closely spaced integrated multiple ultramicro microdisc electrode.
The technical solution used in the present invention is for achieving the above object: a kind of preparation method of integrated multiple ultramicro microdisc electrode may further comprise the steps:
(1) two are connected with the enamel-cover tinsel of front end coating removal respectively with the top electrode microfilament obtain two with top electrode;
(2) the front end current-carrying part of the electrode that step (1) is obtained, comprise that electrode microfilament, electrode microfilament and enamel-cover tinsel junction and enamel-cover coating removal wiry place are immersed in the solution that is dissolved with insulation macromolecular material Kynoar or Nafion, the characteristic of this Polymer Solution is can be attached on the electrode surface, and can form polymeric membrane insulation, that antiacid alkali ability is arranged after the solvent evaporates.Guarantee to have one deck solution to take out attached to back on the electrode surface, make solvent evaporates after, the polymeric membrane that one deck insulate has all been adhered at the electrode microfilament of electrode front end, electrode microfilament and enamel-cover tinsel junction and enamel-cover coating removal wiry place;
(3) the electrode microfilament paralleling binding of the electrode that step (2) is obtained with cementing agent obtains many microelectrodes conglomerate of incorporate mutually insulated together;
(4) many microelectrodes conglomerate is penetrated in the glass tube, and be installed with the glass tube of electrode conglomerate until epoxy resin cure with epoxy sealing;
(5) the polishing electrode end surface promptly obtains integrated multiple ultramicro microdisc electrode.
According to the present invention, also can be in step (3) when electrode microfilament paralleling binding be together, with enamel-cover tinsel paralleling binding together with cementing agent.
The used cementing agent of the present invention can be the cementing agent used always such as epoxy resin etc., also can be the solution of above-mentioned insulation macromolecular material.
Said method of the present invention is applicable to the many microdisk electrodes of micron order of various different materials of preparation and different size.That the multiple ultramicro microdisc electrode of this method preparation has is cheap, preparation is simple, need not advantages such as supplementary instrument equipment, electrode separation is little, number of poles is unrestricted.
Description of drawings
The structural representation of of the present invention pair of ultra micro carbon fiber/platinum microdisk electrode of Fig. 1 (1. scribbles the carbon fiber of polyvinylidene fluoride film; 2. scribble the platinum filament of polyvinylidene fluoride film; 3. elargol; 4. enamel-cover copper wire; 5. polyvinylidene difluoride film; 6. epoxy resin; 7. glass tube).
(wherein, a is diameter 7 μ m carbon fiber plates to Fig. 2 for the stereoscan photograph of 500 times on two ultra micro carbon fibers of the present invention preparation/platinum microdisk electrode end face amplification; B is a Kynoar; C is diameter 20 μ m platinum dishes).
(wherein m is the cyclic voltammetry curve of diameter 7 μ m carbon fiber ultramicro disc electrodes to the cyclic voltammetry curve of two ultra micro carbon fibers/platinum microdisk electrode in the potassium ferricyanide solution of 20mM that Fig. 3 prepares for the present invention; N is the cyclic voltammetry curve of diameter 20 μ m platinum ultramicro disc electrodes; Sweep speed: 10mV/s).
Fig. 4 amplifies 200 times of photos for six ultra micro platinum microdisk electrodes (d is the platinum dish of diameter 100 μ m, and e is the Nafion film that is coated on the platinum) the end face optics of the present invention's preparation.
The cyclic voltammetry curve of the six ultra micro platinum microdisk electrodes (diameter 100 μ m) that Fig. 5 polished for the first summary of the present invention preparation in the potassium ferricyanide solution of 20mM (swept speed: 10mV/s).
Embodiment
Embodiment 1:
The preparation of two ultra micro carbon fibers/platinum microdisk electrode
1. with diameter be 7 μ m to be about the carbon fiber (CF) of 1.5cm and diameter be that platinum (Pt) silk that 20 μ m are about 1.5cm was used acetone, absolute ethyl alcohol, ultrapure water ultrasonic cleaning 3～5 minutes successively, use ultrapure water drip washing after the taking-up again; The electrode microfilament of cleaning is placed in the drying box 50 ℃ of dryings 10 hours, standby.
2. carbon fiber is connected with the enamel-cover copper wire of front end coating removal with elargol and obtains carbon fiber electrode.
3. the front end of carbon fiber electrode is immersed mass ratio and be in the acetone soln of 0.5% Kynoar, take out, air-dry in air, make carbon fiber, carbon fiber and the enamel-cover copper wire junction of electrode front end and the coating removal place of enamel-cover copper wire all coat the polyvinylidene difluoride film that one deck insulate.
4. platinum filament is connected with the enamel-cover copper wire with elargol and obtains platinum electrode; The front end of platinum electrode is also immersed in the acetone soln with the Kynoar of concentration, takes out, air-dry before, utilize the viscosity of Kynoar solution, platinum filament on the platinum electrode and the carbon fiber paralleling binding on the carbon fiber electrode are got up; Simultaneously, the electronic wire enamel-cover copper wire of two electrodes with 5% Kynoar solution paralleling binding, after solution is air-dry, the two microelectrodes of incorporate carbon fiber/platinum have just been obtained.
5. penetrate this incorporate pair of microelectrode in the glass tube carefully; Fill up glass tube with sealing and fixed electorde with epoxy resin then.
6. after the epoxy resin full solidification, the polishing electrode end surface promptly obtains the two ultramicro microdisc electrodes of carbon fiber/platinum as shown in Figure 1; The electromicroscopic photograph of electrode end surface illustrates that the spacing of this pair ultramicro microdisc electrode is small among Fig. 2.
7. carbon fiber and the platinum ultramicro disc electrode mutually insulated in two two ultramicro microdisc electrodes of distinct cyclic voltammetric characteristic curve explanation carbon fiber/platinum among Fig. 3, and chemical property is good.
Embodiment 2
The preparation of six ultra micro platinum disk electrodes
1. getting 6 diameters is the platinum filament that 100 μ m are about 2cm, cleans by the step 1 of embodiment 1.
2. with elargol 6 platinum filaments are connected with 6 enamel-cover copper wires of front end coating removal respectively, obtain 6 platinum electrodes.
3. the front end of 6 platinum electrodes is immersed mass ratio respectively and be in the ethanolic solution of 5% Nafion, take out, air-dry in air, make platinum filament, platinum filament and the enamel-cover copper wire junction of 6 platinum electrode front ends and the Nafion film that enamel-cover coating removal wiry place all coats one deck insulation.
4. use liquid-state epoxy resin, with 6 platinum microfilaments that coated Nafion film bonding that is parallel to each other; Simultaneously, utilize 6 enamel-cover copper wires of Kynoar solution paralleling binding of 5%, behind the epoxy resin cure, obtain incorporate 6 ultra micro platinum electrodes.
5. penetrate these incorporate 6 ultra micro platinum electrodes in the glass tube carefully; Fill up glass tube with sealing and fixed electorde with epoxy resin then.
6. after the epoxy resin full solidification, the polishing electrode end surface promptly obtains 6 ultra micro platinum disk electrodes; The optical microscope photograph of electrode end surface illustrates that this spacing that surpasses between 6 little platinum disk electrodes is small among Fig. 4.
7. the cyclic voltammetric characteristic curve that six are separated among Fig. 5 illustrates that each platinum ultramicro disc electrode mutually insulated in the 6 ultra micro platinum disk electrodes is good; And chemical property is good.
Claims (3)
1. the preparation method of an integrated multiple ultramicro microdisc electrode is characterized in that, may further comprise the steps:
(1) two are connected with the enamel-cover tinsel of front end coating removal respectively with the top electrode microfilament obtain two with top electrode;
(2) the front end current-carrying part of the electrode that step (1) is obtained is immersed in the solution that is dissolved with insulation macromolecular material Kynoar or Nafion, takes out that the back is air-dry to obtain the electrode that front end current-carrying part surface attachment has the polymeric membrane of insulation;
(3) the electrode microfilament paralleling binding of the electrode that step (2) is obtained with cementing agent obtains many microelectrodes conglomerate of incorporate mutually insulated together;
(4) many microelectrodes conglomerate is penetrated in the glass tube, and be installed with the glass tube of electrode conglomerate until epoxy resin cure with epoxy sealing;
(5) the polishing electrode end surface promptly obtains integrated multiple ultramicro microdisc electrode.
2. preparation method according to claim 1 is characterized in that: in step (3) when electrode microfilament paralleling binding together, with enamel-cover tinsel paralleling binding together with cementing agent.
3. preparation method according to claim 1 and 2 is characterized in that: used cementing agent is the solution of above-mentioned insulation macromolecular material.
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| CNB2006100189714A CN100395545C (en) | 2006-04-28 | 2006-04-28 | Method for preparing integrated multiple ultramicro microdisc electrode |
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| CN100395545C true CN100395545C (en) | 2008-06-18 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100533135C (en) * | 2006-12-29 | 2009-08-26 | 中国科学院长春应用化学研究所 | Rotary point-disk electrode |
| CN100545648C (en) * | 2007-05-15 | 2009-09-30 | 中国科学院长春应用化学研究所 | The preparation method of a kind of microdisk electrode or little disk array electrode |
| CN103048368B (en) * | 2011-10-14 | 2016-03-09 | 深圳市海盈科技有限公司 | A kind of simple method for preparing of ultramicroelectrode |
| CN111505071B (en) * | 2020-04-13 | 2022-06-10 | 商丘师范学院 | Integrated microelectrode sensor for simultaneous detection of pH and AA and preparation method and application thereof |
Citations (8)
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|---|---|---|---|---|
| US5185922A (en) * | 1990-08-17 | 1993-02-16 | Cornell Research Foundation, Inc. | Method of making submicrometer microelectrodes |
| US5254235A (en) * | 1992-02-26 | 1993-10-19 | The Yellow Springs Instrument Company | Microelectrode arrays |
| CN1110786A (en) * | 1994-04-29 | 1995-10-25 | 武汉大学 | Ultramicro nm electrode and ultramicro sensor |
| JP2001021580A (en) * | 1999-06-22 | 2001-01-26 | Ind Technol Res Inst | Manufacture of probe device |
| CN1282870A (en) * | 1999-07-30 | 2001-02-07 | 武汉大学 | Process for preparing low-noise non-class carbon fibre electrode |
| US20030116447A1 (en) * | 2001-11-16 | 2003-06-26 | Surridge Nigel A. | Electrodes, methods, apparatuses comprising micro-electrode arrays |
| JP2004285405A (en) * | 2003-03-20 | 2004-10-14 | Kanagawa Acad Of Sci & Technol | Microelectrode array and manufacturing method therefor |
| CN1544928A (en) * | 2003-11-17 | 2004-11-10 | 中国科学院长春应用化学研究所 | Preparing method of micro disk array electrode |
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- 2006-04-28 CN CNB2006100189714A patent/CN100395545C/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5185922A (en) * | 1990-08-17 | 1993-02-16 | Cornell Research Foundation, Inc. | Method of making submicrometer microelectrodes |
| US5254235A (en) * | 1992-02-26 | 1993-10-19 | The Yellow Springs Instrument Company | Microelectrode arrays |
| CN1110786A (en) * | 1994-04-29 | 1995-10-25 | 武汉大学 | Ultramicro nm electrode and ultramicro sensor |
| JP2001021580A (en) * | 1999-06-22 | 2001-01-26 | Ind Technol Res Inst | Manufacture of probe device |
| CN1282870A (en) * | 1999-07-30 | 2001-02-07 | 武汉大学 | Process for preparing low-noise non-class carbon fibre electrode |
| US20030116447A1 (en) * | 2001-11-16 | 2003-06-26 | Surridge Nigel A. | Electrodes, methods, apparatuses comprising micro-electrode arrays |
| JP2004285405A (en) * | 2003-03-20 | 2004-10-14 | Kanagawa Acad Of Sci & Technol | Microelectrode array and manufacturing method therefor |
| CN1544928A (en) * | 2003-11-17 | 2004-11-10 | 中国科学院长春应用化学研究所 | Preparing method of micro disk array electrode |
Non-Patent Citations (2)
| Title |
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| 碳纤维组合超微圆盘电极的伏安特性与理论验证. 赵凯元等.分析化学，第31卷第2期. 2003 |
| 碳纤维组合超微圆盘电极的伏安特性与理论验证. 赵凯元等.分析化学，第31卷第2期. 2003 * |
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