CN101051033A - Method for preparing micro disc electrode or micro disc array electrode - Google Patents
Method for preparing micro disc electrode or micro disc array electrode Download PDFInfo
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- CN101051033A CN101051033A CN 200710055628 CN200710055628A CN101051033A CN 101051033 A CN101051033 A CN 101051033A CN 200710055628 CN200710055628 CN 200710055628 CN 200710055628 A CN200710055628 A CN 200710055628A CN 101051033 A CN101051033 A CN 101051033A
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Abstract
A method for preparing micro-plate electrode includes using transparent glue tap to enclose groove on teflon plate, laying metal wire vertical to groove and fixing metal wire above groove, using resin to embed metal wire, curing it under room temperature then removing off said resin, bending it and inserting it into glass tube, leading exposed end of metal wire out by wire, inserting another end into resin and sealing it by siphon, curing it under room temperature, grinding out end surface of metal wire and polishing surface of electrode.
Description
Technical field
The invention belongs to the preparation method of a kind of microdisk electrode or little disk array electrode.
Background technology
Microelectrode is meant that the one dimension of electrode is of a size of a micron-sized class electrode.When the size of electrode surface was reduced to micron order, electrode shows many good electrochemical properties that are different from conventional electrodes: the electric current of microelectrode can reach stable state at short notice, and the response time is short; The current density height; The ratio of charging current and faradic currents is very little, helps to improve signal to noise ratio (S/N ratio); Low solution potential falls, and can be used for the high impedance system.According to the geometric configuration difference, microelectrode can be divided into polytype, and wherein the surface is discoid little disk electrode that is called, and is a kind of more common electrode, claims microdisk electrode again.In actual experiment, because the electric current of single microdisk electrode is restricted so use sometimes less than the detection lower limit of conventional electrochemical apparatus.
Tiny array electrode is meant by a plurality of microelectrodes and integrates the electrode of being formed, its electric current be adding of each unitary electrode electric current and.Tiny array electrode has kept the characteristic of original unitary electrode, can obtain bigger strength of current again, and conventional electrochemical apparatus can be measured its signal, so help analytical applications.
People such as V.Rehacek [Vacuum 80,2005,132] use photoetching process; People [Sensor andActuatorB 113,2006,545] such as Laurent G use the microelectronics printing technology; H.X.He[Langmuir 16,2000, and 9684] obtained tiny array electrode respectively with soft printing stencil method.But the equal more complicated of above method needs special exact instrument, and cost is higher, and ordinary laboratory is difficult for carrying out; The electrode surface of making can not grind renewal, poor reproducibility.Document: [A.J.Bard, F.Fan, M.V.Mirkin, in:Bard A.J. (Ed.), ElectroanalyticalChemistry, vol.18, Marcel Dekker, New York, 1993, p.243.], reported a kind of method that obtains microelectrode in the thermoplastic soft glass pipe that the micron order platinum filament is enclosed in.Though this method does not need complicated large-scale instrument, complicated operation is difficult for grasping, and is difficult to make array electrode.Chinese patent notification number CN1544928A, open day is on November 10th, 2004, and name is called to mention with quartz capillary encapsulated electrode material among the preparation method of little disk array electrode makes array electrode, and this method step is many, operates more loaded down with trivial details.
Summary of the invention
The present invention has overcome above-mentioned many shortcomings of prior art, and the preparation method of a kind of microdisk electrode or little disk array electrode is provided.Its step and condition are:
(1) preparation of embedding resin material film wiry
Shown in attached Fig. 1 and 2,1. go up with adhesive tape at the teflon flat board and 2. to surround strip groove; 2. paste double sticky tape 3. at adhesive tape on, with an one metal wire or the 4. parallel teflon flat board of many one metal wires 1. and perpendicular to trench length direction fixed placement or side by side uniformly-spaced fixed placement on double sticky tape, make the teflon flat board top 1. that is suspended from the groove, the modulation resin material 5., 4. it also buried tinsel in above-mentioned groove, and then 5. resin material flattened, after 5. resin material solidifies under the room temperature, tinsel on the one side double sticky tape blocked along this side trench inner face together with resin material abandon it, tinsel on the opposite side double sticky tape is together peeled together with resin material, obtain being embedded with tinsel and the exposed resin material film of an end wiry;
Described resin material is preferred: rigidity polyesters mould material or resin material;
(2) encapsulation of electrode
The exposed resin material film of a tinsel and an end wiry will be embedded with, be curled into column along described strip groove length direction, insert in the glass tube of both ends open, the end that tinsel in the described glass tube is exposed connects lead with conductive tape and draws, the glass tube other end is inserted siphon sealing in the fresh resin material together with wherein being embedded with resin material film wiry, place again under the room temperature and solidify, obtain microdisk electrode or little disk array electrode semi-manufacture;
(3) polishing of electrode
The sealed end of microdisk electrode or the half-finished insertion resin of little disk array electrode is exposed tinsel end face and polishing with sand papering, obtain electrode surface,, obtain a kind of microdisk electrode or little disk array electrode with this electrode surface of secondary water ultrasonic cleaning.
Be embedded in microdisk electrode or the little disk array electrode that kind wiry in the resin material can obtain different metal by change, be embedded in number wiry in the resin material by change, can the array of controls electrode in the number of working electrode; Electrode surface can grind renewal, and electrode can stand to be repeatedly used.
Optimum condition is in the preparation process (1) of embedding of the present invention resin material film wiry: the described width of 1. going up the strip groove that 2. surrounds with adhesive tape at the teflon flat board is 2-5 centimetre, the degree of depth is the 0.3-0.8 millimeter, and length can be selected as required;
3. 1. and perpendicular to the trench length direction the 4. parallel teflon flat board of described many one metal wires uniformly-spaced gone up for the 0.5-1 millimeter is fixed on double sticky tape side by side.
Means of testing: adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s.Whether be S shape, if S shape, the preparation that shows tiny array electrode is successful if detecting cyclic voltammetry curve, can be used for actual electrochemistry experiment; If cyclic voltammetry curve is not a S shape, continue the grinding and polishing electrode, clean, ultrasonic, S-shaped up to cyclic voltammetry curve.After finishing, test uses secondary water cleaning electrode surface.
This preparation method's cost is extremely low, simple to operate, and without any need for instrument, ordinary laboratory can be prepared easily.
Description of drawings
Fig. 1 is the cross section view of front view of making the groove of microdisk electrode or little disk array electrode.
Fig. 2 is a vertical view of making the groove of microdisk electrode or little disk array electrode.
Embodiment
Embodiment 1 (golden microdisk electrode):
1. go up at the teflon flat board that 2. to surround length with adhesive tape be 5 centimetres, width is 5 centimetres, and the degree of depth is 0.8 millimeter strip groove; 2. paste double sticky tape 3. at adhesive tape on, with a diameter is that 4. 25 microns spun gold is fixed on the double sticky tape perpendicular to the trench length direction, make spun gold 4. be suspended from the groove top, modulation polyesters rigidity mould material 5., fall in above-mentioned groove, 5. polyesters rigidity mould material is flattened, after solidifying under the room temperature 4. the spun gold on the side double sticky tape blocked along this side trench inner face together with resin material and abandon it, 4. spun gold on the opposite side double sticky tape is together peeled together with resin material, and obtaining being embedded with a diameter is 25 microns the spun gold and the exposed resin material film of an end of spun gold; This film is curled into column, inserts in the glass tube of both ends open, the end that spun gold exposes connects lead with conductive tape and draws, and the other end inserts fresh polyesters rigidity mould material siphon sealing, places under the room temperature and solidifies, and obtains the microdisk electrode semi-manufacture; The sealed end of the half-finished insertion resin of microdisk electrode is exposed spun gold end face and polishing with sand papering, obtains electrode surface,, be that 600 abrasive paper for metallograph polishes electrode surface with granularity then, with α-Al of 1 micron
2O
3Powder with secondary water ultrasonic cleaning electrode surface, obtains a kind of golden microdisk electrode on polishing cloth upthrow optoelectronic pole surface.
Adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s, detecting cyclic voltammetry curve is S shape, the preparation that shows microelectrode is successful.
Embodiment 2 (platinum microdisk electrode):
1. go up at the teflon flat board that 2. to surround length with adhesive tape be 5 centimetres, width is 2 centimetres, and the degree of depth is 0.3 millimeter strip groove; 2. paste double sticky tape 3. at adhesive tape on, with a diameter is that 20 microns platinum filament is fixed on the double sticky tape perpendicular to the trench length direction, make platinum filament be suspended from the groove top, modulation polyesters rigidity mould material 5., fall in above-mentioned groove, 5. polyesters rigidity mould material is flattened, after solidifying under the room temperature platinum filament on the side double sticky tape blocked along this side trench inner face together with resin material and abandon it, platinum filament on the opposite side double sticky tape is together peeled together with resin material, and obtaining being embedded with a diameter is 20 microns the platinum filament and the exposed resin material film of an end of platinum filament; This film is curled into column, inserts in the glass tube of both ends open, the end that platinum filament exposes connects lead with conductive tape and draws, and the other end inserts fresh polyesters rigidity mould material siphon sealing, places under the room temperature and solidifies, and obtains the microdisk electrode semi-manufacture; The sealed end of the half-finished insertion resin of microdisk electrode is exposed platinum filament end face and polishing with sand papering, obtains electrode surface,, be that 600 abrasive paper for metallograph polishes electrode surface with granularity then, with α-Al of 1 micron
2O
3Powder with secondary water ultrasonic cleaning electrode surface, obtains a kind of platinum microdisk electrode on polishing cloth upthrow optoelectronic pole surface.。
Adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s, detecting cyclic voltammetry curve is S shape, the preparation that shows the platinum microdisk electrode is successful.
Embodiment 3 (golden little disk array electrode):
1. go up at the teflon flat board that 2. to surround length with adhesive tape be 5 centimetres, width is 4 centimetres, and the degree of depth is the strip groove of 0.5 millimeter strip groove; 2. paste double sticky tape 3. at adhesive tape on, with 32 diameters be 25 microns spun gold 4. side by side perpendicular to the trench length direction uniformly-spaced 0.5 millimeter be fixed on double sticky tape and 3. go up, make spun gold be suspended from the groove top, modulation polyesters rigidity mould material 5., fall in above-mentioned groove, polyesters rigidity mould material is flattened, after solidifying under the room temperature spun gold on the side double sticky tape blocked along this side trench inner face together with resin material and abandon it, spun gold on the opposite side double sticky tape is together peeled together with resin material, and obtaining being embedded with 32 diameters is 25 microns the spun gold and the exposed resin material film of an end of spun gold; This film is curled into column, insert in the glass tube of both ends open, the end that spun gold exposes connects lead with conductive tape and draws, and the other end inserts fresh polyesters rigidity mould material siphon sealing, place under the room temperature and solidify, obtain little disk array electrode semi-manufacture; The sealed end of the half-finished insertion resin of little disk array electrode is exposed spun gold end face and polishing with sand papering, obtains electrode surface,, be that 600 abrasive paper for metallograph polishes electrode surface with granularity then, with α-Al of 1 micron
2O
3Powder with secondary water ultrasonic cleaning electrode surface, obtains the little disk array electrode of a kind of gold on polishing cloth upthrow optoelectronic pole surface.
Adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s, detecting cyclic voltammetry curve is S shape, the preparation that shows golden little disk array electrode is successful.
Embodiment 4 (golden little disk array electrode):
1. go up at the teflon flat board that 2. to surround length with adhesive tape be 5 centimetres, width is 4 centimetres, and the degree of depth is the strip groove of 0.5 millimeter strip groove; 2. paste double sticky tape 3. at adhesive tape on, with 17 diameters be 25 microns spun gold 4. side by side perpendicular to the trench length direction uniformly-spaced 0.5 millimeter be fixed on double sticky tape and 3. go up, make spun gold be suspended from the groove top, modulating epoxy resin 5., fall in above-mentioned groove, epoxy resin is flattened, after solidifying under the room temperature spun gold on the side double sticky tape blocked along this side trench inner face together with resin material and abandon it, spun gold on the opposite side double sticky tape is together peeled together with resin material, and obtaining being embedded with 17 32 diameters is 25 microns the spun gold and the exposed resin material film of an end of spun gold; This film is curled into column, inserts in the glass tube of both ends open, the end that spun gold exposes connects lead with conductive tape and draws, and the other end inserts fresh epoxy resin siphon sealing, places under the room temperature and solidifies, and obtains little disk array electrode semi-manufacture; The sealed end of the half-finished insertion resin of little disk array electrode is exposed spun gold end face and polishing with sand papering, obtains electrode surface,, be that 600 abrasive paper for metallograph polishes electrode surface with granularity then, with α-Al of 1 micron
2O
3Powder with secondary water ultrasonic cleaning electrode surface, obtains the little disk array electrode of a kind of gold on polishing cloth upthrow optoelectronic pole surface.
Adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s, detecting cyclic voltammetry curve is S shape, the preparation that shows golden little disk array electrode is successful.
Embodiment 5 (the little disk array electrode of platinum):
1. go up at the teflon flat board that 2. to surround length with adhesive tape be 5 centimetres, width is 4 centimetres, and the degree of depth is the strip groove of 0.5 millimeter strip groove; 2. paste double sticky tape 3. at adhesive tape on, with 10 diameters be 20 microns platinum filament 4. side by side perpendicular to the trench length direction uniformly-spaced 1 millimeter be fixed on double sticky tape and 3. go up, make platinum filament be suspended from the groove top, modulating epoxy resin 5., fall in above-mentioned groove, epoxy resin is flattened, after solidifying under the room temperature platinum filament on the side double sticky tape blocked along this side trench inner face together with resin material and abandon it, platinum filament on the opposite side double sticky tape is together peeled together with resin material, and obtaining being embedded with a diameter is 20 microns the platinum filament and the exposed resin material film of an end of platinum filament; This film is curled into column, inserts in the glass tube of both ends open, the end that platinum filament exposes connects lead with conductive tape and draws, and the other end inserts fresh epoxy resin siphon sealing, places under the room temperature and solidifies, and obtains little disk array electrode semi-manufacture; The sealed end of the half-finished insertion resin of little disk array electrode is exposed platinum filament end face and polishing with sand papering, obtains electrode surface,, be that 600 platinum phase sand paper polishes electrode surface with granularity then, with α-Al of 1 micron
2O
3Powder with secondary water ultrasonic cleaning electrode surface, obtains the little disk array electrode of a kind of platinum on polishing cloth upthrow optoelectronic pole surface.
Adopt three-electrode system, contrast electrode is Ag/AgCl (saturated KCl), is the spiral fashion platinum filament to electrode.At the Fe of 1mM (CN)
6 3-0.5M KCl aqueous solution in electric potential scanning, potential range is 0.6-0V, sweeps speed for 0.01V/s, detecting cyclic voltammetry curve is S shape, shows that the preparation of the little disk array electrode of platinum is successful.
Claims (2)
1, the preparation method of a kind of microdisk electrode or little disk array electrode is characterized in that, step and condition are as follows:
(1) preparation of embedding resin material film wiry
On the teflon flat board, surround strip groove with adhesive tape; On adhesive tape, paste double sticky tape, with the parallel teflon of an one metal wire or many one metal wires dull and stereotyped and perpendicular to trench length direction fixed placement or side by side uniformly-spaced fixed placement on double sticky tape, make the top that is suspended from the teflon flat board in the groove, the modulation resin material, it is buried in above-mentioned groove and tinsel, and then resin material flattened, after resin material solidifies under the room temperature, tinsel on the one side double sticky tape blocked along this side trench inner face together with resin material abandon it, tinsel on the opposite side double sticky tape is together peeled together with resin material, obtain being embedded with tinsel and the exposed resin material film of an end wiry;
Described resin material is preferred: rigidity polyesters mould material or resin material;
(2) encapsulation of electrode
The exposed resin material film of a tinsel and an end wiry will be embedded with, be curled into column along described strip groove length direction, insert in the glass tube of both ends open, the end that tinsel in the described glass tube is exposed connects lead with conductive tape and draws, the glass tube other end is inserted siphon sealing in the fresh resin material together with wherein being embedded with resin material film wiry, place again under the room temperature and solidify, obtain microdisk electrode or little disk array electrode semi-manufacture;
(3) polishing of electrode
The sealed end of microdisk electrode or the half-finished insertion resin of little disk array electrode is exposed tinsel end face and polishing with sand papering, obtain electrode surface,, obtain a kind of microdisk electrode or little disk array electrode with this electrode surface of secondary water ultrasonic cleaning.
2, the preparation method of a kind of microdisk electrode as claimed in claim 1 or little disk array electrode, it is characterized in that, the width of the described strip groove that surrounds with adhesive tape on the teflon flat board is 2-5 centimetre, and the degree of depth is the 0.3-0.8 millimeter, and length can be selected as required;
The parallel teflon of described many one metal wires is dull and stereotyped and uniformly-spaced be fixed on the double sticky tape for the 0.5-1 millimeter side by side perpendicular to the trench length direction.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101726524B (en) * | 2009-12-21 | 2013-04-10 | 中国科学院长春应用化学研究所 | Micro-disk array electrode assembly and method for preparing micro-disk array electrode |
| CN108680627A (en) * | 2018-06-27 | 2018-10-19 | 宁波大学 | Micro-nano sensor and preparation method thereof for detecting Organic substance in water content |
| CN111879832A (en) * | 2020-06-12 | 2020-11-03 | 宁波水表(集团)股份有限公司 | Sensor for detecting residual chlorine in tap water and preparation method thereof |
| CN111948267A (en) * | 2020-08-20 | 2020-11-17 | 哈尔滨工业大学 | Method for preparing electrochemical nano point array electrode by using ultra-long nanowire |
| CN112134140A (en) * | 2020-09-07 | 2020-12-25 | 南京邮电大学 | Electrically-controlled active coupled cavity laser |
Family Cites Families (3)
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| SE523309E (en) * | 2001-06-15 | 2009-10-26 | Replisaurus Technologies Ab | Method, electrode and apparatus for creating micro- and nanostructures in conductive materials by patterning with master electrode and electrolyte |
| CN100362342C (en) * | 2005-11-18 | 2008-01-16 | 武汉大学 | Method for preparing carbon fiber ultramicro disc electrode |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101726524B (en) * | 2009-12-21 | 2013-04-10 | 中国科学院长春应用化学研究所 | Micro-disk array electrode assembly and method for preparing micro-disk array electrode |
| CN108680627A (en) * | 2018-06-27 | 2018-10-19 | 宁波大学 | Micro-nano sensor and preparation method thereof for detecting Organic substance in water content |
| CN108680627B (en) * | 2018-06-27 | 2023-09-12 | 宁波大学 | Micro-nano sensor for detecting organic matter content in water and manufacturing method thereof |
| CN111879832A (en) * | 2020-06-12 | 2020-11-03 | 宁波水表(集团)股份有限公司 | Sensor for detecting residual chlorine in tap water and preparation method thereof |
| CN111948267A (en) * | 2020-08-20 | 2020-11-17 | 哈尔滨工业大学 | Method for preparing electrochemical nano point array electrode by using ultra-long nanowire |
| CN111948267B (en) * | 2020-08-20 | 2023-07-18 | 哈尔滨工业大学 | Method for preparing electrochemical nanodot array electrode by using ultra-long nanowires |
| CN112134140A (en) * | 2020-09-07 | 2020-12-25 | 南京邮电大学 | Electrically-controlled active coupled cavity laser |
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