CN1544928A - Preparing method of micro disk array electrode - Google Patents
Preparing method of micro disk array electrode Download PDFInfo
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- CN1544928A CN1544928A CNA2003101100437A CN200310110043A CN1544928A CN 1544928 A CN1544928 A CN 1544928A CN A2003101100437 A CNA2003101100437 A CN A2003101100437A CN 200310110043 A CN200310110043 A CN 200310110043A CN 1544928 A CN1544928 A CN 1544928A
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Abstract
The invention is a method of preparing microdisc array, adopting 4 steps: firstly inserting micron or nano fiber electrode material in quartz capillaries, then placing these capillaries in different shaped templates and fixing them into electrode array with different appearance on the surface. Inserting the template in the glass tube, one end of the electrode material is connected and led out by copper wires using Ag conductive glue, and the other end is injected with epoxy glue and packaged, and placing and solidifying the electrode array at room temperature. Placing the solidified microdisc array electrodes in sequence on the rough sand paper and 1.5, 0.5, and 0.03 mum alpha -Al2O3 for smoothing and polishing, then making circulating volt-ampere in the Fe(CN)63- water solution at 5mmol/L, where the supporting electrolyte is KCl at 1mol/L, the potential range is 0.6-0v, and the scanning speed is 0.01V/s and if the circulating volt-ampere graph is S-shaped, it shows that the microdisc array electrodes are successful.
Description
Technical field
The invention belongs to the preparation method of little disk array electrode.
Background technology
Microelectrode is meant that the one dimension of electrode is of a size of a micron or a nano level class electrode, when the one dimension size of electrode when the millimeter level is reduced to micron, show many good electrochemical properties that are different from conventional electrodes: the intrinsic very little RC time constant of microelectrode makes it to be used for quick, transient state electrochemical reaction are studied; The IR that little polarization current has reduced system on the microelectrode falls, make it to be used for high-resistance system, comprise low supporting electrolyte concentration even do not have supporting electrolyte solution, gas phase system, semisolid and all solid state system, these characteristics provide a kind of powerful measure for people explore the micromechanism of material.According to the difference of electrode geometry, microelectrode can be divided into different types, and wherein a kind of electrode surface is discoid little disk electrode that is called, because its structure is relative simple with preparation, is the most frequently used electrode in the experiment.But single little disk electrode is when the high-resistance system of research, and faradic currents sometimes are lower than 10
-12A, conventional electrochemical apparatus is difficult to measure its signal.Little disk array electrode can well address this problem, it is meant by a plurality of little disk electrodes combines the single set electrode of formed outward appearance, can obtain strength of current and the electrochemical signals more much bigger by the electrode number that increases in the array than single microelectrode, the characteristic that has kept little disk electrode simultaneously, common electrochemical apparatus can satisfy the requirement of test high impedance low current system.
C.R.Martin[Anal.Chem.67,1995,1920] nanowires of gold is deposited in the micropore of film, H.X.He[Langmuir 16,2000,9684] with the method for soft printing stencil, H.Kaden[Electrochem.Commun.2,2000,606] with exact instrument electrode material is sealed in and has prepared little disk array electrode in the epoxy glue.But generally speaking there is following shortcoming in above-mentioned these several preparation method's more complicated: the exact instrument that needs are special, and cost is higher, and ordinary laboratory is difficult to preparation; Electrode material is stochastic distribution in encapsulant, when carrying out electrochemical test, be easy to cause the overlapping of electric capacity between the adjacent electrode and diffusion, cause little disk array electrode to present the electrochemical behavior of conventional large electrode, lost the good characteristic of microelectrode; To test the rear electrode surface intractable that finishes clean at every turn, and poor reproducibility can not be reused.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of little disk array electrode.
The present invention inserts electrode material in the quartz capillary of certain diameter earlier, then these quartz capillaries is fixed on the electrod-array of making various patterns in the difform template.Template is inserted in the glass tube, and an end of electrode material utilizes silver conductive adhesive to connect with copper cash and draws, and the other end seals with epoxy glue, places under the room temperature to solidify.The little disk array electrode that is cured is used flint glass paper, α-Al successively
2O
3Grinding and polishing carries out pre-service and sign then to expose electrode surface.This preparation method is simple, convenient, pervasive, does not need accurate instrument, and ordinary laboratory just can prepare; The overlapping of electric capacity and diffusion between the adjacent electrode avoided in calculating by in advance and design, can make the electrod-array of the required various surface topographies of test; Electrode can be reused, and cost is very cheap.
Method of the present invention adopts following 4 steps to carry out:
(1) electrode material is inserted in the quartz capillary
With long 2cm diameter is micron order or nano level fibrous electrode material: the tinsel or the carbon fiber of platinum, gold, insert in the quartz capillary of long 1cm.For array electrode, for fear of electric capacity between the contiguous microelectrode and the overlapping generation of diffusion, requiring the distance between the contiguous microelectrode generally speaking is more than 6 times of electrode material diameter at least, is the pipe wall thickness that has greater than 6 times of electrode material diameters for the requirement of quartz capillary.
(2) curing of electrode material and encapsulation
Many quartz capillaries that are inserted with electrode material are fixed on composition linearity, annular, disc or rectangular electrod-array in the difform template, then template is inserted in the glass tube, one end of electrode material utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.
(3) pre-service of little disk array electrode surface
The little disk array electrode that is cured is ground off epoxy glue unnecessary outside the glass tube earlier on flint glass paper, expose electrode surface, use α-Al of 1,0.3,0.05 μ m then successively
2O
3Electrode surface is polished polishing, with secondary water flushing electrode surface, ultrasonic 1-3 minute.
(4) sign of little disk array electrode
At the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCl of 1mol/L, potential range 0.6-0V sweeps speed for 0.01V/s, contrast electrode is Ag/AgCl.Detect whether the cyclic voltammetric figure is the S shape of standard, if be the S shape of standard, the preparation that shows this little disk array electrode is successful, can be used for actual electrochemistry experiment; If cyclic voltammogram is not the S shape for standard, continue with α-Al
2O
3The grinding and polishing electrode cleans, and is ultrasonic, presents the S shape of standard up to cyclic voltammogram.With secondary water cleaning electrode surface, recover the clean conditions of electrode itself after test finishes, electrode can be reused by grinding and polishing.
Embodiment
Embodiment 1:
The preparation of the little dish linear array of platinum electrode.Under laboratory environment, it is in 320 microns the quartz capillary that Pt silk that diameter is about 20 microns inserts external diameter, 12 quartz capillaries that are inserted with the Pt silk are put into glass tube with template is fixing after in line, one end of Pt silk utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.With the little disk Pt array electrode that is cured successively in rough sand paper and 1,0.3, α-Al of 0.05 μ m
2O
3Polish polishing, then at the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCL of 1mol/L, potential range is 0.6-0V, sweeps speed for 0.01V/s, cyclic voltammogram is the S shape of standard, the preparation that shows this little disk array electrode is successful.
Embodiment 2:
The preparation of the little dish quadrate array of platinum electrode.Under laboratory environment, it is in 320 microns the quartz capillary that Pt silk that diameter is about 20 microns inserts external diameter, put into glass tube after 16 quartz capillaries that are inserted with the Pt silk are fixed into square with template, one end of Pt silk utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.With the little disk Pt array electrode that is cured successively in rough sand paper and 1,0.3, α-Al of 0.05 μ m
2O
3Polish polishing, then at the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCL of 1mol/L, potential range is 0.6-0V, sweeps speed for 0.01V/s, cyclic voltammogram is the S shape of standard, the preparation that shows this little disk array electrode is successful.
Embodiment 3:
The preparation of the little dish disc of carbon fiber array electrode.Under laboratory environment, the carbon fiber that diameter is about 20 microns inserts in the quartz capillary of 320 microns of external diameters, put into glass tube after 16 quartz capillaries that are inserted with carbon fiber are fixed into disc with template, one end of carbon fiber utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.With the little disk array electrode of the carbon fiber that is cured successively in rough sand paper and 1,0.3, α-Al of 0.05 μ m
2O
3Polish polishing, then at the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCL of 1mol/L, potential range is 0.6-0V, sweeps speed for 0.01V/s, cyclic voltammogram is the S shape of standard, the preparation that shows this little disk array electrode is successful.
Embodiment 4:
The preparation of the little disc-annular shape array electrode of carbon fiber.Under laboratory environment, the carbon fiber that diameter is about 8 microns inserts in the quartz capillary of 270 microns of external diameters, put into glass tube after 10 quartz capillaries that are inserted with carbon fiber are fixed into annular with template, one end of carbon fiber utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.With the little disk array electrode of the carbon fiber that is cured successively in rough sand paper and 1,0.3, α-Al of 0.05 μ m
2O
3Polish polishing, then at the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCL of 1mol/L, potential range is 0.6-0V, sweeps speed for 0.01V/s, cyclic voltammogram is the S shape of standard, the preparation that shows this little disk array electrode is successful.
Embodiment 5:
The preparation of Jin Wei dish linear array electrode.Under laboratory environment, the spun gold that diameter is about 30 microns inserts in the quartz capillary of 380 microns of external diameters, 6 quartz capillaries that are inserted with spun gold are put into glass tube with template is fixing after in line, one end of spun gold utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours.With the golden little disk array electrode that is cured successively in rough sand paper and 1,0.3, α-Al of 0.05 μ m
2O
3Polish polishing, then at the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCL of 1mol/L, potential range is 0.6-0V, sweeps speed for 0.01V/s, cyclic voltammogram is the S shape of standard, the preparation that shows this little disk array electrode is successful.
Claims (1)
1. the preparation method of a little disk array electrode is characterized in that adopting following 4 steps to carry out:
(1) electrode material is inserted in the quartz capillary
With long 2cm diameter is micron order or nano level fibrous electrode material: the tinsel or the carbon fiber of platinum, gold, insert in the quartz capillary of long 1cm; The pipe wall thickness of quartz capillary should be more than 6 times of electrode material diameter;
(2) curing of electrode material and encapsulation
Many quartz capillaries that are inserted with electrode material are fixed on composition linearity, annular, disc or rectangular electrod-array in the difform template, then template is inserted in the glass tube, one end of electrode material utilizes silver conductive adhesive to connect with copper cash and draws, the other end injects the epoxy glue encapsulation, places under the room temperature and solidifies 12 hours;
(3) pre-service of little disk array electrode surface
The little disk array electrode that is cured is ground off epoxy glue unnecessary outside the glass tube earlier on flint glass paper, expose electrode surface, use α-Al of 1,0.5,0.03 μ m then successively
2O
3Electrode surface is polished polishing, with secondary water flushing electrode surface, ultrasonic 1-3 minute;
(4) sign of little disk array electrode
At the Fe of 5mmol/L (CN)
6 3-Aqueous solution in do cyclic voltammetric, supporting electrolyte is the KCl of 1mol/L, potential range 0.6-0V, sweep speed and be 0.01V/s, contrast electrode is Ag/AgCl, detects whether the cyclic voltammetric figure is the S shape of standard, if be the S shape of standard, the preparation that shows this little disk array electrode is successful; If cyclic voltammogram is not the S shape for standard, continue with α-Al
2O
3The grinding and polishing electrode cleans, and is ultrasonic, presents the S shape of standard up to cyclic voltammogram; With secondary water cleaning electrode surface, recover the clean conditions of electrode itself after test finishes, electrode can be reused by grinding and polishing.
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| CN 200310110043 CN1223849C (en) | 2003-11-17 | 2003-11-17 | Preparing method of micro disk array electrode |
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| CN 200310110043 CN1223849C (en) | 2003-11-17 | 2003-11-17 | Preparing method of micro disk array electrode |
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| CN1223849C CN1223849C (en) | 2005-10-19 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362342C (en) * | 2005-11-18 | 2008-01-16 | 武汉大学 | Method for preparing carbon fiber ultramicro disc electrode |
| CN100386621C (en) * | 2005-12-05 | 2008-05-07 | 扬州大学 | Method for manufacturing nano carbon disk electrode with radius less than 500nm |
| CN100395545C (en) * | 2006-04-28 | 2008-06-18 | 武汉大学 | Method for preparing integrated multiple ultramicro microdisc electrode |
| CN102890108A (en) * | 2012-10-11 | 2013-01-23 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
| CN102892775A (en) * | 2010-03-26 | 2013-01-23 | 科罗拉多州立大学研究基金会 | Self-assembly of coatings utilizing surface charge |
| 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 |
| CN103776883A (en) * | 2014-02-28 | 2014-05-07 | 中国科学院长春应用化学研究所 | Preparation method of integrated microarray electrode |
| CN103776884A (en) * | 2014-02-28 | 2014-05-07 | 中国科学院长春应用化学研究所 | Preparation method of integrated microarray electrode |
| CN104034773A (en) * | 2014-06-20 | 2014-09-10 | 首都师范大学 | Gold film microelectrode array and manufacture method thereof |
| CN105384138A (en) * | 2015-10-27 | 2016-03-09 | 江西科技师范大学 | Core-shell type ultra-micro electrode prepared through coaxial electrostatic spinning and preparation method thereof |
| CN111664968A (en) * | 2020-07-15 | 2020-09-15 | 襄阳臻芯传感科技有限公司 | Method for manufacturing ceramic capacitive pressure sensor |
| 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 |
-
2003
- 2003-11-17 CN CN 200310110043 patent/CN1223849C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362342C (en) * | 2005-11-18 | 2008-01-16 | 武汉大学 | Method for preparing carbon fiber ultramicro disc electrode |
| CN100386621C (en) * | 2005-12-05 | 2008-05-07 | 扬州大学 | Method for manufacturing nano carbon disk electrode with radius less than 500nm |
| CN100395545C (en) * | 2006-04-28 | 2008-06-18 | 武汉大学 | Method for preparing integrated multiple ultramicro microdisc electrode |
| 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 |
| CN102892775A (en) * | 2010-03-26 | 2013-01-23 | 科罗拉多州立大学研究基金会 | Self-assembly of coatings utilizing surface charge |
| CN102890108B (en) * | 2012-10-11 | 2014-08-27 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
| CN102890108A (en) * | 2012-10-11 | 2013-01-23 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
| CN103776883A (en) * | 2014-02-28 | 2014-05-07 | 中国科学院长春应用化学研究所 | Preparation method of integrated microarray electrode |
| CN103776884A (en) * | 2014-02-28 | 2014-05-07 | 中国科学院长春应用化学研究所 | Preparation method of integrated microarray electrode |
| CN103776884B (en) * | 2014-02-28 | 2016-03-23 | 中国科学院长春应用化学研究所 | A kind of preparation method of integrated microarray electrode |
| CN103776883B (en) * | 2014-02-28 | 2016-03-23 | 中国科学院长春应用化学研究所 | A kind of preparation method of integrated microarray electrode |
| CN104034773A (en) * | 2014-06-20 | 2014-09-10 | 首都师范大学 | Gold film microelectrode array and manufacture method thereof |
| CN104034773B (en) * | 2014-06-20 | 2017-02-01 | 首都师范大学 | Gold film microelectrode array and manufacture method thereof |
| CN105384138A (en) * | 2015-10-27 | 2016-03-09 | 江西科技师范大学 | Core-shell type ultra-micro electrode prepared through coaxial electrostatic spinning and preparation method thereof |
| CN111664968A (en) * | 2020-07-15 | 2020-09-15 | 襄阳臻芯传感科技有限公司 | Method for manufacturing ceramic capacitive pressure sensor |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN1223849C (en) | 2005-10-19 |
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