CN103364467A - Vaseline-based microelectrode array and its manufacturing method - Google Patents
Vaseline-based microelectrode array and its manufacturing method Download PDFInfo
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- CN103364467A CN103364467A CN2013103086457A CN201310308645A CN103364467A CN 103364467 A CN103364467 A CN 103364467A CN 2013103086457 A CN2013103086457 A CN 2013103086457A CN 201310308645 A CN201310308645 A CN 201310308645A CN 103364467 A CN103364467 A CN 103364467A
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Abstract
The invention discloses a Vaseline-based microelectrode array and its manufacturing method. The method comprises the following steps: pretreating a glassy carbon electrode, diamond electrode or other carbon-based material electrode, uniformly coating a solution a or b on the surface of the electrode, and drying to obtain the microelectrode array. In the solution a, a solute is vaseline and a solvent is ether. In the mixed liquor b, a solute contains vaseline and indium tin oxide and a solvent is ether. The method is simple and effective. By the adoption of the method, a microelectrode array can be prepared within several minutes. In addition, the size of the obtained microelectrode array is adjustable. The microelectrode array has important application value.
Description
Technical field
The invention belongs to microelectrode and microelectrode array field, relate to a kind of microelectrode array based on vaseline and preparation method thereof.
Background technology
Ultramicroelectrode and array thereof are owing to having many good electric chemical characteristics that are different from conventional electrodes, list of references ［ 1 ］ A.J.Bard, L.R.Faulkner, Electrochemical Methods:Fundamentals and Applications, second ed., John Wiley and Sons Inc., New York, 2001. middle record microelectrode array have high mass transfer rate, hour between constant, low IR fall, the characteristics such as high s/n ratio, high current density, be the Disciplinary Frontiers of galvanochemistry and analytical chemistry always, and be widely used in a lot of fields.Tiny array electrode is to be composed in parallel by a plurality of microelectrodes, adopt microelectrode array, both can by electrode amplification detection signal in parallel when keeping single microelectrode excellent properties, can improve the reliability of total measurement by the redundancy that increases sensor again.
At present, the method for microelectrode array preparation mainly contains etching method and template.The most frequently used etching method has soft lithographic technique, it is the general name of micro-contact printing, duplicating molded, the little molding of transfer, Micromolding in Capillaries etc., although this method can be used on the surface of various materials and different chemical character, for distortion, the distortion such as elastomeric stamp; The little elastomeric high precision alignment of small scale is aimed at, and prepares the compatibility of complicated multilayer pattern and electronic chip processing etc., still needs to carry out deep research and development.So far, not yet there is the research work of the adjustable nano-indium stannum oxide microelectrode array of preparation size to occur.
Summary of the invention
The purpose of this invention is to provide a kind of microelectrode array based on vaseline and preparation method thereof.
Microelectrode array provided by the invention is comprised of conductive substrates and array layer;
Described array layer is positioned on the described conductive substrates, and partly or entirely covers the surface of described conductive substrates;
During the described conductive substrates of described array layer partial coverage surperficial, described array layer is comprised of vaseline;
When described array layer all covered described conductive substrates surperficial, described array layer was comprised of vaseline and electrical-conductive nanometer particle, and described electrical-conductive nanometer particle is evenly distributed in the described vaseline.
In the above-mentioned array, described conductive substrates is carbon-based electrode;
Described carbon-based electrode is specially glass-carbon electrode or diamond electrode;
Described electrical-conductive nanometer particle is selected from least a in tin indium oxide, nano carbon microsphere and the nano-metal particle;
The particle diameter of described electrical-conductive nanometer particle is 30-80nm, is specially 40-60nm.
The mass ratio of described vaseline and electrical-conductive nanometer particle is 5-15:1-2, is specially 8-12:0.7-1.2.
The method of making microelectrode array provided by the invention comprises the steps:
Solution a or b evenly are coated in the surface of carbon-based electrode, drying obtains described microelectrode array;
Among the described solution a, solute is vaseline, and solvent is ether;
Among the described solution b, solute is vaseline and electrical-conductive nanometer particle, and solvent is ether.
In the said method, described carbon-based electrode is glass-carbon electrode or diamond electrode; Described electrical-conductive nanometer particle is selected from least a in tin indium oxide, nano carbon microsphere and the nano-metal particle.
The concentration of described solution a is 10-30mg/mL, is specially 20mg/mL, 18-20mg/mL, 20-25mg/mL or 18-25mg/mL;
Among the described solution b, the mass ratio of vaseline and electrical-conductive nanometer particle is 5-15:1-2, is specially 8-12:0.7-1.2, more specifically is 8:0.75,8:0.8,8:0.85,8:0.75-0.85,8:0.75-0.8 or 8:0.8-0.85;
The concentration of vaseline in described solution b is 50-100mg/mL, is specially 70-90mg/mL, more specifically is 80mg/mL, 85mg/mL or 80-85mg/mL.
The particle diameter of described electrical-conductive nanometer particle is 30-80nm, is specially 40-60nm or 50nm or 50-60nm or 40-50nm.
The method of described coating can be various methods commonly used, as dip, spin coating etc.;
In the described method, before the surface that solution a or b evenly is coated in carbon-based electrode, comprise the steps:
A, be that the alumina powder of 1.0 μ m, 0.3 μ m and 0.05 μ m polishes at polishing cloth with particle diameter successively with described carbon-based electrode;
B, the carbon-based electrode ultrasonic cleaning in intermediate water after will polishing;
C, with the carbon-based electrode after the ultrasonic cleaning at 0.1molL
-1Potassium ferricyanide solution in ,-0.4 and+carry out cyclic voltammetry scan between the 0.7V, until obtain typical cyclic voltammetric spectrogram, namely finish the pre-service of described carbon-based electrode.
In the said method, because solution a or b evenly are coated in the carbon-based electrode surface, and ether namely volatilizees at last drying steps and removes, and stays the nano conducting powderses such as vaseline and/or nano-indium stannum oxide and stays electrode surface.Among the method for the invention a, vaseline is insulator, when carbon electrodes is partly covered by vaseline owing to the ether volatilization, the part of naked leakage can be used as electrode generation electrochemical reaction, and the SI semi-insulation that is covered by vaseline, therefore electrochemical reaction can not occur, therefore the electrochemical zone of local generation has formed microelectrode, and a lot of local microelectrode areal distribution have just formed microelectrode array on whole plane;
Among the method for the invention b, vaseline is insulator, the nano conducting powderses such as nano-indium stannum oxide are conductors, when both compounds are coated on electrode surface, nano conducting powders is embedded in the vaseline insulation course, and the aggregate of each nano conducting powders or several nano conducting powderses can be as a microelectrode generation electrochemical reaction, and petrolatum layer on every side then plays insulating effect, come each microelectrode is isolated, form microelectrode array.
The microelectrode array for preparing according to the method described above also belongs to protection scope of the present invention.
The present invention has made up the method that a kind of potpourri with variable concentrations vaseline or vaseline and nano-indium stannum oxide prepares microelectrode array in conjunction with vaseline good plasticity and the good electric conductivity of the nano conducting powderses such as insulativity and nano-indium stannum oxide.In the method, tin indium oxide is as electric conductor, and vaseline is as insulator, and ether is as spreading agent and the solvent of tin indium oxide and vaseline.The gained microelectrode array has two kinds of structures, and a kind of is that the electrode surface part is covered by vaseline, and unlapped part can be used as electrode generation electrochemical reaction; Another kind of structural formula electrode surface is all covered by vaseline, but evenly is inlaid with the tin indium oxide nano particle in the vaseline.
Compare with existing method, method involved in the present invention is easy, effectively, can make a microelectrode array in several minutes; And the microelectrode array dimension adjustable that obtains has important using value.
Description of drawings
Fig. 1 is based on the process schematic diagram of microelectrode array of vaseline and preparation method thereof among the present invention;
Fig. 2 is the cyclic voltammetric phenogram of embodiment 1 gained microelectrode array.
Embodiment
The present invention is further elaborated below in conjunction with specific embodiment, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.Described starting material all can get from open commercial sources if no special instructions.
Microelectrode array preparation method provided by the invention is based on microelectrode array of vaseline and preparation method thereof.Its concrete principle is as follows:
Shown in the left figure of Fig. 1, first vaseline is dissolved in the solution that forms in the ether and is designated as a solution, then the glass-carbon electrode of handling well is dipped a solution, the electrode surface ether is dried, the glass-carbon electrode surface portion of dipping a solution is covered by vaseline, forms the microelectrode array model;
Perhaps, as shown at right, again add nano indium oxide tin particles after being dissolved in the ether to vaseline, shake ultrasonic being uniformly dispersed, the dispersion liquid that forms is designated as the b mixed liquor, then the glass-carbon electrode of handling well is dipped respectively the b mixed liquor, and the electrode surface ether is dried, the glass-carbon electrode surface is formed the model of microelectrode array by vaseline and tin indium oxide potpourri uniform fold.
Embodiment 1:
The first step, the pre-service of glass-carbon electrode
A, be that the alumina powder of 1.0 μ m, 0.3 μ m and 0.05 μ m polishes at polishing cloth with particle diameter successively with glass-carbon electrode;
B, the glass-carbon electrode ultrasonic cleaning in intermediate water after will polishing;
C, with the glass-carbon electrode after the ultrasonic cleaning at 0.1molL
-1Potassium ferricyanide solution in ,-0.4 and+carry out cyclic voltammetry scan between the 0.7V, until obtain typical cyclic voltammetric spectrogram, namely finish the pre-service of described glass-carbon electrode, obtain a clean glass-carbon electrode.
Second step, configuration vaseline solution and vaseline/tin indium oxide mixed liquor:
In vaseline dissolving ether, concentration is 20mg/ml, and formed solution is designated as a solution.
Be vaseline and particle diameter that the nano indium oxide tin particles of 50nm is dissolved in the ether, the concentration of vaseline is 80mg/ml, and the concentration of nano-indium stannum oxide is 8mg/ml, shakes ultrasonic being uniformly dispersed, and the dispersion liquid of formation is designated as b solution.
The 3rd step, electrode modification:
The glass-carbon electrode that pre-service is good was dipped respectively a solution and b solution each 1 second.
The 4th step, pole drying:
The electrode that modification is complete blows at the lower or auxiliary nitrogen of uniform temperature condition and allows solvent ether volatilize under the condition, obtains two kinds of microelectrode arrays provided by the invention.
Wherein, the microelectrode array of dipping a solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer on the described conductive substrates of partial coverage surface forms;
The microelectrode array of dipping b solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer that all covers the conductive substrates surface forms; Described array layer is comprised of vaseline and electrical-conductive nanometer particle nano-indium stannum oxide particle, and electrical-conductive nanometer particle nano-indium stannum oxide uniform particles is distributed in the vaseline.
Wherein, the particle diameter of nano indium oxide tin particles is 50nm; The mass ratio of vaseline and nano-indium stannum oxide is 80:8;
Two kinds of microelectrode arrays that the invention described above provides are put into respectively 0.1mol L
-1The pH value of the potassium ferricyanide is in 7.0 the phosphate buffer solution, adopts three-electrode system, utilize cyclic voltammetry-0.4 and+carry out cyclic voltammetry scan between the 0.7V, measure electric current with the variation tendency of voltage.
Utilize impedance method to measure the variation of different modifying method rear electrode surface electronic transfer resistance.
Acquired results as shown in Figure 2.As seen from the figure, the steady-state response electric current of microelectrode array does not change along with the variation of sweeping speed, presents typical microelectrode electrochemical behavior.
Embodiment 2:
Step according to embodiment 1.Only the concentration with a solution replaces with 25mg/ml;
B solution configures as follows and gets: be vaseline and particle diameter that the nano indium oxide tin particles of 60nm is dissolved in the ether, the concentration of vaseline is 85mg/ml, the concentration of nano-indium stannum oxide is 8mg/ml, shakes ultrasonic being uniformly dispersed, and the dispersion liquid of formation is designated as b solution.
This embodiment prepares in two kinds of microelectrode arrays of gained, and the microelectrode array of dipping a solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer on the described conductive substrates of partial coverage surface forms;
The microelectrode array of dipping b solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer that all covers the conductive substrates surface forms; Array layer is comprised of vaseline and electrical-conductive nanometer particle nano-indium stannum oxide particle, and electrical-conductive nanometer particle nano-indium stannum oxide uniform particles is distributed in the vaseline.
Wherein, the particle diameter of nano indium oxide tin particles is 60nm; The mass ratio of vaseline and nano-indium stannum oxide is 85:8;
The cyclic voltammetric phenogram of two kinds of microelectrode arrays of gained and Fig. 1 repeat no more without substantive difference.
Embodiment 3:
Step according to embodiment 1.Only the concentration with a solution replaces with 18mg/ml;
B solution configures as follows and gets: be vaseline and particle diameter that the nano indium oxide tin particles of 40nm is dissolved in the ether, the concentration of vaseline is 85mg/ml, the concentration of nano-indium stannum oxide is 9mg/ml, shakes ultrasonic being uniformly dispersed, and the dispersion liquid of formation is designated as b solution.
This embodiment prepares in two kinds of microelectrode arrays of gained, and the microelectrode array of dipping a solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer on the described conductive substrates of partial coverage surface forms;
The microelectrode array of dipping b solution gained is by the conductive substrates glass-carbon electrode and be positioned on the conductive substrates and the array layer that all covers the conductive substrates surface forms; Array layer is comprised of vaseline and electrical-conductive nanometer particle nano-indium stannum oxide particle, and electrical-conductive nanometer particle nano-indium stannum oxide uniform particles is distributed in the vaseline.
Wherein, the particle diameter of nano indium oxide tin particles is 40nm; The mass ratio of vaseline and nano-indium stannum oxide is 85:9;
The cyclic voltammetric phenogram of two kinds of microelectrode arrays of gained and Fig. 1 repeat no more without substantive difference.
Claims (9)
1. a microelectrode array is comprised of conductive substrates and array layer;
Described array layer is positioned on the described conductive substrates, and partly or entirely covers the surface of described conductive substrates;
During the described conductive substrates of described array layer partial coverage surperficial, described array layer is comprised of vaseline;
When described array layer all covered described conductive substrates surperficial, described array layer was comprised of vaseline and electrical-conductive nanometer particle, and described electrical-conductive nanometer particle is evenly distributed in the described vaseline.
2. array according to claim 1, it is characterized in that: described conductive substrates is carbon-based electrode;
Described carbon-based electrode is specially glass-carbon electrode or diamond electrode;
Described electrical-conductive nanometer particle is selected from least a in tin indium oxide, nano carbon microsphere and the nano-metal particle;
The particle diameter of described electrical-conductive nanometer particle is 30-80nm, is specially 40-60nm.
3. array according to claim 1 and 2, it is characterized in that: the mass ratio of described vaseline and electrical-conductive nanometer particle is 5-15:1-2, is specially 8-12:0.7-1.2.
4. a method of making microelectrode array comprises the steps:
Solution a or b evenly are coated in the surface of carbon-based electrode, drying obtains described microelectrode array;
Among the described solution a, solute is vaseline, and solvent is ether;
Among the described solution b, solute is vaseline and electrical-conductive nanometer particle, and solvent is ether.
5. method according to claim 4, it is characterized in that: described carbon-based electrode is glass-carbon electrode or diamond electrode;
Described electrical-conductive nanometer particle is selected from least a in tin indium oxide, nano carbon microsphere and the nano-metal particle.
6. according to claim 4 or 5 described methods, it is characterized in that: the concentration of described solution a is 10-30mg/mL, is specially 18-25mg/mL;
Among the described solution b, the mass ratio of vaseline and electrical-conductive nanometer particle is 5-15:1-2, is specially 8-12:0.7-1.2.
7. arbitrary described method according to claim 4-6, it is characterized in that: the concentration of described vaseline in described solution b is 50-100mg/mL, is specially 70-90mg/mL.
8. arbitrary described method according to claim 4-7, it is characterized in that: the particle diameter of described electrical-conductive nanometer particle is 30-80nm, is specially 40-60nm.
9. arbitrary described method according to claim 4-8 is characterized in that: in the described method, comprised the steps: before the surface that solution a or b evenly is coated in carbon-based electrode
A, be that the alumina powder of 1.0 μ m, 0.3 μ m and 0.05 μ m polishes at polishing cloth with particle diameter successively with described carbon-based electrode;
B, the carbon-based electrode ultrasonic cleaning in intermediate water after will polishing;
C, with the carbon-based electrode after the ultrasonic cleaning at 0.1molL
-1Potassium ferricyanide solution in ,-0.4 and+carry out cyclic voltammetry scan between the 0.7V, until obtain typical cyclic voltammetric spectrogram, namely finish the pre-service of described carbon-based electrode.
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| CN101804960A (en) * | 2010-01-13 | 2010-08-18 | 西安交通大学 | Ultra-fine cone electrode array and method for manufacturing same |
| US20110125001A1 (en) * | 2009-11-25 | 2011-05-26 | Weileun Fang | 3d microelectrode structure and method for assembling the same |
| CN103101878A (en) * | 2013-02-28 | 2013-05-15 | 中国科学院半导体研究所 | Method for preparing silicon-based microelectrode |
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- 2013-07-22 CN CN201310308645.7A patent/CN103364467B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5468366A (en) * | 1992-01-15 | 1995-11-21 | Andcare, Inc. | Colloidal-gold electrosensor measuring device |
| CN1837808A (en) * | 2006-04-22 | 2006-09-27 | 福州大学 | Microfluidic chip electrode for electrochemical detection and method for manufacturing microfluidic chip |
| US20110125001A1 (en) * | 2009-11-25 | 2011-05-26 | Weileun Fang | 3d microelectrode structure and method for assembling the same |
| CN101804960A (en) * | 2010-01-13 | 2010-08-18 | 西安交通大学 | Ultra-fine cone electrode array and method for manufacturing same |
| CN103101878A (en) * | 2013-02-28 | 2013-05-15 | 中国科学院半导体研究所 | Method for preparing silicon-based microelectrode |
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