CN103364467B - Based on the microelectrode array and preparation method thereof of vaseline - Google Patents
Based on the microelectrode array and preparation method thereof of vaseline Download PDFInfo
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- CN103364467B CN103364467B CN201310308645.7A CN201310308645A CN103364467B CN 103364467 B CN103364467 B CN 103364467B CN 201310308645 A CN201310308645 A CN 201310308645A CN 103364467 B CN103364467 B CN 103364467B
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Abstract
The invention discloses a kind of microelectrode array based on vaseline and preparation method thereof.The method, comprises the steps: glass-carbon electrode, and after diamond electrode or other carbon-based material electrode pre-service, solution a or b is evenly coated in the surface of described electrode, drying obtains described microelectrode array; In described solution a, solute is vaseline, and solvent is ether; In described mixed liquor b, solute is vaseline and tin indium oxide, and solvent is ether.The method is easy, effectively, can obtain a microelectrode array in several minutes; And the microelectrode array dimension adjustable obtained, there is important using 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 being 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, record in 2001. that microelectrode array has high mass transfer rate, small time constant, low IR fall, the feature 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 composed in parallel by multiple microelectrode, adopt microelectrode array, both by electrode amplification detection signal in parallel while keeping single microelectrode excellent properties, the reliability of total measurement can be improved again by the redundancy increasing sensor.
At present, the method that prepared by microelectrode array mainly contains etching method and template.The most frequently used etching method has Soft lithograph technology, it is the general name of micro-contact printing, duplicating molded, microtransfer molding, Micromolding in Capillaries etc., although this method can be applied on the surface of various material and different chemical character, for distortion, the distortion of such as elastomeric stamp; The high precision overlay alignment of small scale submissile gonosome, prepares the compatibility etc. that complicated multilayer pattern and electronic chip are processed, still needs to carry out deep research and development.So far, the research work of the adjustable nano-indium stannum oxide microelectrode array of preparation size is not yet had to occur.
Summary of the invention
The object 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 made up of conductive substrates and array layer;
Described array layer is positioned on described conductive substrates, and partly or entirely covers the surface of described conductive substrates;
When described array layer part covers described conductive substrates surperficial, described array layer is made up of vaseline;
When described array layer all covers described conductive substrates surperficial, described array layer is made up of vaseline and conducting nanoparticles, and described conducting nanoparticles is evenly distributed in described vaseline.
In above-mentioned array, described conductive substrates is carbon-based electrode;
Described carbon-based electrode is specially glass-carbon electrode or diamond electrode;
Described conducting nanoparticles is selected from least one in tin indium oxide, nano carbon microsphere and nano-metal particle;
The particle diameter of described conducting nanoparticles is 30-80nm, is specially 40-60nm.
The mass ratio of described vaseline and conducting nanoparticles 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 is evenly coated in the surface of carbon-based electrode, drying obtains described microelectrode array;
In described solution a, solute is vaseline, and solvent is ether;
In described solution b, solute is vaseline and conducting nanoparticles, and solvent is ether.
In said method, described carbon-based electrode is glass-carbon electrode or diamond electrode; Described conducting nanoparticles is selected from least one in tin indium oxide, nano carbon microsphere and 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;
In described solution b, the mass ratio of vaseline and conducting nanoparticles is 5-15:1-2, is specially 8-12:0.7-1.2, is more specifically 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, is more specifically 80mg/mL, 85mg/mL or 80-85mg/mL.
The particle diameter of described conducting nanoparticles is 30-80nm, is specially 40-60nm or 50nm or 50-60nm or 40-50nm.
The method of described coating can be various conventional method, as dipped, spin coating etc.;
In described method, comprised the steps: before surface solution a or b being evenly coated in carbon-based electrode
A, be alumina powder polishing on polishing cloth of 1.0 μm, 0.3 μm and 0.05 μm successively with particle diameter by described carbon-based electrode;
B, by the ultrasonic cleaning in intermediate water of the carbon-based electrode after polishing;
C, by the carbon-based electrode after ultrasonic cleaning at 0.1molL
-1potassium ferricyanide solution in, between-0.4 and+0.7V, carry out cyclic voltammetry scan, until obtain typical cyclic voltammetric spectrogram, namely complete the pre-service of described carbon-based electrode.
In said method, because solution a or b is evenly coated in carbon-based electrode surface, and namely ether to volatilize removing at last drying steps, leaves the nano conducting powders such as vaseline and/or nano-indium stannum oxide and stays electrode surface.In the method for the invention a, vaseline is insulator, when due to ether volatilization, part is covered by vaseline carbon electrodes, the part of naked leakage can as electrode generation electrochemical reaction, and by SI semi-insulation that vaseline covers, therefore electrochemical reaction can not occur, therefore electrochemical region locally occur and defines microelectrode, a lot of local microelectrode areal distribution just define microelectrode array in whole plane;
In 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 time, nano conducting powders is embedded in vaseline insulation course, and the aggregate of each nano conducting powders or several nano conducting powders can as a microelectrode generation electrochemical reaction, and petrolatum layer around then plays insulating effect, come isolated for each microelectrode, form microelectrode array.
The microelectrode array prepared according to the method described above, also belongs to protection scope of the present invention.
The present invention is in conjunction with the good plasticity of vaseline and the good electric conductivity of the nano conducting powders such as insulativity and nano-indium stannum oxide, and the potpourri constructing a kind of variable concentrations vaseline or vaseline and nano-indium stannum oxide prepares the method for microelectrode array.In the method, tin indium oxide is as electric conductor, and vaseline is as insulator, and ether is as the spreading agent of tin indium oxide and vaseline and solvent.Gained microelectrode array has two kinds of structures, and one is that electrode surface part is covered by vaseline, and unlapped part can as electrode generation electrochemical reaction; Another kind of structural formula electrode surface is all covered by vaseline, but is evenly inlaid with indium tin oxide nanoparticles in vaseline.
Compared with the conventional method, method involved in the present invention is easy, effectively, can obtain a microelectrode array in several minutes; And the microelectrode array dimension adjustable obtained, there is important using value.
Accompanying drawing explanation
Fig. 1 is the process schematic based on the microelectrode array of vaseline and preparation method thereof in the present invention;
Fig. 2 is the cyclic voltammetric phenogram of embodiment 1 gained microelectrode array.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.
Microelectrode array preparation method provided by the invention is the microelectrode array and preparation method thereof based on vaseline.Its concrete principle is as follows:
Shown in figure as left in Fig. 1, first vaseline is dissolved in the solution formed in ether is designated as a solution, then the glass-carbon electrode handled well is dipped a solution, electrode surface ether is dried, the glassy carbon electrode surface part dipping a solution is covered by vaseline, forms microelectrode array model;
Or, as shown at right, vaseline is dissolved in after in ether and adds nano indium oxide tin particles again, concussion ultrasonic disperse is even, the dispersion liquid formed is designated as b mixed liquor, then the glass-carbon electrode handled well is dipped b mixed liquor respectively, electrode surface ether is dried, glassy carbon electrode surface, by vaseline and tin indium oxide potpourri uniform fold, forms the model of microelectrode array.
Embodiment 1:
The first step, the pre-service of glass-carbon electrode
A, be alumina powder polishing on polishing cloth of 1.0 μm, 0.3 μm and 0.05 μm successively with particle diameter by glass-carbon electrode;
B, by the ultrasonic cleaning in intermediate water of the glass-carbon electrode after polishing;
C, by the glass-carbon electrode after ultrasonic cleaning at 0.1molL
-1potassium ferricyanide solution in, between-0.4 and+0.7V, carry out cyclic voltammetry scan, until obtain typical cyclic voltammetric spectrogram, namely complete 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:
Vaseline is dissolved in ether, and concentration is 20mg/ml, and the solution formed is designated as a solution.
The nano indium oxide tin particles being 50nm vaseline and particle diameter is dissolved in ether, and the concentration of vaseline is 80mg/ml, and the concentration of nano-indium stannum oxide is 8mg/ml, and concussion ultrasonic disperse is even, and the dispersion liquid of formation is designated as b solution.
3rd step, electrode modification:
Glass-carbon electrode good for pre-service is dipped respectively a solution and each 1 second of b solution.
4th step, pole drying:
By modify complete electrode under uniform temperature condition in or auxiliary nitrogen blow condition under allow solvent ether volatilize, obtain two kinds of microelectrode arrays provided by the invention.
Wherein, the microelectrode array dipping a solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer that part covers described conductive substrates surface forms;
The microelectrode array dipping b solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer all covering conductive substrates surface forms; Described array layer is made up of vaseline and conducting nanoparticles nano-indium stannum oxide particle, and conducting nanoparticles nano-indium stannum oxide uniform particles is distributed in 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 the invention described above provided put into 0.1mol L respectively
-1the pH value of the potassium ferricyanide is in the phosphate buffer solution of 7.0, adopts three-electrode system, utilizes cyclic voltammetry to carry out cyclic voltammetry scan between-0.4 and+0.7V, measures the variation tendency of electric current with voltage.
Impedance method is utilized to measure the change 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 change of sweeping speed, presents typical microelectrode electrochemical behavior.
Embodiment 2:
According to the step of embodiment 1.Only the concentration of a solution is replaced with 25mg/ml;
B solution configures as follows and obtains: the nano indium oxide tin particles being 60nm vaseline and particle diameter is dissolved in ether, the concentration of vaseline is 85mg/ml, the concentration of nano-indium stannum oxide is 8mg/ml, and concussion ultrasonic disperse is even, and the dispersion liquid of formation is designated as b solution.
This embodiment is prepared in gained two kinds of microelectrode arrays, and the microelectrode array dipping a solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer that part covers described conductive substrates surface forms;
The microelectrode array dipping b solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer all covering conductive substrates surface forms; Array layer is made up of vaseline and conducting nanoparticles nano-indium stannum oxide particle, and conducting nanoparticles nano-indium stannum oxide uniform particles is distributed in 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 gained two kinds of microelectrode arrays and Fig. 1, without substantive difference, repeat no more.
Embodiment 3:
According to the step of embodiment 1.Only the concentration of a solution is replaced with 18mg/ml;
B solution configures as follows and obtains: the nano indium oxide tin particles being 40nm vaseline and particle diameter is dissolved in ether, the concentration of vaseline is 85mg/ml, the concentration of nano-indium stannum oxide is 9mg/ml, and concussion ultrasonic disperse is even, and the dispersion liquid of formation is designated as b solution.
This embodiment is prepared in gained two kinds of microelectrode arrays, and the microelectrode array dipping a solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer that part covers described conductive substrates surface forms;
The microelectrode array dipping b solution gained is by conductive substrates glass-carbon electrode and to be positioned on conductive substrates and the array layer all covering conductive substrates surface forms; Array layer is made up of vaseline and conducting nanoparticles nano-indium stannum oxide particle, and conducting nanoparticles nano-indium stannum oxide uniform particles is distributed in 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 gained two kinds of microelectrode arrays and Fig. 1, without substantive difference, repeat no more.
Claims (14)
1. a microelectrode array, is made up of conductive substrates and array layer;
Described array layer is positioned on described conductive substrates, and covers the surface of described conductive substrates; Described array layer is two kinds;
A kind of array layer is made up of vaseline; Described array layer is obtained by solution a; In described solution a, solute is vaseline, and solvent is ether; The concentration of described solution a is 10-30mg/mL;
Another kind of array layer is made up of vaseline and conducting nanoparticles, and described conducting nanoparticles is evenly distributed in described vaseline; Described array layer is obtained by solution b;
In described solution b, solute is vaseline and conducting nanoparticles, and solvent is ether; The concentration of vaseline in described solution b is 50-100mg/mL.
2. array according to claim 1, is characterized in that: described conductive substrates is carbon-based electrode;
Described conducting nanoparticles is selected from least one in tin indium oxide, nano carbon microsphere and nano-metal particle;
The particle diameter of described conducting nanoparticles is 30-80nm.
3. array according to claim 2, is characterized in that: described carbon-based electrode is glass-carbon electrode or diamond electrode;
The particle diameter of described conducting nanoparticles is 40-60nm.
4., according to the arbitrary described array of claim 1-3, it is characterized in that: the mass ratio of described vaseline and conducting nanoparticles is 5-15:1-2.
5. array according to claim 4, is characterized in that: the mass ratio of described vaseline and conducting nanoparticles is 8-12:0.7-1.2.
6. make a method for microelectrode array, comprise the steps:
Solution a or b is evenly coated in the surface of carbon-based electrode, drying obtains described microelectrode array;
In described solution a, solute is vaseline, and solvent is ether;
In described solution b, solute is vaseline and conducting nanoparticles, and solvent is ether.
7. method according to claim 6, is characterized in that: described carbon-based electrode is glass-carbon electrode or diamond electrode;
Described conducting nanoparticles is selected from least one in tin indium oxide, nano carbon microsphere and nano-metal particle.
8. method according to claim 6, is characterized in that: the concentration of described solution a is 10-30mg/mL;
In described solution b, the mass ratio of vaseline and conducting nanoparticles is 5-15:1-2.
9. method according to claim 8, is characterized in that: the concentration of described solution a is 18-25mg/mL;
In described solution b, the mass ratio of vaseline and conducting nanoparticles is 8-12:0.7-1.2.
10. method according to claim 6, is characterized in that: the concentration of described vaseline in described solution b is 50-100mg/mL.
11. methods according to claim 10, is characterized in that: the concentration of described vaseline in described solution b is 70-90mg/mL.
12. methods according to claim 6, is characterized in that: the particle diameter of described conducting nanoparticles is 30-80nm.
13. methods according to claim 12, is characterized in that: the particle diameter of described conducting nanoparticles is 40-60nm.
14., according to the arbitrary described method of claim 6-13, is characterized in that: in described method, comprised the steps: before surface solution a or b being evenly coated in carbon-based electrode
A, be alumina powder polishing on polishing cloth of 1.0 μm, 0.3 μm and 0.05 μm successively with particle diameter by described carbon-based electrode;
B, by the ultrasonic cleaning in intermediate water of the carbon-based electrode after polishing;
C, by the carbon-based electrode after ultrasonic cleaning at 0.1molL
-1potassium ferricyanide solution in, between-0.4 and+0.7V, carry out cyclic voltammetry scan, until obtain typical cyclic voltammetric spectrogram, namely complete 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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