CN103776884A - Preparation method of integrated microarray electrode - Google Patents
Preparation method of integrated microarray electrode Download PDFInfo
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- CN103776884A CN103776884A CN201410071940.XA CN201410071940A CN103776884A CN 103776884 A CN103776884 A CN 103776884A CN 201410071940 A CN201410071940 A CN 201410071940A CN 103776884 A CN103776884 A CN 103776884A
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Abstract
The invention provides a preparation method of an integrated microarray electrode, which comprises the following steps: inserting a first electrode material into glass capillaries to obtain first glass capillaries; sealing a second electrode material to one end of a first thin glass tube by fusing, adding a first conducting medium from the other end, and sealing by connecting with a first wire to obtain a reference electrode and counter electrode; and inserting the reference electrode and counter electrode and the first glass capillaries into a glass tube, filling a glass product in the gap, filling a second conducting medium, and sealing by connecting with a second wire to obtain the integrated microarray electrode. Compared with the prior art, the glass-tube-packagedd integrated microarray electrode is integrated and convenient to use, and has fixed electrode gap and small sample batch detection test errors; and by adopting glass tube packaging, the prepared microarray electrode has the advantages of high corrosion resistance, high stain resistance and favorable stability. The reference electrode and counter electrode is integrated, and thus, the integrated microarray electrode is simple to manufacture and convenient to maintain.
Description
Technical field
The invention belongs to Technology of Microelectrodes field, relate in particular to a kind of preparation method of integrated microarray electrode.
Background technology
Microelectrode refers to the electrode that is at least less than 25 μ m in unidimensional scale, and this yardstick is called critical dimension.Now can prepare the little electrode to 0.1 μ m of critical dimension, the electrode that critical dimension is less is commonly called nano electrode.Owing to will possessing the character of microelectrode, electrode only need to be enough little just passable in a dimension, so microelectrode can have many shapes: modal is micro-disk electrode, is that to be encapsulated in by tinsel the interface obtaining in insulator be discoid microelectrode; In addition, also have micro-strip electrode, be encapsulated in insulator and obtain by metal forming; Micro-cylinder electrode, simply exposes one end tinsel or carbon fiber and obtains.
With respect to the electrode of stock size, small-sized microelectrode has advantages of a lot of unusual.The steady-state current density of microelectrode is better than the electric current of conventional electrodes under forced convertion, and meanwhile, the steady-state current of microelectrode calculates by theory and laboratory facilities all obtain than being easier to.As prerequisite, the work of much studying dynamics or reaction mechanism is all take microelectrode as basis, as: the small size that research stock size electrode cannot be approaching or the live body in little space detect; Effects on surface carries out imaging, as scan-type electrochemical microscope; Be used for glitch-free detection/the monitor variation of other electroactive surface electroactive materials.
Tiny array electrode refers to by multiple microelectrodes and integrates formed electrode, and its electric current is the algebraic sum of each unitary electrode electric current.Tiny array electrode has kept the characteristic of original unitary electrode, can obtain again larger strength of current, and conventional electrochemical apparatus can detect its signal, is conducive to analytical applications.
H.X.He(Langmuir16, 2000, 9684) by the method for soft printing stencil, H.Kaden(Electrochem.Commun.2, 2000, 606) with exact instrument, electrode material is sealed in and in epoxy resin, prepares micro-array electrode, but above-mentioned preparation method needs special exact instrument, cost is higher, common lab is difficult to preparation, and wire electrode stochastic distribution, easily cause the overlapping of electric capacity between adjacent electrode and diffusion, cause micro-array electrode to present the electrochemical behavior of conventional large electrode, lose the good characteristic of microelectrode, and after each test, surface is difficult to process.
Publication number is the preparation method that the Chinese patent of CN1544928A discloses micro-array electrode, it makes array electrode with quartz capillary encapsulated electrode material, but the method curing materials is epoxy resin, it can also make golden tiny array electrode, but electrode very easily pollutes, limit its range of application.
At present, three-electrode system generally adopts the working electrode, contrast electrode of dispersion and to electrode composition, very inconvenient for the measurement in roving environment, and distance between electrode is also difficult for fixingly, causes larger error.It is silver/silver chloride to be placed in to a glass tube with ceramic core make that generally acknowledged silver/silver chloride (Ag/AgCl) contrast electrode has a kind of, and in method, kind electrode easily pollutes, and easy cleaning not; And directly adopt filamentary silver to have the unsettled shortcoming of current potential as contrast electrode, so that cannot accurately measure in the time using conventional electrochemical method as cyclic voltammetry.
Application number is that the Chinese patent of ZL03137469.7 discloses a kind of preparation method of compound microelectrode and Chinese patent that application number is ZL03266018.9 discloses needle three-in-one microelectrodes, in these two patents, mention three electrodes have been compounded in to one, although there is lot of advantages and purposes widely, but three electrodes are just simply assembled together, and do not organically blend.Detection electric current on microelectrode is conventionally in nA level, detects so little electric current very high to the requirement of detecting device, in actual applications, and because the electric current of single microelectrode is less than the detection lower limit of conventional electrochemical apparatus sometimes, so application is restricted.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of integrated microarray electrode, and integrated microarray electrode prepared by the method is easy to use and stability is better.
The preparation method who the invention provides a kind of integrated microarray electrode, comprises the following steps:
The first electrode material is injected in glass capillary, obtain the first glass capillary; The length of length L EssT.LTssT.LT first electrode material of described glass capillary;
The second electrode material sealing by fusing, in one end of thin glass tube, is then added to the first conducting medium from the other end, connect the first wire, by the thin glass tube sealing connecting after the first wire, obtain contrast electrode and hold concurrently to electrode; Or the second electrode material is injected in thin glass tube, seal after then the second electrode material being drawn to thin glass tube, obtain contrast electrode and hold concurrently to electrode;
Described contrast electrode is held concurrently electrode and many described the first glass capillaries are injected in glass tube, and described the first glass capillary, described contrast electrode are held concurrently and are adopted glassware to fill to the space between electrode and described glass tube, obtain the first glass tube; The length that described in the length L EssT.LTssT.LT of described the first glass capillary, described in the length L EssT.LTssT.LT of glass tube, contrast electrode is held concurrently to electrode;
By filling described the first glass tube the second conducting medium, connect the second wire, by the first glass tube sealing connecting after the second wire, obtain integrated microarray electrode.
Preferably, the internal diameter of described glass capillary is less than or equal to 3 times of the first electrode material diameter.
Preferably, the pipe thickness of described glass capillary is greater than 3 times of the first electrode material radius.
Preferably, described the first electrode material and the second electrode material are fibrous electrodes material.
Preferably, described the first electrode material is one or more in carbon fiber, platinum, gold, copper, palladium, silver, nickel, iridium, iron, tin oxide and indium oxide.
Preferably, described the second electrode material is platinum, platinum black or carbon.
Preferably, described the first conducting medium and the second conducting medium are dag, silver powder or conducting resinl independently of one another.
Preferably, described glassware is glass bar, glass dust or glass tube.
Preferably, after the first electrode material is injected in glass capillary, also comprise:
By one end end-blocking of the glass capillary of reeve the first electrode material.
Preferably, by after the first glass tube sealing connecting after the second wire, also comprise:
Adopt ultrasound wave to process, obtain integrated microarray electrode.
The preparation method who the invention provides a kind of integrated microarray electrode, comprises the following steps: the first electrode material is injected in glass capillary, obtain the first glass capillary; The length of length L EssT.LTssT.LT first electrode material of described glass capillary; The second electrode material sealing by fusing, in one end of thin glass tube, is then added to the first conducting medium from the other end, connect the first wire, by the thin glass tube sealing connecting after the first wire, obtain contrast electrode and hold concurrently to electrode; Or the second electrode material is injected in thin glass tube, seal after then the second electrode material being drawn to thin glass tube, obtain contrast electrode and hold concurrently to electrode; Described contrast electrode is held concurrently electrode and many described the first glass capillaries are injected in glass tube, and described the first glass capillary, described contrast electrode are held concurrently and are adopted glassware to fill to the space between electrode and described glass tube, obtain the first glass tube; The length that described in the length L EssT.LTssT.LT of described the first glass capillary, described in the length L EssT.LTssT.LT of glass tube, contrast electrode is held concurrently to electrode; By filling described the first glass tube the second conducting medium, connect the second wire, by the first glass tube sealing connecting after the second wire, obtain integrated microarray electrode.Compared with prior art, first, the present invention all adopts the glass tube encapsulation and integration array electrode that declines, thereby it is integrated in one, easy to use, and electrode separation fixes, and it is less that sample batch detects test error, meanwhile, the encapsulation of employing glass tube makes the tiny array electrode of preparation corrosion-resistant, resistance tocrocking is strong, stability is better; Secondly, the present invention is prepared as contrast electrode by the second electrode material and holds concurrently to electrode, makes simple, easy to maintenance; Again, the electric current of integrated microarray electrode is large compared with microelectrode, and sensitivity is higher.
Accompanying drawing explanation
Fig. 1 is the structural representation of the integrated microarray electrode for preparing of the embodiment of the present invention 1;
Fig. 2 is electric current-frequency curve figure of the integrated microarray electrode for preparing of the embodiment of the present invention 1.
Embodiment
The preparation method who the invention provides a kind of integrated microarray electrode, comprises the following steps:
The first electrode material is injected in glass capillary, obtain the first glass capillary; The length of length L EssT.LTssT.LT first electrode material of described glass capillary;
The second electrode material sealing by fusing, in one end of thin glass tube, is then added to the first conducting medium from the other end, connect the first wire, by the thin glass tube sealing connecting after the first wire, obtain contrast electrode and hold concurrently to electrode; Or the second electrode material is injected in thin glass tube, seal after then the second electrode material being drawn to thin glass tube, obtain contrast electrode and hold concurrently to electrode;
Described contrast electrode is held concurrently electrode and many described the first glass capillaries are injected in glass tube, and described the first glass capillary, described contrast electrode are held concurrently and are adopted glassware to fill to the space between electrode and described glass tube, obtain the first glass tube; The length that described in the length L EssT.LTssT.LT of described the first glass capillary, described in the length L EssT.LTssT.LT of glass tube, contrast electrode is held concurrently to electrode;
By filling described the first glass tube the second conducting medium, connect the second wire, by the first glass tube sealing connecting after the second wire, obtain integrated microarray electrode.
According to the present invention, the first electrode material is injected in glass capillary, obtain the first glass capillary.Wherein, described the first electrode material is preferably fibrous electrodes material; Described the first electrode material is electrode material well known to those skilled in the art, and the present invention is preferably one or more in carbon fiber, platinum, gold, copper, palladium, silver, nickel, iridium, iron, tin oxide and indium oxide.Adopt different electrode materials can make the tiny array electrode that performance is different; The internal diameter of described glass capillary is preferably greater than the diameter of the first electrode material, and is less than or equal to 3 times of the first electrode material diameter; The pipe thickness of described glass capillary is preferably the more than 3 times of the first electrode material radius.
In the present invention, after the first electrode material is injected in glass capillary, preferably by one end end-blocking of the glass capillary of reeve the first electrode material.The method of described end-blocking is method well known to those skilled in the art, is preferably heating and melting end-blocking.Because the length of glass capillary is less than the length of the first electrode material, therefore after end-blocking, obtain the first glass capillary that one end end-blocking, the other end the first electrode material expose.
The second electrode material sealing by fusing, in one end of thin glass tube, is then added to the first conducting medium from the other end.Wherein, described the second electrode material is preferably fibrous electrodes material; Described the second electrode material is contrast electrode and the electrode material to electrode of can be used as well known to those skilled in the art, there is no special restriction, and the present invention is preferably platinum, platinum black or carbon; Described the first conducting medium is conducting medium well known to those skilled in the art, there is no special restriction, and the present invention is preferably dag, silver powder or conducting resinl.
Add after the first conducting medium, connect the first wire, described the first wire is wire well known to those skilled in the art, there is no special restriction, is preferably copper wire in the present invention.By the thin glass tube sealing connecting after the first wire, obtain contrast electrode and hold concurrently to electrode.Described sealing preferably adopts sealed membrane to seal.
According to the present invention, described contrast electrode is held concurrently and also can be adopted following methods to be prepared to electrode: the second electrode material is injected in thin glass tube, seal after then the second electrode material being drawn to thin glass tube, obtain contrast electrode and hold concurrently to electrode.The method directly adopts second electrode material of whole to draw thin glass tube, without adding conducting medium.
Many described the first glass capillaries and described contrast electrode are held concurrently in electrode reeve glass tube, and described the first glass capillary, described contrast electrode are held concurrently and are adopted glassware to fill to the space between electrode and described glass tube, thereby obtain the first glass tube.Wherein, described glassware is preferably glass bar, glass dust or glass tube, holds concurrently to electrode in order to fix the first glass capillary and contrast electrode.In the present invention preferably between many first glass capillary electrode materials, the first glass capillary and the double radius that spacing between electrode electrode material is greater than to first electrode material of 6 times of contrast electrode.If the spacing between described electrode material is too small, easily cause the diffusion closing between electrode overlapping, cause integrated microarray electrode to present the electrochemical behavior of large electrode.
According to the present invention, the preparation method of described the first glass tube is specially: many described the first glass capillaries and described contrast electrode are held concurrently in electrode reeve glass tube, described the first glass capillary, described contrast electrode is held concurrently and is adopted glassware to fill to the space between electrode and described glass tube, by the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently electrode is flushed with glass tube, and by described glass tube, described the first glass capillary melts end-blocking with the double one end that electrode is flushed of described contrast electrode, vacuumize, and from end-blocking to upper end heating and melting, with after annealing, cooling, obtain the first glass tube.In the process of above-mentioned preparation the first glass tube, described heating and melting with described in the operation that vacuumizes be all in order to prevent that air is enclosed in glass tube, thereby affect electrode performance.
Obtain after the first glass tube, filling the second conducting medium in described the first glass tube, connects the second wire, by the first glass tube sealing connecting after the second wire, obtains integrated microarray electrode.Wherein, described the second conducting medium is conducting medium well known to those skilled in the art, there is no special restriction, is preferably dag, silver powder or conducting resinl in the present invention; Described the second wire is preferably copper wire or copper rod.
According to the present invention, by after the first glass tube sealing connecting after the second wire, preferably also carry out ultrasound wave processing.Ultrasound wave processing can make conducting medium tightly packed, strengthens electric conductivity, reduces measuring-signal noise.
In the present invention, obtain after integrated microarray electrode, preferably carried out pre-service.Described pretreated step is specially: integrated microarray electrode, successively with 600 orders, 1200 orders, 2000 order 3000 orders, 5000 orders and 7000 object abrasive paper for metallograph is from coarse to fine that end face is polished to cunning, is then used to α-Al of 0.5 μ m and 0.03 μ m successively
2o
3on polishing sponge cloth, electrode surface is polished, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1～3min, can carry out performance test by integrated microarray electrode.
The present invention all adopts the glass tube encapsulation and integration array electrode that declines, thereby it is integrated in one, easy to use, and electrode separation is fixed, it is less that sample batch detects test error, meanwhile, the encapsulation of employing glass tube makes the tiny array electrode of preparation corrosion-resistant, resistance tocrocking is strong, stability is better; In addition, the present invention is prepared as contrast electrode by the second electrode material and holds concurrently to electrode, makes simple, easy to maintenance; And the electric current of integrated microarray electrode is large compared with microelectrode, sensitivity is higher.
In order to further illustrate the present invention, below in conjunction with embodiment, the preparation method of a kind of integrated microarray electrode provided by the invention is described in detail.
In following examples, agents useful for same is commercially available.
1.1 get one section of raw glass pipe, clean successively glass tube inside and outside wall by ethanol, secondary deionized water, dry, and gaslight heating is drawn into glass capillary (more than wall thickness 100 μ m), is cut into 15mm segment, obtains glass capillary; The platinum filament that is 20 μ m by diameter is cut into the long segment of 20mm, pierces in glass capillary, and one section of heating and melting end-blocking, obtains the first glass capillary.
1.2 at one section of platinum filament of thin glass tube one end sealing by fusing (Φ=1.0mm), adds dag from the other end, contacts with the platinum filament exposing in thin glass tube, then copper wire is inserted in dag as the first wire, with sealed membrane sealing, obtains contrast electrode and holds concurrently to electrode.
1.3 arrange by difformity the first glass capillary obtaining in many 1.1 fill in (external diameter 4mm in the glass tube cleaning up in advance, internal diameter 3mm, long 7cm) in, the contrast electrode that also has preparation in 1.2 inserting in the lump in glass tube is held concurrently to electrode, with the full space of empty glass tube filling of not wearing platinum filament, to guarantee that position is fixed each other, the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently concordant with glass tube to electrode, platinum filament indentation 3mm, with spirit lamp by glass tube, the double thin glass tube melting end-blocking to electrode of the first glass capillary and contrast electrode, the other end inserts syringe needle, seal with sealed membrane, connect vacuum pump, vacuumize, start to upper end heating and melting from end-blocking, annealing, cooling rear filling dag, insertion copper rod is drawn, sealing compound sealing, ultrasound wave processing makes dag tightly packed.Clip melted ends 3mm with glass cutter after cooling, use successively 600 orders, 2000 orders, 3000 orders, 5000 orders and 7000 order abrasive paper for metallograph by thick to carefully by interface polishing, " 8 " font alternating direction is milled, and prevents electrode mill partially, then uses successively α-Al of 0.5 μ m and 0.03 μ m
2o
3on polishing sponge cloth, electrode surface is polished into minute surface, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1min, obtains integrated microarray electrode.
Fig. 1 is the schematic diagram of the integrated microarray electrode that obtains in 1.3.Wherein, 1 is the first wire copper wire; 2 is thin glass tube; 3 is dag; 4 is platinum filament; 5 is micron order platinum filament; 6 is dag; 7 is glass tube; 8 is the second wire copper rod.
The integrated microarray electrode obtaining in 1.3 is measured to its current value (value while getting 10s) in 25mM potassium ferrocyanide (0.1M KCl solution is as supporting electrolyte) solution, obtain the electric current-frequency curve of this integrated microarray electrode, as shown in Figure 2.This integrated microarray electrode pair sample batch detection test error is less as seen from Figure 2.
2.1 get one section of raw glass pipe, clean successively glass tube inside and outside wall by ethanol, secondary deionized water, dry, and gaslight heating is drawn into glass capillary (more than wall thickness 100 μ m), is cut into 15mm segment, obtains glass capillary; The carbon fiber that is 7 μ m by diameter is cut into the long segment of 20mm, pierces in glass capillary, and one section of heating and melting end-blocking, obtains the first glass capillary.
2.2 at one section of platinum filament of thin glass tube one end sealing by fusing (Φ=1.0mm), adds dag from the other end, contacts with the platinum filament exposing in thin glass tube, then copper wire is inserted in dag as the first wire, with sealed membrane sealing, obtains contrast electrode and holds concurrently to electrode.
2.3 arrange by difformity the first glass capillary obtaining in many 2.1 fill in (external diameter 4mm in the glass tube cleaning up in advance, internal diameter 3mm, long 7cm) in, the contrast electrode that also has preparation in 2.2 inserting in the lump in glass tube is held concurrently to electrode, with the full space of empty glass tube filling of not wearing carbon fiber, to guarantee that position is fixed each other, the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently concordant with glass tube to electrode, carbon fiber indentation 3mm, with spirit lamp by glass tube, the double thin glass tube melting end-blocking to electrode of the first glass capillary and contrast electrode, the other end inserts syringe needle, seal with sealed membrane, connect vacuum pump, vacuumize, start to upper end heating and melting from end-blocking, annealing, cooling rear filling dag, insertion copper rod is drawn, sealing compound sealing, ultrasound wave processing makes dag tightly packed.Clip melted ends 3mm with glass cutter after cooling, use successively 600 orders, 2000 orders, 3000 orders, 5000 orders and 7000 order abrasive paper for metallograph by thick to carefully by interface polishing, " 8 " font alternating direction is milled, and prevents electrode mill partially, then uses successively α-Al of 0.5 μ m and 0.03 μ m
2o
3on polishing sponge cloth, electrode surface is polished into minute surface, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1min, obtains integrated microarray electrode.
3.1 get one section of raw glass pipe, clean successively glass tube inside and outside wall by ethanol, secondary deionized water, dry, and gaslight heating is drawn into glass capillary (more than wall thickness 100 μ m), is cut into 15mm segment, obtains glass capillary; The palladium silk that is 10 μ m by diameter is cut into the long segment of 20mm, pierces in glass capillary, and one section of heating and melting end-blocking, obtains the first glass capillary.
3.2 at one section of platinum filament of thin glass tube one end sealing by fusing (Φ=1.0mm), adds dag from the other end, contacts with the platinum filament exposing in thin glass tube, then copper wire is inserted in dag as the first wire, with sealed membrane sealing, obtains contrast electrode and holds concurrently to electrode.
3.3 arrange by difformity the first glass capillary obtaining in many 3.1 fill in (external diameter 4mm in the glass tube cleaning up in advance, internal diameter 3mm, long 7cm) in, the contrast electrode that also has preparation in 3.2 inserting in the lump in glass tube is held concurrently to electrode, with the full space of empty glass tube filling of not wearing palladium silk, to guarantee that position is fixed each other, the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently concordant with glass tube to electrode, palladium silk indentation 3mm, with spirit lamp by glass tube, the double thin glass tube melting end-blocking to electrode of the first glass capillary and contrast electrode, the other end inserts syringe needle, seal with sealed membrane, connect vacuum pump, vacuumize, start to upper end heating and melting from end-blocking, annealing, cooling rear filling dag, insertion copper rod is drawn, sealing compound sealing, ultrasound wave processing makes dag tightly packed.Clip melted ends 3mm with glass cutter after cooling, use successively 600 orders, 2000 orders, 3000 orders, 5000 orders and 7000 order abrasive paper for metallograph by thick to carefully by interface polishing, " 8 " font alternating direction is milled, and prevents electrode mill partially, then uses successively α-Al of 0.5 μ m and 0.03 μ m
2o
3on polishing sponge cloth, electrode surface is polished into minute surface, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1min, obtains integrated microarray electrode.
4.1 get one section of raw glass pipe, clean successively glass tube inside and outside wall by ethanol, secondary deionized water, dry, and gaslight heating is drawn into glass capillary (more than wall thickness 100 μ m), is cut into 15mm segment, obtains glass capillary; The spun gold that is 25 μ m by diameter is cut into the long segment of 20mm, pierces in glass capillary, and one section of heating and melting end-blocking, obtains the first glass capillary.
4.2 at one section of platinum filament of thin glass tube one end sealing by fusing (Φ=1.0mm), adds dag from the other end, contacts with the platinum filament exposing in thin glass tube, then copper wire is inserted in dag as the first wire, with sealed membrane sealing, obtains contrast electrode and holds concurrently to electrode.
4.3 arrange by difformity the first glass capillary obtaining in many 4.1 fill in (external diameter 4mm in the glass tube cleaning up in advance, internal diameter 3mm, long 7cm) in, the contrast electrode that also has preparation in 4.2 inserting in the lump in glass tube is held concurrently to electrode, with the full space of empty glass tube filling of not wearing spun gold, to guarantee that position is fixed each other, the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently concordant with glass tube to electrode, spun gold indentation 3mm, with spirit lamp by glass tube, the double thin glass tube melting end-blocking to electrode of the first glass capillary and contrast electrode, the other end inserts syringe needle, seal with sealed membrane, connect vacuum pump, vacuumize, start to upper end heating and melting from end-blocking, annealing, cooling rear filling dag, insertion copper rod is drawn, sealing compound sealing, ultrasound wave processing makes dag tightly packed.Clip melted ends 3mm with glass cutter after cooling, use successively 600 orders, 2000 orders, 3000 orders, 5000 orders and 7000 order abrasive paper for metallograph by thick to carefully by interface polishing, " 8 " font alternating direction is milled, and prevents electrode mill partially, then uses successively α-Al of 0.5 μ m and 0.03 μ m
2o
3on polishing sponge cloth, electrode surface is polished into minute surface, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1min, obtains integrated microarray electrode.
5.1 get one section of raw glass pipe, clean successively glass tube inside and outside wall by ethanol, secondary deionized water, dry, and gaslight heating is drawn into glass capillary (more than wall thickness 100 μ m), is cut into 15mm segment, obtains glass capillary; The filamentary silver that is 15 μ m by diameter is cut into the long segment of 20mm, pierces in glass capillary, and one section of heating and melting end-blocking, obtains the first glass capillary.
5.2 at one section of platinum filament of thin glass tube one end sealing by fusing (Φ=1.0mm), adds dag from the other end, contacts with the platinum filament exposing in thin glass tube, then copper wire is inserted in dag as the first wire, with sealed membrane sealing, obtains contrast electrode and holds concurrently to electrode.
5.3 arrange by difformity the first glass capillary obtaining in many 5.1 fill in (external diameter 4mm in the glass tube cleaning up in advance, internal diameter 3mm, long 7cm) in, the contrast electrode that also has preparation in 5.2 inserting in the lump in glass tube is held concurrently to electrode, with the full space of empty glass tube filling of not wearing filamentary silver, to guarantee that position is fixed each other, the first glass capillary of end-blocking, the contrast electrode of end-blocking is held concurrently concordant with glass tube to electrode, filamentary silver indentation 3mm, with spirit lamp by glass tube, the double thin glass tube melting end-blocking to electrode of the first glass capillary and contrast electrode, the other end inserts syringe needle, seal with sealed membrane, connect vacuum pump, vacuumize, start to upper end heating and melting from end-blocking, annealing, cooling rear filling dag, insertion copper rod is drawn, sealing compound sealing, ultrasound wave processing makes dag tightly packed.Clip melted ends 3mm with glass cutter after cooling, use successively 600 orders, 2000 orders, 3000 orders, 5000 orders and 7000 order abrasive paper for metallograph by thick to carefully by interface polishing, " 8 " font alternating direction is milled, and prevents electrode mill partially, then uses successively α-Al of 0.5 μ m and 0.03 μ m
2o
3on polishing sponge cloth, electrode surface is polished into minute surface, be finally placed on respectively ethanol and secondary deionized water ultrasonic cleaning three times, each 1min, obtains integrated microarray electrode.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for integrated microarray electrode, is characterized in that, comprises the following steps:
The first electrode material is injected in glass capillary, obtain the first glass capillary; The length of length L EssT.LTssT.LT first electrode material of described glass capillary;
The second electrode material sealing by fusing, in one end of thin glass tube, is then added to the first conducting medium from the other end, connect the first wire, by the thin glass tube sealing connecting after the first wire, obtain contrast electrode and hold concurrently to electrode; Or the second electrode material is injected in thin glass tube, seal after then the second electrode material being drawn to thin glass tube, obtain contrast electrode and hold concurrently to electrode;
Described contrast electrode is held concurrently electrode and many described the first glass capillaries are injected in glass tube, and described the first glass capillary, described contrast electrode are held concurrently and are adopted glassware to fill to the space between electrode and described glass tube, obtain the first glass tube; The length that described in the length L EssT.LTssT.LT of described the first glass capillary, described in the length L EssT.LTssT.LT of glass tube, contrast electrode is held concurrently to electrode;
By filling described the first glass tube the second conducting medium, connect the second wire, by the first glass tube sealing connecting after the second wire, obtain integrated microarray electrode.
2. preparation method according to claim 1, is characterized in that, the internal diameter of described glass capillary is less than or equal to 3 times of the first electrode material diameter.
3. preparation method according to claim 1, is characterized in that, the pipe thickness of described glass capillary is greater than 3 times of the first electrode material radius.
4. preparation method according to claim 1, is characterized in that, described the first electrode material and the second electrode material are fibrous electrodes material.
5. preparation method according to claim 1, is characterized in that, described the first electrode material is one or more in carbon fiber, platinum, gold, copper, palladium, silver, nickel, iridium, iron, tin oxide and indium oxide.
6. preparation method according to claim 1, is characterized in that, described the second electrode material is platinum, platinum black or carbon.
7. preparation method according to claim 1, is characterized in that, described the first conducting medium and the second conducting medium are dag, silver powder or conducting resinl independently of one another.
8. preparation method according to claim 1, is characterized in that, described glassware is glass bar, glass dust or glass tube.
9. preparation method according to claim 1, is characterized in that, after the first electrode material is injected in glass capillary, also comprises:
By one end end-blocking of the glass capillary of reeve the first electrode material.
10. preparation method according to claim 1, is characterized in that, by after the first glass tube sealing connecting after the second wire, also comprises:
Adopt ultrasound wave to process, obtain integrated microarray electrode.
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| CN111505071A (en) * | 2020-04-13 | 2020-08-07 | 商丘师范学院 | Integrated microelectrode sensor for simultaneous detection of pH and AA and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5380422A (en) * | 1991-07-18 | 1995-01-10 | Agency Of Industrial Science And Technology | Micro-electrode and method for preparing it |
| 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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| US5380422A (en) * | 1991-07-18 | 1995-01-10 | Agency Of Industrial Science And Technology | Micro-electrode and method for preparing it |
| 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 |
| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111505071A (en) * | 2020-04-13 | 2020-08-07 | 商丘师范学院 | Integrated microelectrode sensor for simultaneous detection of pH and AA and preparation method and application thereof |
| 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 |
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