CN2632675Y - Needle three-in-one microelectrodes - Google Patents

Needle three-in-one microelectrodes Download PDF

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Publication number
CN2632675Y
CN2632675Y CN 03266018 CN03266018U CN2632675Y CN 2632675 Y CN2632675 Y CN 2632675Y CN 03266018 CN03266018 CN 03266018 CN 03266018 U CN03266018 U CN 03266018U CN 2632675 Y CN2632675 Y CN 2632675Y
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CN
China
Prior art keywords
silver
electrode
glass capillary
microelectrode
millimeters
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Expired - Fee Related
Application number
CN 03266018
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Chinese (zh)
Inventor
张君
袁倬斌
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Institute Of Applied Chemistry Graduate School Chinese Academy Of Sciences
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Institute Of Applied Chemistry Graduate School Chinese Academy Of Sciences
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Priority to CN 03266018 priority Critical patent/CN2632675Y/en
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Publication of CN2632675Y publication Critical patent/CN2632675Y/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

The utility model provides a pinhead type three in one microelectrode, which can be used for an environment which is often moved, which adopts a glass capillary (whose head outside diameter is less than 0. 150 millimeters) to insulate a micron sized filamentary silver (whose diameter is less than 0. 060 millimeters), a platinum filament (whose diameter is less then 0. 060 millimeters) and a carboform (whose diameter is less than 8 microns) then assembles the filamentary silver, the platinum filament and the carboform into a pinhead inner cavity ( whose outside diameter is less than 2. 000 millimeters), and finally welds an electrode down lead tin on three terminals of an electrode plug, thereby forming the microelectrode. Wherein, the connection of the carboform in a carboform electrode and a brass wire is realized by a secondary copper plating; the platinum filament uses melted solid paraffin to seal the two sides of the electrode glass capillary; a micro reference electrode of a micro silver or a silver chloride (Ag/Ag Cl) is realized by arranging silver or silver chloride filaments in a well drawing glass capillary and lays up a section of potassium chloride saturated solutions of the silver chloride in the glass capillary, a metrical tip diameter of the reference electrode of the silver or the silver chloride can reach 0. 018 millimeters; a steady reference electric potential can be provided in the cell measurement.

Description

The three-in-one microelectrode of needle-based
Affiliated technical field
The utility model relates to a kind of microelectrode device of electro-chemical test research, especially can provide the needle-based with stable reference potential three-in-one microelectrode.
Background technology
At present, known silver/silver chloride (Ag/AgCl) contrast electrode is to place silver/silver chloride the glass tube of a band ceramic core to form, although in the potentiometric analysis of routine, silver/silver chloride (Ag/AgCl) contrast electrode plays a significantly greater role, but its relatively large volume (external diameter is a centimetre-sized) can't satisfy the requirement of present cell (diameter 0.010-0.100 millimeter) live body, original position, online study, and the reason on the preparation method causes it to be difficult to microminiaturization again; Though directly adopt the silver electrode can reduced volume, as contrast electrode the unsettled shortcoming of current potential arranged again, so that in using conventional electrochemical method such as cyclic voltammetry, can't accurately measure.In addition, existing three-electrode structure disperses when measuring, and volume is big, and is not easy to operate.
Summary of the invention
Can not carry out the cell live body in order to overcome existing silver/silver chloride contrast electrode, original position, online electrochemical research, directly do the unstable and existing three electrode dispersion of contrast electrode current potential with filamentary silver, fragile and not easy-operating deficiency, the utility model proposes a kind of microminiaturized silver/silver chloride electrode device, adopt not only volume little (external diameter can reach 18 microns) of miniature silver/silver chloride electrode, can insert in the big cell, and can provide stable reference potential, and on this basis, adopt glass capillary to make insulator and supporter three kinds of microelectrodes, be assembled in the syringe needle (external diameter 1-2 millimeter) of a millimeter level internal diameter, be welded as a whole with the miniplug of standard, can obtain a kind of simple, the three-in-one microelectrode of easy-to-use and non-damageable needle-based.
The technical scheme that its technical matters that solves the utility model adopts is: the silver of handling with electrochemical method/silver chloride filament is packed into to be drawn in the good glass capillary, and in kapillary, seal the saturated potassium chloride solution of one section saturated silver chloride up for safekeeping, this silver/silver chloride contrast electrode can provide stable reference potential; On this basis, the employing glass capillary is as the insulator between three electrodes and support each electrode, and three electrodes are assembled in the syringe needle (external diameter 1-2 millimeter) of a millimeter level internal diameter, adopt the method for secondary copper coating and welding, reduce resistance and background noise that the traditional carbon fibres electrode adopts the conducting resinl sealing-in, improve resolution, and the way of employing and standard plug assembling welding, make it the three-in-one microelectrode of becoming one, reaching to provide stable reference potential, miniature, simple, easy-to-use and non-damageable purpose.
The beneficial effects of the utility model are, when adopting the electrochemical method three-electrode system to carry out cell measurement, adopt the miniature silver/silver chloride electrode of this method preparation that stable on-the-spot reference potential can be provided, and, further three electrodes of traditional dispersion are carried out microminiaturization and integrated, easy to use.
Description of drawings
Below in conjunction with drawings and Examples the utility model is further specified.
Fig. 1: the three-in-one microelectrode diagrammatic cross-section of needle-based.
Among Fig. 1: 1. syringe needle (head outer diameter to be good) less than 2 millimeters, 2. shell, 3. electrode plug, 4. carbon fiber (diameter to be good) less than 8 microns, 5. glass capillary, 6. copper wire, 7. electrode plug binding post, 8. platinum filament (diameter to be good) less than 0.03 millimeter, 9. saturated potassium chloride solution, 10. filamentary silver (diameter to be good) less than 0.05 millimeter, 11. by the miniature working electrode of 4,5 carbon fibers of forming, 12. miniature to electrode by 5,8 platinum of forming (Pt), 13. by 5,9,10 silver/silver chloride of forming (Ag/AgCl) miniature reference electrodes.
Embodiment:
1. the drawing of glass capillary (5): take out the glass tubule of a cleaning, both hands pinch two respectively, burning to the deliquescing that reddens on the spirit lamp flame envelope, move apart flame, elongate rapidly, are cut into suitable segment with pocket knife after cooling;
2. the assembling of the miniature working electrode of carbon fiber (11):
Choose a branch of carbon fiber and use acetone, alcohol and secondary redistilled water washed twice respectively, remove greasy dirt and dust on the carbon fiber (4), in air, dry naturally, choose the carbon fiber (4) of several 8-10 centimeter length, carry out first copper facing;
The carbon fiber that has plated copper (4) is washed three times with the secondary redistilled water, in the glass capillary (5) of packing into after drying; At the afterbody thin copper wire (6) of packing into, fully contact with the copper sheet of (4) plating on the carbon fiber, and jam-pack slightly firmly, but it is too violent to exert oneself, in case carbon fiber (4) fractures, prune the carbon fiber that exposes with little scissors afterwards, make carbon fiber (4) expose the about 2-3 millimeter of glass capillary (5) head;
Downward glass capillary (5) head that installs carbon fiber (4) and copper wire (6), in the solid paraffin that dissolves, soak, its head is sealed, because there is surface tension in fusion, thereby carbon fiber (4) tip can be exposed;
The glass capillary (5) that installs carbon fiber (4) and copper wire (6) is put into copper plating device, carry out secondary copper facing,, guarantee that the electric conductivity of electrode is good so that thin copper wire (6) contacts closely with carbon fiber (4);
With secondary redistilled water washing three times, dry the back and immerse in the solid paraffin that dissolves, afterbody is sealed;
3. the assembling of silver/silver chloride (Ag/AgCl) miniature reference electrodes (13):
Get the thin filamentary silver (10) of a 8-10 centimeter length, choose suitable glass capillary (5), filamentary silver (10) is carefully filled in the end that makes filamentary silver (10) arrive expanding end from a thicker end, but the fortress is too not tight, in case block kapillary (5) front end, then make glass capillary (5) expanding end rear portion near spirit lamp flame, carefully glass capillary (5) is bent a little right angle with pincet, the purpose at curved right angle is in order both to keep kapillary unobstructed, prevents that again filamentary silver (10) from deviating from;
Filamentary silver (10) end with the curved little hook of pincet, is hung on the chloridizing unit, and the kapillary lower end is immersed in the saturated KCl solution (9), makes the filamentary silver chlorination about 30 minutes;
The miniature assembling of 4 platinum (Pt) to electrode (12):
Get the thin platinum filament of a 8-10 centimeter length, choose suitable glass capillary (5), platinum filament is carefully packed into, and make the platinum filament tip expose kapillary front end 2 millimeter, the rear end is reserved about 3 centimetres, soaks in molten solids paraffin, makes it to seal;
5. the assembling of microneedle hair style electrochemical probe:
Get 2 millimeters of external diameters with (1) one at interior syringe needle, after with pocket knife it being handled, the miniature working electrode of carbon fiber (11) of packing into earlier bumps folding for preventing carbon fiber (4) tip, can pack into from syringe needle (1) tip, then uses little hook that copper wire (6) is carefully chosen; It is miniature to electrode (12) to reinstall platinum (Pt), and the load mode of the miniature working electrode of the same carbon fiber of load mode is for guaranteeing the straight and upright of platinum filament tip, in case collide and conducting with pinhead wall equally; At last, silver/silver chloride (Ag/AgCl) miniature reference electrodes (13) from after pack into the syringe needle, the lead-in wire of each electrode that installs is welded in respectively on each binding post (7) of electrode plug, twist good plug body (2), the electrode probe assembling finishes (diagrammatic cross-section of the three-in-one microelectrode of needle-based as shown in Figure 1)

Claims (4)

1. three-in-one microelectrode of needle-based, by silver/silver chloride (Ag/AgCl) contrast electrode, platinum filament electrode and carbon fiber working electrode are formed, it is characterized in that: adopt insulator and the stilt of glass capillary as micron-sized filamentary silver, platinum filament and carbon fiber, and be assembled in the millimetre-sized metal needle inner chamber, the lead-in wire of three electrodes is welded in respectively on the corresponding binding post of electrode plug.
2. the three-in-one microelectrode of needle-based according to claim 1, it is characterized in that: miniature silver/silver chloride (Ag/AgCl) contrast electrode is silver/silver chloride filament of handling with electrochemical method to be packed into draw in the good glass capillary, and seals the saturated potassium chloride solution of one section saturated silver chloride in kapillary up for safekeeping.
3. the three-in-one microelectrode of needle-based according to claim 1 is characterized in that: the carbon fiber of carbon fiber working electrode and being connected of copper wire are to realize through the secondary copper plating treatment, and with the solid paraffin that melts to the glass capillary sealing two ends.
4. the three-in-one microelectrode of needle-based according to claim 1 is characterized in that: the dress platinum filament seals with the solid paraffin fusing the glass capillary two ends of electrode.
CN 03266018 2003-06-25 2003-06-25 Needle three-in-one microelectrodes Expired - Fee Related CN2632675Y (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 03266018 CN2632675Y (en) 2003-06-25 2003-06-25 Needle three-in-one microelectrodes

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 03266018 CN2632675Y (en) 2003-06-25 2003-06-25 Needle three-in-one microelectrodes

Publications (1)

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CN2632675Y true CN2632675Y (en) 2004-08-11

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103499623A (en) * 2013-09-03 2014-01-08 西安建筑科技大学 Composite N2O selective microelectrode and preparation method thereof
CN109187696A (en) * 2018-08-06 2019-01-11 上海交通大学 The acquisition of electrochemical sensor and density of hydrogen and the foundation of hydrogen treating mode

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103499623A (en) * 2013-09-03 2014-01-08 西安建筑科技大学 Composite N2O selective microelectrode and preparation method thereof
CN103499623B (en) * 2013-09-03 2015-12-23 西安建筑科技大学 A kind of combined type N 2o selects microelectrode and preparation method thereof
CN109187696A (en) * 2018-08-06 2019-01-11 上海交通大学 The acquisition of electrochemical sensor and density of hydrogen and the foundation of hydrogen treating mode

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