CN202075263U - Device for detecting electrochemical performance of lead powder based on ultramicroelectrodes - Google Patents
Device for detecting electrochemical performance of lead powder based on ultramicroelectrodes Download PDFInfo
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- CN202075263U CN202075263U CN2011201296461U CN201120129646U CN202075263U CN 202075263 U CN202075263 U CN 202075263U CN 2011201296461 U CN2011201296461 U CN 2011201296461U CN 201120129646 U CN201120129646 U CN 201120129646U CN 202075263 U CN202075263 U CN 202075263U
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Abstract
Aiming at the limitation of the traditional lead powder performance detecting method, the utility model provides a device for detecting the electrochemical performance of lead powder based on ultramicroelectrodes, which greatly increases the detecting efficiency. The device comprises a counter electrode, a reference electrode, a working electrode and an electrolytic cell, wherein the electrolytic cell is internally filled with electrolyte; one ends of the counter electrode, the reference electrode and the working electrode are all inserted in the electrolytic cell; and the working electrode is a micropore electrode with micron-sized and is internally filled with lead powder as an active substance. High-efficiency electrochemistry detecting information can be obtained at low cost by using the device which has rapid signal response, high sensitivity and low detection limit. Through the device, capacitive property, cycle performance and other information of the lead powder can be directly obtained, and the traditional device for detecting the electrochemical performance of the lead powder for producing finished batteries is possible to be replaced.
Description
Technical field
The utility model belongs to electrochemical techniques, is specifically related to a kind of lead powder chemical property pick-up unit based on ultramicroelectrode.
Background technology
Lead-acid accumulator is a kind of ancient secondary cell, the development course that has experienced so far surplus in the of 150 year from invention, even to this day, its dominate still in secondary battery industry.The lead-acid battery electrode active material that at present domestic most lead-acid accumulator manufacturing enterprise adopts is a lead powder, and its composition is meant by 70%～80% PbO and 20%～30% free plumbous (Pb, PbO
2And Pb
3O
4) potpourri formed.
Because the appearance of modern electrochemical detection method is later than the application of lead-acid accumulator, therefore be later than the application of battery itself far away about the Electrochemical Properties of lead powder.The lead-acid accumulator industry belongs to typically the field of " use afterwards earlier and study ".At present, the general finished product battery of making earlier of existing method, its capacity of back test, cycle indicator etc.This class methods technological process is long, and manufacturing process is disturbed easily, and the consumption of lead powder amount is big.
Ultramicroelectrode is meant that one dimension is of a size of a micron or a nano level class electrode.It was invented the sixties in last century, and after this developing rapidly becomes field, electrochemical forward position.It has advantages such as high steady-state current density, high electronics mass transfer rate, high s/n ratio, low detection material consumption, signal response are fast, sensitivity height.In recent years, the ultramicroelectrode technology has obtained bigger progress in the application exploration in fields, forward position such as Optical Electro-Chemistry, bioelectrochemistry and biomedicine.Specifically the application in scanning microtechnic, biosensor technology, spectroelectrochemistry, trace materials mensuration, biological cell analysis etc. has promoted material science, nano science, medical science, biological fast development greatly.
In the prior art, application few people research or the report of ultramicroelectrode in lead-acid accumulator galvanochemistry.Yet, in field of batteries, great at the Research Significance of the redox reaction mechanism of electrode active material, reversibility, cyclical stability, interface performance etc.Detect based on the lead powder chemical property of ultramicroelectrode and can be lead-acid accumulator direct electrochemical theory foundation is provided, greatly enrich the battery electrochemical content in lead-acid accumulator field.
Summary of the invention
The utility model provides a kind of lead powder chemical property pick-up unit based on ultramicroelectrode at the limitation of existing lead powder method for testing performance, has improved detection efficiency greatly.
The lead powder chemical property pick-up unit that the utility model provides based on ultramicroelectrode, it is characterized in that, this device comprises electrode, contrast electrode, working electrode and electrolytic tank, be marked with electrolytic solution in the electrolytic tank, end to electrode, contrast electrode and working electrode all inserts electrolytic tank, working electrode is the micro-porous electrode of μ m level yardstick, is filled with lead powder in it as active substance.
The utlity model has following advantage:
(1) the utility model provides a kind of lead powder chemical property pick-up unit based on ultramicroelectrode at the limitation of existing lead powder method for testing performance, and the sacrificial electrode active substance is few, and signal response is fast, and is highly sensitive, and detectability is low, the detection efficiency height.
(2) use the chemical property of ultramicroelectrode test lead powder, need not to make the finished product battery, shorten test period, reduced in the battery manufacturing process solidifies, change into, the interference of adjuvant etc., the real-time detection between realization electrode active material and the chemical property.
(3) the utility model is simple in structure, can save electrode material, effectively reduces the cost of high-efficient detection.
(4) the utility model device can directly connect electrochemical workstation, implements the Electrochemical Detection of cyclic voltammetric, AC impedance, corrosive nature etc.These detections can obtain lead powder capacity, cycle performance etc. rapidly.
Description of drawings
The structural representation of the pick-up unit that Fig. 1 provides for the utility model;
Fig. 2 is the structural representation of micropore working electrode among Fig. 1.
Embodiment
Below by by accompanying drawing and example the utility model being described in further detail, but following examples only are illustrative, and protection domain of the present utility model is not subjected to the restriction of these embodiment.
As shown in Figure 1, the pick-up unit that the utility model provides comprises electrode 2, contrast electrode 3, working electrode 4 and electrolytic tank 5, be marked with electrolytic solution 6 in the electrolytic tank 5, end to electrode 2, contrast electrode 3 and working electrode 4 all inserts electrolytic tank 5, in working electrode 4, be filled with active substance 7, active substance is object to be detected, as lead powder.
Electrode 2 is adopted monolithic or biplate inert electrode (as: platinized platinum electrode, gold plaque electrode), and surface area is much larger than working electrode.Simultaneously, close as far as possible for reducing the internal resistance of cell to electrode and working electrode, about 1 cm.Contrast electrode 3 adopts the mereurous sulfate electrode.Detection cell is sealable special-purpose there-necked flask or the electrolytic tank that is used for Electrochemical Detection.Three electrodes place electrolytic tank 5, and its spacing is fixed by the pitch-row of electrolytic tank lid.
As shown in Figure 2, the structure of working electrode 4 is: the end of electrode body 44 is by epoxy resin 42 sealings, it in it vacuum chamber 43, one end of platinum microfilament 45 passes vacuum chamber 43 and extend out to outside the electrode body 44, the other end links to each other with copper conductor 41, and the end that copper conductor 41 links to each other with platinum microfilament 45 is encapsulated in the epoxy resin 42.After electrode completes, place little chloroazotic acid that boils to corrode 15～60 min, the aperture can be used after suitable as required.Zhi Bei micro-porous electrode yardstick is a μ m level by this method, belongs to ultramicroelectrode.
Example:
It is that the platinum microfilament 45 of 100 μ m is electric transmission carrier, electrode body 44 adopting quartz glass pipes that diameter is chosen in the making of micropore research electrode.Platinum filament leading portion landfill advances in the vitreum, and front end must stretch out (as indicating among the figure), and vitreum need polish smooth after pressing and burying; The platinum filament stage casing vacuumizes encapsulation in the glass tube of diameter 1 cm, length is 8 cm; The platinum filament back segment links to each other with copper conductor 41 in the blacking part, and with epoxy resin 42 encapsulation firmly.Electrode places the hole that obtains suitable size behind little chloroazotic acid corrosion 45 min that boil, and cleans, oven dry can use.
During detection, with a small amount of active substance 7(powder to be measured or lotion) place on the flat glass plate, directly hold working electrode 4 and on determinand, mill repeatedly, it can be embedded in the micropore, be used for electro-chemical test.
Three-electrode system is connected on the electrochemical workstation 1, carries out the test of cyclic voltammetric (CV) and electrochemical impedance (PEIS).The test parameter of CV test can be dE/dt=0.1～100 mV/s, 20 mV/s optimums; E
i=-1.2V, E
f=2.0V.The parameter of PEIS test can be Vpp=20mV, frequency range 200 KHz～50 mHz.
Carry out the cyclic voltammogram that the CV test can obtain different lead powder by the utility model, relatively the size at its redox peak can obtain the volumetric properties information of different lead powder.Simultaneously, a certain lead powder is carried out repeatedly the CV test, the volume change after can repeatedly circulating by lead powder obtains its cycle performance information.
Confirmed the said advantage of the utility model after testing, obtained the high-level efficiency Electrochemical Detection information under low-cost, signal response is fast, and is highly sensitive, and detectability is low.
The above is preferred embodiment of the present utility model, but the utility model should not be confined to the disclosed content of this embodiment and accompanying drawing.So everyly do not break away from the equivalence of finishing under the spirit disclosed in the utility model or revise, all fall into the scope of the utility model protection.
Claims (3)
1. lead powder chemical property pick-up unit based on ultramicroelectrode, it is characterized in that, this device comprises electrode (2), contrast electrode (3), working electrode (4) and electrolytic tank (5), be marked with electrolytic solution (6) in the electrolytic tank (5), end to electrode (2), contrast electrode (3) and working electrode (4) all inserts electrolytic tank (5), working electrode (4) is the micro-porous electrode of μ m level yardstick, is filled with lead powder in it as active substance (7).
2. the lead powder chemical property pick-up unit based on ultramicroelectrode according to claim 1 is characterized in that, electrode (2) is adopted monolithic or biplate inert electrode, and its surface area is much larger than the surface area of working electrode (4).
3. the lead powder chemical property pick-up unit based on ultramicroelectrode according to claim 1 and 2, it is characterized in that, the structure of working electrode (4) is: the end of electrode body (44) is sealed by epoxy resin (42), it in it vacuum chamber (43), one end of platinum microfilament (45) passes vacuum chamber (43) and extend out to outside the electrode body (44), the other end links to each other with copper conductor (41), and the end that copper conductor (41) links to each other with platinum microfilament (45) is encapsulated in the epoxy resin (42).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201296461U CN202075263U (en) | 2011-04-28 | 2011-04-28 | Device for detecting electrochemical performance of lead powder based on ultramicroelectrodes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201296461U CN202075263U (en) | 2011-04-28 | 2011-04-28 | Device for detecting electrochemical performance of lead powder based on ultramicroelectrodes |
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|---|---|
| CN202075263U true CN202075263U (en) | 2011-12-14 |
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|---|---|---|---|
| CN2011201296461U Expired - Lifetime CN202075263U (en) | 2011-04-28 | 2011-04-28 | Device for detecting electrochemical performance of lead powder based on ultramicroelectrodes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424782A (en) * | 2015-12-22 | 2016-03-23 | 湖北金洋冶金股份有限公司 | Lead powder electrochemical performance detection method based on small polar plate and test system therefor |
| CN106990157A (en) * | 2017-02-20 | 2017-07-28 | 骆驼集团襄阳蓄电池有限公司 | A kind of detection method of lead bullion material and its application |
-
2011
- 2011-04-28 CN CN2011201296461U patent/CN202075263U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424782A (en) * | 2015-12-22 | 2016-03-23 | 湖北金洋冶金股份有限公司 | Lead powder electrochemical performance detection method based on small polar plate and test system therefor |
| CN106990157A (en) * | 2017-02-20 | 2017-07-28 | 骆驼集团襄阳蓄电池有限公司 | A kind of detection method of lead bullion material and its application |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20111214 |