CN110887782A - Working electrode for corrosion detection and preparation method thereof - Google Patents
Working electrode for corrosion detection and preparation method thereof Download PDFInfo
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- CN110887782A CN110887782A CN201911228734.4A CN201911228734A CN110887782A CN 110887782 A CN110887782 A CN 110887782A CN 201911228734 A CN201911228734 A CN 201911228734A CN 110887782 A CN110887782 A CN 110887782A
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Abstract
The invention discloses a working electrode for corrosion detection, which comprises a metal sample to be detected, wherein a lead is pressed and adhered on the non-detection surface of the metal sample and is adhered on the surface of a glass substrate, the lead is arranged between the metal sample and the glass substrate, and the tail part of the lead extends out of the glass substrate for packaging; the invention also discloses a novel method for preparing the working electrode for corrosion detection, which comprises the steps of preprocessing the non-detection surface of the metal sample, pressing and bonding a lead and packaging epoxy resin. The invention has simple structure and process, high preparation efficiency, extremely low cost and good sealing performance, can effectively ensure good contact of electrode system loops, avoids corrosion test interference caused by incomplete gap packaging, is easy to realize large-scale preparation production, and provides a working electrode for corrosion detection with simple structure and a novel high-efficiency and low-cost preparation method thereof for the technical field of electrochemical tests.
Description
Technical Field
The invention belongs to the technical field of electrochemical corrosion tests, and particularly relates to a working electrode for corrosion detection and a preparation method of the working electrode.
Background
Electrochemical corrosion tests generally employ a three-electrode system consisting of an auxiliary electrode, a reference electrode, and a working electrode. The working electrode is the subject of corrosion testing research, the primary task of corrosion testing being to prepare the working electrode. The manufacture of the working electrode requires simple structure and process, good contact of the electrode system loop, and corrosion test interference caused by incomplete gap packaging.
A detachable electrochemical working electrode (application date: 2019.04.29, bulletin date: 2019.08.02, bulletin number: CN110082408A) disclosed a traditional working electrode preparation method, a cavity for accommodating a spring is arranged in a top cover of the detachable working electrode, one end of a bottom shell, which is abutted to a metal sample, comprises an inner bottom surface and an outer bottom surface, an included angle α (0 degree < α < 90 degrees) needs to be formed between the inner bottom surface and the inner wall surface of the bottom shell, a chamfer β (β > 30 degrees) and a conical opening need to be formed on the outer bottom surface, a lead needs to be provided with a bent angle gamma (0 degree < gamma < 90 degrees), and an included angle gamma (gamma) needs to be formed between a first working surface of the2(γ2Not less than 90 percent). Meanwhile, an internal thread is arranged at one end, connected with the top cover, of the bottom shell, an external thread is arranged on the top cover, and the length of the internal thread of the bottom shell is larger than or equal to that of the internal thread of the top cover. In conclusion, the preparation of the working electrode needs to specially design a bottom surface included angle, an outer bottom chamfer angle, an outer bottom conical opening, a lead bent angle, a metal sample horizontal included angle and the like, the preparation process is complicated, and the structure is complicated due to the fact that a threaded connection, an axial hollow structure, a bottom shell, a top cover, a sealing ring and a sealing block need to be designed.
More importantly, the connection mode of the detachable working electrode metal flexible lead and the metal sample is as follows: one end of the metal flexible wire is a free end, the other end of the metal flexible wire is fixed on the top cover through the sealing block and penetrates through the top cover to be connected with one end of the spring, and the other end of the spring is abutted to the metal sample. However, spring contact is prone to poor contact of the electrode working circuit. Meanwhile, the spring is easy to generate plastic deformation, fatigue fracture and stress corrosion fracture in the corrosion detection process under the action of alternating stress, and the working electrode is directly failed. Therefore, the exploration of a new technology for preparing the fully-encapsulated working electrode with simple structural process, high construction efficiency and good electrode circuit contact becomes an important direction and a hot spot in the current electrochemical corrosion detection research.
Disclosure of Invention
The invention aims to provide a working electrode system for corrosion detection, which has a simple structure, avoids corrosion test interference caused by incomplete packaging of gaps, and effectively ensures good contact of a loop of the electrode system.
Another object of the present invention is to provide a method for preparing a working electrode for corrosion detection, which is simple and efficient.
The first technical scheme adopted by the invention is that the working electrode for corrosion detection comprises a metal sample to be detected, a lead is pressed and adhered to the non-detection surface of the metal sample and is adhered to the surface of a glass substrate, the adhesion surface area of the glass plate is larger than the non-detection surface area of the metal sample, the metal sample is packaged except for the detection surface, the lead is positioned between the metal sample and the glass plate, and the tail part of the lead extends out of the package.
The first technical scheme of the invention is also characterized in that:
the wire is a metal flexible wire.
The lead is pressed and adhered on the non-detection surface of the metal sample through the conductive adhesive.
The non-detection surface of the metal sample is adhered to the glass plate by an epoxy resin adhesive.
The second technical scheme adopted by the invention is a preparation method of the working electrode for corrosion detection, which is used for preparing the working electrode system for corrosion detection in the first technical scheme of the invention and is implemented according to the following steps:
and 3, adhering the non-detection surface of the metal sample to the surface of the material substrate, wherein the material substrate is non-conductive and does not generate electrochemical reaction with the corrosion test electrolyte, and the metal sample is packaged and the detection surface of the metal sample is exposed, so that the preparation of the working electrode for corrosion detection is completed.
The second technical scheme of the invention is also characterized in that:
in the step 1, when the metal sample is a metal material which is easy to oxidize, the pretreatment is to polish and ultrasonically clean the non-detection surface of the metal sample; when the metal sample is a metal material which is not easy to oxidize, the pretreatment is only to carry out ultrasonic cleaning on the non-detection surface of the metal sample.
In the step 1, the ultrasonic cleaning is to sequentially place the metal sample into acetone, absolute ethyl alcohol and deionized water to carry out ultrasonic cleaning for 10min respectively so as to remove organic matters, oil stains and impurities on the surface of the metal sample, and then blow-dry the metal sample after ultrasonic cleaning by 99.999% high-purity nitrogen.
And 2, pressing and sticking the lead on the non-detection surface of the metal sample by adopting conductive adhesive.
And 3, sticking the non-detection surface of the metal sample and the material substrate by using an epoxy resin adhesive, and packaging the metal sample except the detection surface.
In step 3, the material substrate is not conductive and does not electrochemically react with the corrosion test electrolyte.
The invention has the beneficial effects that:
1. structural aspect of working electrode:
1) the working electrode for corrosion detection has a simple structure and extremely low cost;
2) the metal flexible lead is pressed and adhered to the non-detection surface of the metal sample by adopting conductive adhesive, the non-detection surface of the metal sample is adhered to the surface of the glass plate by adopting epoxy resin adhesive, and the periphery of the sample is packaged, so that corrosion test interference caused by incomplete packaging of the electrode in a gap can be effectively avoided;
3) the connection mode of the lead and the metal sample belongs to line connection, and good contact of a working electrode system loop can be effectively ensured.
2. The preparation process of the working electrode comprises the following steps:
1) the preparation method of the working electrode for corrosion detection is simple and clear, and has strong operability;
2) the conductive adhesive is adopted for pressure bonding and epoxy resin packaging treatment, the process is simple, the preparation efficiency is high, and the large-scale preparation and production of the working electrode are easy to realize.
3. The corrosion detection effect of the working electrode is as follows:
the electrochemical experiment test result shows that the open circuit potential value of the metal sample is measured for corrosion detection, the good corrosion detection effect is shown, and the metal sample can be used as a good electrode device for metal corrosion detection.
Drawings
FIG. 1 is a schematic structural view of a working electrode for corrosion detection according to the present invention;
FIG. 2 is a cross-sectional view taken along the line A-A of the working electrode structure of FIG. 1;
FIG. 3 is a flow chart of a method of fabricating a working electrode for corrosion detection according to the present invention;
FIG. 4 is a schematic diagram of a three-electrode system for testing open-circuit potential;
FIG. 5 is a graph showing the open circuit potential of an aluminum block in 3.5% NaCl electrolyte as measured by a working electrode for corrosion detection according to the present invention.
In the figure, 1 is a metal sample non-detection surface, 2 is conductive adhesive, 3 is a metal flexible lead, 4 is epoxy resin-based adhesive, 5 is a glass plate, 6 is a metal sample detection surface, 7 is a metal sample, 8 is an auxiliary electrode, 9 is a working electrode, and 10 is a reference electrode.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more clear, the following detailed description of the embodiments, structural features and corrosion detection functional characteristics of the present invention is provided with reference to the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention, which is described in detail below with reference to the accompanying drawings and the detailed description.
The invention relates to a working electrode for corrosion detection, which comprises a metal sample 7 to be detected, wherein a lead 3 is pressed and adhered on a non-detection surface 1 of the metal sample 7 through a conductive adhesive 2, the lead 3 is a metal flexible lead, the non-detection surface 1 of the metal sample 7 is adhered on the surface of a glass plate 5 through an epoxy resin adhesive 4, the adhering surface area of the glass plate 5 is larger than the area of the non-detection surface 1 of the metal sample 7, the metal sample 7 is packaged except for a detection surface 6, and the lead 3 is positioned between the metal sample 7 and the glass plate 5, and the tail part of the lead extends out of the package.
The preparation method of the working electrode for corrosion detection is used for preparing the working electrode system for corrosion detection, and is specifically implemented according to the following steps as shown in fig. 2:
in the step 1, the ultrasonic cleaning is to sequentially place the metal sample 7 into acetone, absolute ethyl alcohol and deionized water to perform ultrasonic cleaning for 10min respectively so as to remove organic matters, oil stains and impurities on the surface of the metal sample 7, and then blow-dry the metal sample 7 subjected to ultrasonic cleaning by 99.999% high-purity nitrogen.
And 2, pressing and sticking the wire 3 on the non-detection surface 1 of the metal sample 7 by adopting the conductive adhesive 2, wherein the wire 3 is a metal flexible wire and can be a copper wire core or an aluminum wire core.
And 3, adhering the non-detection surface 1 of the metal sample 7 to the surface of a substrate by using an epoxy resin adhesive 4, wherein the substrate is non-conductive and does not have electrochemical reaction with corrosion test electrolyte, the substrate is made of a glass plate 5, the metal sample 7 is packaged by using the epoxy resin adhesive 4, and only the detection surface 6 of the metal sample 7 is exposed, so that the preparation of the working electrode for corrosion detection is completed.
The invention conception is as follows: the working electrode for corrosion detection and the preparation method thereof are further researched and made based on the defects of the existing working electrode and the preparation method thereof, and although the corrosion performance detection can be realized by the common traditional detachable working electrode preparation method, the electrode preparation needs to design a bottom surface included angle, an outer bottom chamfer angle, an outer bottom conical opening, a lead bent angle and a metal sample horizontal included angle, so that the preparation process is complicated; meanwhile, a threaded connection, an axial hollow structure, a bottom shell, a top cover, a sealing ring and a sealing block are specially designed, so that the structure is complex; more importantly, poor contact of an electrode system loop is easily caused by the contact of the abutting point of the spring, and the spring is easily subjected to plastic deformation, fatigue fracture and stress corrosion fracture in the corrosion detection process under the action of alternating stress, so that the working electrode is directly failed. In order to prepare the working electrode system for corrosion detection more simply and effectively, the inventor begins to make a more ideal working electrode system for corrosion detection and a preparation method thereof by continuously adjusting experimental parameters and steps to a novel method for preparing a fully-packaged working electrode with simple structural process, high construction efficiency and good electrode circuit contact.
For further comparison and verification, the working electrode for corrosion detection and the preparation method thereof have simple structure and process. Table 1 shows the preparation method of the working electrode, the contact manner of the lead wire and the metal sample, and the structural characteristics of the electrode. The problems of complex structure, complex process, low efficiency, poor contact of a motor system loop, incomplete encapsulation of a gap, high construction cost and the like in the conventional working electrode preparation are comprehensively evaluated. Compared with the existing working electrode preparation method (see table 1), the invention comprises a glass plate, a metal flexible lead, an epoxy resin adhesive and a conductive adhesive, and has simple structure and extremely low cost; the connection mode of the metal flexible lead and the metal sample belongs to pressure bonding wire connection, and good contact of a working electrode system loop can be ensured; the non-detection surface of the metal sample is adhered to the surface of the glass plate by using the epoxy resin adhesive, and the periphery of the sample is packaged, so that corrosion detection interference caused by incomplete packaging surfaces in gaps can be effectively avoided.
TABLE 1
To further verify the corrosion detection effect of the working electrode for corrosion detection according to the present invention, an electrochemical experiment test is performed, as shown in fig. 4, a three-electrode system is adopted, a platinum wire with a diameter of 0.5mm is used as an auxiliary electrode 8, an aluminum block with a diameter of 10mm x 2mm is used as a working electrode 9, a saturated calomel electrode SCE is used as a reference electrode 10, and a change curve of an aluminum electrode potential with time when a current density is zero, i.e., a change curve of an open circuit potential with time (the open circuit potential represents an electrode potential when the current density is 0, i.e., a potential difference between the working electrode and the reference electrode when no load exists) is measured in a 3.5% NaCl electrolyte, as shown in fig. 5. As can be seen from FIG. 5, the open circuit potential of the aluminum block fluctuates in negative shift with the extension of the test time, but the overall trend is slowly shifted in positive shift, and finally a relatively stable potential value of-1.035V is reached. According to electrochemical test data, the open circuit potential of the aluminum block measured by the working electrode for corrosion detection is close to the standard open circuit potential value of aluminum material, namely-1.05V (the error is less than 2%), so that the working electrode for corrosion detection shows a good corrosion detection effect and can be used as a good electrode device for metal corrosion performance detection.
In conclusion, the working electrode for corrosion detection has the advantages of simple structure, extremely low cost and good sealing performance, can effectively ensure good contact of electrode system loops, and avoids corrosion test interference caused by incomplete gap packaging. The preparation method of the working electrode for corrosion detection, provided by the invention, has the advantages of simple process and high preparation efficiency, is easy to realize large-scale preparation and production, and provides a novel high-efficiency and low-cost preparation method of the working electrode for corrosion detection for the technical field of electrochemical test.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. The utility model provides a working electrode for corrosion detection, its characterized in that presses metal sample (7) that has wire (3) including non-detection face (1), non-detection face (1) of metal sample (7) are pasted on glass board (5) surface, the area that pastes of glass board (5) is greater than non-detection face (1) of metal sample (7) is big, all encapsulate except that its detection face (6) metal sample (7), wire (3) are located between metal sample (7) and glass board (5) and its afterbody stretches out the encapsulation.
2. The working electrode for corrosion detection according to claim 1, wherein the wire (3) is a flexible metal wire.
3. The working electrode for corrosion detection according to claim 1, wherein the lead (3) is bonded to the non-detection surface (1) of the metal sample (7) by means of a conductive adhesive (2).
4. The working electrode for corrosion detection according to claim 1, wherein the non-detection surface (1) of the metal sample (7) is adhered to the glass plate (5) by an epoxy adhesive (4).
5. A method for producing a working electrode for corrosion detection, which is used for producing the working electrode for corrosion detection according to any one of claims 1 to 4, and which is carried out specifically according to the following steps:
step 1, preprocessing a non-detection surface (1) of the metal sample (7);
step 2, pressing and sticking the lead (3) on the non-detection surface (1) of the metal sample (7);
and 3, adhering the non-detection surface (1) of the metal sample (7) to the surface of the material substrate, packaging the metal sample (7), exposing the detection surface (6) of the metal sample (7), and completing the preparation of the working electrode for corrosion detection.
6. The method for preparing the working electrode for corrosion detection according to claim 5, wherein in the step 1, when the metal sample (7) is a metal material which is easy to oxidize, the pretreatment is polishing and ultrasonic cleaning of the non-detection surface (1) of the metal sample (7); when the metal sample (7) is a metal material which is not easy to oxidize, the pretreatment is only to carry out ultrasonic cleaning on the non-detection surface of the metal sample (7).
7. The method for preparing a working electrode for corrosion detection as claimed in claim 6, wherein the ultrasonic cleaning in step 1 is to sequentially place the metal sample 7 in acetone, absolute ethanol and deionized water for ultrasonic cleaning for 10min to remove organic matters, oil stains and impurities on the surface of the metal sample 7, and then blow-dry the ultrasonically cleaned metal sample 7 with 99.999% high purity nitrogen.
8. The method for preparing a working electrode for corrosion detection according to claim 5, wherein in the step 2, the conducting wire (3) is pressed and adhered to the non-detection surface (1) of the metal sample (7) by using the conductive adhesive (2).
9. The method for preparing a working electrode for corrosion detection according to claim 5, wherein in the step 3, the non-detection surface (1) of the metal sample (7) is adhered to the material substrate by using the epoxy resin adhesive (4), and the exterior of the metal sample (7) except the detection surface (6) is encapsulated.
10. The method of claim 5, wherein the substrate of material in step 3 is non-conductive and does not electrochemically react with the corrosion test electrolyte.
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| CN113899688B (en) * | 2021-10-27 | 2024-05-28 | 广东电网有限责任公司广州供电局 | Working electrode for metal corrosion test and preparation method and test method thereof |
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Application publication date: 20200317 |