CN112730555A - Zinc-based alloy working electrode and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of electrochemical performance testing, in particular to a zinc-based alloy working electrode and a preparation method thereof. The working electrode comprises a zinc-based alloy test piece, a lead, a conductive layer and an insulating layer; the wire comprises a multi-strand conductive metal wire part with an insulating shell part and without the insulating shell part; the conductive layer is formed by dispersing conductive metal wires on the side and the top of the zinc-based alloy test piece and fixing the conductive metal wires by using the copper adhesive tape; the insulating layer is formed by coating a cold embedding agent outside the conductive layer by a cold embedding method, and the conducting wire part with the insulating shell is positioned at the top of the zinc-based alloy and penetrates through the insulating layer to be communicated with a test circuit. The working electrode has the advantages of low raw material cost, simple and convenient preparation process operation, large contact surface between the conducting layer and the zinc-based alloy, avoidance of infirm bonding and gaps, contribution to reducing contact resistance, protection of the structure of the zinc-based alloy and better sealing property, conductivity and processability of the electrode; and the zinc-based working electrode has good application effect in the electrochemical corrosion performance test.
Description
Technical Field
The invention relates to the field of electrochemical performance testing, in particular to a zinc-based alloy working electrode and a preparation method thereof.
Background
In an electrochemical experiment, a working electrode is a commonly used electrode for measuring a component to be measured, and the working electrode is generally obtained by welding a copper wire with a waterproof rubber sheet at one end of a non-working surface of a test piece, then packaging and molding the copper wire by using epoxy resin or paraffin, and grinding and polishing the other end of the working electrode serving as a working surface on the premise of ensuring good electric conduction between the wire and the test piece. Firstly, the test piece, the lead and the welding flux are required to be simultaneously controlled to complete welding, so that the three parts are ensured to be in good contact with each other with high difficulty; secondly, the high temperature of the weld also affects the flux adhesion, and cooling tends to be time consuming; thirdly, the mould is difficult to demould, the sample is easy to incline during cold inlaying, the paraffin is sealed and is easy to pollute the working surface, the grinding is easy to incline the working surface, in addition, the paraffin falls off and can also cause gap corrosion, the effective area and the test result of the working surface of the test piece are directly influenced, the manufacturing cost is high, the period is long, except for time consumption of cooling, in the welded contact points, conductive silver paste is often coated to reduce the contact resistance and increase the conductivity, but if other tests are needed later, the packaging layer is required to be opened and the conductive silver paste layer is required to be cleaned, which can damage the test piece body, in addition, the cost and the working procedure are increased by a demoulding agent or a customized mould blank used for demoulding; high temperature affects the test effect, zinc belongs to low-melting-point metal, and the high temperature generated in the welding and wax sealing process can cause the structural change of zinc-based alloy, so that the experimental result is inaccurate.
The other electrode making process is screw rotating and nesting connection technology, and includes machining hard plastic or PTFE plastic into cylindrical female screw end and sealed back cover, machining the circular hole in the female screw end for contacting the working surface of the cylindrical test piece with medium, machining the female screw hole in the other end to the diameter slightly greater than the circular hole, machining inner thread inside the female screw hole to ensure the inner screw hole diameter equal to the test piece diameter, machining outer thread in the male screw end of the cylinder and ensuring the male screw end diameter and the outer thread to match the female screw hole. The external lead is nested on the sealed rear cover and is connected with the male wire end. And grinding and polishing the machined surface of the test piece to be used as a working surface, wherein the working surface faces to the hole opening of the female screw, one end of the male screw end is aligned to the non-working surface and rotates to push the test piece to the female screw hole of the female screw end, and the female screw end can be completely contacted with the sealed rear cover by appropriately screwing, so that the electrode is manufactured. The method does not need heating, is convenient to manufacture and take out, can easily finish sample preparation especially for a thin cylindrical test piece which is difficult to grind, but has high requirement on the precision of the test piece and a nested connecting structural component and high price, the structure and the connecting mode of the electrode can cause the sealing of a non-working surface of the test piece to be poor, and contact resistance can be increased due to the uneven working surface or deepened corrosion, so that electrolyte flows into the side surface of the test piece or a gap of a nested thread, and particularly the gap is gradually increased due to multiple use, so that the effective test area of the electrode is increased.
Disclosure of Invention
The invention aims to solve the technical problems of operation, sealing, high temperature, high cost, long period and application in the preparation method of the working electrode in the prior art, the conductive metal wires in the conducting wires are adhered to and cover the side and the top of a zinc-based alloy test piece, the conducting layer is formed by fixing the conducting wires by using the conductive adhesive tape, and the insulating layer material is coated on the conducting layer by using a cold embedding method, so that the obtained working electrode has small contact resistance and good sealing property, can well protect the structure of the zinc-based alloy, and has good application effect in an electrochemical corrosion performance test.
In order to realize the aim, the invention firstly provides a zinc-based alloy working electrode, which specifically comprises a zinc-based alloy test piece, a lead, a conductive layer and an insulating layer;
the wire comprises a multi-strand conductive wire part with an insulating shell part and without the insulating shell part;
the conducting layer is formed by overlapping a plurality of conducting metal wires without an insulating shell conducting wire part and two layers of double-sided copper adhesive tapes in a layered and crossed manner, and the conducting metal wires are dispersed on the side and the top of the zinc-based alloy test piece and are fixed by the copper adhesive tapes;
the insulating layer is a cold embedding agent and is coated outside the conductive layer by a cold embedding method, and the conducting wire part with the insulating shell is positioned at the top of the zinc-based alloy and penetrates through the insulating layer to be communicated with a test circuit.
Further, the cold setting agent is a mixture of crystal glue and a curing agent, and the mass ratio of the crystal glue to the curing agent is 10-20: 1.
Based on the same inventive concept, the invention also provides a preparation method of the zinc-based alloy working electrode, which comprises the following steps:
s1, uniformly dispersing the conductive wires of the wire part without the insulating shell on the side and the top of the time, and winding and fixing the conductive wires by adopting a copper adhesive tape to obtain a conductive assembly;
s2, preparing a cold embedding agent, placing the conductive assembly in a flat-mouth round-bottom soft test tube mold and fixing, adding the cold embedding agent into the mold and carrying out cold embedding for 20-30min to obtain a cold embedding working electrode;
s3, taking out the cold-embedding working electrode, cutting off redundant cold-embedding agent at the bottom of the zinc-based alloy test piece, and then solidifying for 20-30 min;
and S4, grinding the bottom of the working electrode obtained in the step S3 with sand paper for multiple times, polishing with diamond polishing solution, ultrasonically cleaning with alcohol, and cold-blowing to dry to obtain the zinc-based working electrode.
Further, the multiple sanding in step S4 specifically includes:
successively adopting 100# Al2O3Sandpaper, 1000# SiC sandpaper and 1500# Al2O3And (5) polishing with sand paper.
Further, the diamond micro powder of the diamond polishing solution has a particle size of 3 μm.
Has the advantages that:
according to the invention, the conductive material is fixed on the zinc-based alloy test piece through the conductive adhesive tape, the insulating layer is coated outside the zinc-based alloy test piece through a cold embedding method, and the zinc-based working electrode is obtained through grinding, polishing and cold blow-drying; the structure of the zinc-based alloy is also protected by cold bonding, cold inlaying and cold blow drying, and the cutting plane in the middle stage of the cold inlaying process reduces the grinding difficulty, so that the electrode has better sealing property, conductivity and processability; and the zinc-based working electrode has good application effect in the electrochemical corrosion performance test.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a zinc-based alloy working electrode provided by the invention;
FIG. 2 is a schematic diagram of a three-electrode testing system according to an embodiment of the present invention;
FIG. 3 is a Tafel curve obtained by an EG electrochemical experiment of a zinc-based alloy working electrode provided by an application example of the invention;
FIG. 4 is a Tafel curve obtained by an electrochemical experiment of a zinc-based alloy working electrode CG1 provided by an application example of the invention;
FIG. 5 is Tafel curve obtained by electrochemical experiment of zinc-based alloy working electrode CG2 provided by the application example of the invention;
fig. 6 is a Tafel curve obtained by electrochemical experiments of the zinc-based alloy working electrodes EG, EG1 and EG2 provided by the application example of the invention.
[ description of reference ]
1-zinc base alloy test pieces; 2-a wire; 3-a conductive layer; 4-an insulating layer; 5-reference electrode I; 6-pair of electrodes; 7-reference electrode II; 8-an electrolytic cell; 9-mould.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
As shown in figure 1, the invention provides a zinc-based alloy working electrode, which comprises a zinc-based alloy test piece 1, a lead 2, a conducting layer 3 and an insulating layer 4, wherein the lead 2 comprises a multi-strand conducting metal wire part with an insulating shell part and without an insulating shell, the conducting metal wires without the insulating shell part are dispersed on the side surface and the top of the zinc-based alloy test piece 1 and are wound and fixed by two layers of double-sided copper adhesive tapes to form the conducting layer 3, the insulating layer is coated outside the conducting layer 3 by a cold embedding method through a cold embedding agent, and the lead 2 with the insulating shell penetrates through the insulating layer to form a cylindrical zinc-based alloy working electrode.
Example 1
S1 test piece of cylindrical zinc-based alloy with the diameter of 10 mm by 20mm (the Mg content is
) And select the copper wire, go out some insulating housing, with the conductive copper wire in the wire stranded back individual layer dispersion paste in test piece side and top: tightly fixing the conductive copper wires on the side surface of the test piece by using a double-sided conductive copper adhesive tape, reversely folding the copper wires with the length exceeding that of the zinc-based alloy test piece on the adhesive tape, tightly fixing the copper wires by winding a layer of double-sided conductive copper adhesive tape, and twisting the dispersed copper wires to be tightly attached to the top surface of the test piece; and (5) sticking a test piece label on the outer layer of the copper adhesive tape to obtain a conductive assembly.
S2, using a phi 15 x 40mm flat round bottom soft test tube as a mold, ironing a round fixing hole with the diameter slightly smaller than the outer diameter of a lead in the center of the bottom of the test tube, enabling the lead to downwards penetrate through the round fixing hole to fix a conductive assembly in the mold, preparing a cold embedding agent of crystal glue epoxy resin and a curing agent p-hydroxybenzene sulfonic acid according to the mass ratio of 10:1, pouring the cold embedding agent into a grinding tool to perform cold embedding for 22min, molding and taking out to obtain the cold embedding working electrode.
And S3, cutting the crystal glue radially at a position 2mm away from the bottom surface of the test piece by the cold-embedded working electrode to obtain a cross section parallel to the bottom surface of the test piece, and then solidifying for 26min to increase the bonding strength and the wear-resisting strength.
S4 use of 100# Al in sequence for bottom of working electrode obtained in S32O3Grinding off crystal glue covering the bottom surface of the test piece by using abrasive paper to expose a rough working surface, and sequentially using 1000# SiC abrasive paper and 1500# Al2O3And (3) grinding the bottom surface to be flat by using sand paper, then polishing the bottom surface by using diamond polishing solution with the particle size of 3 mu m, finally ultrasonically cleaning the bottom surface by using alcohol for 10min, and drying the bottom surface by using cold air to obtain the zinc-based working electrode.
Example 2
S1 test piece of cylindrical zinc-based alloy with the diameter of 10 mm by 20mm (the Mg content is
) And select the copper wire, go out some insulating housing, with the conductive copper wire in the wire stranded back individual layer dispersion paste in test piece side and top: tightly fixing the conductive copper wires on the side surface of the test piece by using a double-sided conductive copper adhesive tape, reversely folding the copper wires with the length exceeding that of the zinc-based alloy test piece on the adhesive tape, tightly fixing the copper wires by winding a layer of double-sided conductive copper adhesive tape, and twisting the dispersed copper wires to be tightly attached to the top surface of the test piece; and (5) sticking a test piece label on the outer layer of the copper adhesive tape to obtain a conductive assembly.
S2, using a phi 15 x 40mm flat round bottom soft test tube as a mold, ironing a round fixing hole with the diameter slightly smaller than the outer diameter of a lead in the center of the bottom of the test tube, enabling the lead to downwards penetrate through the round fixing hole to fix a conductive assembly in the mold, preparing a cold embedding agent of crystal glue epoxy resin and a curing agent p-hydroxybenzene sulfonic acid according to the mass ratio of 15:1, pouring the cold embedding agent into a grinding tool to perform cold embedding for 25min, molding and taking out to obtain the cold embedding working electrode.
And S3, cutting the crystal glue radially at a position 1.5mm away from the bottom surface of the test piece by the cold-embedded working electrode to obtain a cross section parallel to the bottom surface of the test piece, and then solidifying for 30min to increase the bonding strength and the wear-resisting strength.
S4 use of 100# Al in sequence for bottom of working electrode obtained in S32O3The water covering the bottom surface of the test piece is ground by abrasive paperCrystal glue, exposing a rough working surface, using 1000# SiC sand paper and 1500# Al in sequence2O3And (3) grinding the bottom surface to be flat by using sand paper, then polishing the bottom surface by using diamond polishing solution with the particle size of 3 mu m, finally ultrasonically cleaning the bottom surface by using alcohol for 10min, and drying the bottom surface by using cold air to obtain the zinc-based working electrode.
Example 3
S1 test piece of cylindrical zinc-based alloy with the diameter of 10 mm by 20mm (the Mg content is
) And select the copper wire, go out some insulating housing, with the conductive copper wire in the wire stranded back individual layer dispersion paste in test piece side and top: tightly fixing the conductive copper wires on the side surface of the test piece by using a double-sided conductive copper adhesive tape, reversely folding the copper wires with the length exceeding that of the zinc-based alloy test piece on the adhesive tape, tightly fixing the copper wires by winding a layer of double-sided conductive copper adhesive tape, and twisting the dispersed copper wires to be tightly attached to the top surface of the test piece; and (5) sticking a test piece label on the outer layer of the copper adhesive tape to obtain a conductive assembly.
S2, using a phi 15 x 40mm flat round bottom soft test tube as a mold, ironing a round fixing hole with the diameter slightly smaller than the outer diameter of a lead in the center of the bottom of the test tube, enabling the lead to downwards penetrate through the round fixing hole to fix a conductive assembly in the mold, preparing a cold embedding agent of crystal glue epoxy resin and a curing agent p-hydroxybenzene sulfonic acid according to the mass ratio of 20:1, pouring the cold embedding agent into a grinding tool to perform cold embedding for 30min, molding and taking out to obtain the cold embedding working electrode.
And S3, cutting the crystal glue radially at a position 1mm away from the bottom surface of the test piece by the cold-embedded working electrode to obtain a cross section parallel to the bottom surface of the test piece, and then solidifying for 20min to increase the bonding strength and the wear-resisting strength.
S4 use of 100# Al in sequence for bottom of working electrode obtained in S32O3Grinding off crystal glue covering the bottom surface of the test piece by using abrasive paper to expose a rough working surface, and sequentially using 1000# SiC abrasive paper and 1500# Al2O3And (3) grinding the bottom surface to be flat by using sand paper, then polishing the bottom surface by using diamond polishing solution with the particle size of 3 mu m, finally ultrasonically cleaning the bottom surface by using alcohol for 10min, and drying the bottom surface by using cold air to obtain the zinc-based working electrode.
Comparative example 1
Taking a cylindrical zinc-based alloy test piece with the diameter of 10 multiplied by 20mm (the Mg content is
) The tin wire is used as solder, the conductive copper wire is fixed at one end of the non-working surface of the test piece by adopting a soft soldering process, the paraffin is melted, the temperature of the paraffin is cooled to be slightly lower than 40 ℃, and the paraffin is manually coated on the top and the side of an electrode assembly and immediately molded to obtain the zinc-based working electrode.
Comparative example 2
Taking a cylindrical zinc-based alloy test piece with the diameter of 10 multiplied by 20mm (the Mg content is
) The tin wire is used as solder, the conductive copper wire is fixed at one end of the non-working surface of the test piece by adopting a soft soldering process, the conductive assembly is completely immersed into the molten liquid by adopting a dipping and pulling method after paraffin is melted, and the assembly is immediately transferred into water for cooling and forming to obtain the zinc-based working electrode.
And (3) performance testing:
experimental example 1
According to the test method in the GB/T16886.15-2003 standard, 0.9% NaCl solution is used as electrolyte, and the height of a working electrode is controlled by fixing a lead through a fixing hole on a die, so that a stable three-electrode test system is formed and shown in the attached drawing 2, wherein 5 a reference electrode I is a calomel electrode, 7 a reference electrode II is a zinc-based working electrode prepared by the method, and 6 pairs of electrodes are platinum electrodes. The zinc-based working electrodes obtained in example 1 and comparative examples 1 and 2 were respectively marked as working electrodes EG, CG1 and CG2 by using CHI-604E electrochemical workstation, polarization curve test was performed to obtain Tafel curve, and self-corrosion potential (E) was obtained by analyzing the curvecorr) And self-etching current density (i)corr) Etc., detailed in fig. 3-5, and table 1.
TABLE 1 electrochemical test results for zinc-based working electrodes
As can be seen from Table 1 and FIGS. 3-5, the polarization curve of CG1 electrode has three strong polarization regions, corresponding to E, as can be seen from FIG. 4corrSequentially at-1.239V, -1.201V and-1.125V, wherein-1.125V is the E of CG1 electrode working surface analyzed by polarization curve test softwarecorrCorresponding to icorrIs 0.590A · cm-2According to the CG1 scheme, the performance parameters of the CG1 electrode are changed due to high temperature, and the side or the top of the test piece subjected to high temperature is exposed in electrolyte to cause corrosion due to the fact that paraffin is not sealed tightly or the paraffin falls off due to long-time soaking. As can be seen from FIG. 5, the CG2 electrode only has a strong polarization region near-1.201V, which is near-1.201V of CG1, while the strong polarization region near-1.239V of CG1 is not present in FIG. 2, and it is speculated that the strong polarization region near-1.239V in CG1 may be from a top solder site subjected to high temperature, while the better sealing of G2 to the test piece eliminates corrosion at this site, while the strong polarization region near-1.201V in CG1 may be from a side surface with a slightly lower temperature, while the working surface of test CG2 may be subjected to the same temperature. In addition, the polarization curve software analyzes the E of the CG2 electrodecorris-1.203V, icorrIs 1.010 muA.cm-2Compared with CG1, E of CG2 electrodecorThe lower 0.076V is probably due to the fact that the working surface of CG2 bears higher temperature than the working surface of CG1, while the i of CG2corrCompared with CG1, the improvement is 0.420 muA cm-2And the contact resistance is reduced due to better sealing property. On the other hand, compared with CG1, the strong polarization area of CG2 has lower sharpness and reflects the influence of high temperature on the texture of the working surface, and the results of CG1 and CG2 reflect that welding may cause the overall nonuniformity of the zinc-based alloy test piece.
Compared with CG1 and CG2 electrodes, the EG electrode obtained by the embodiment of the invention has the advantages that the Tafel curve only has a sharp and strong polarization region, and E iscorrE at-1.131V, with CG1corrClose (difference 0.006)V), and i)corr(1.372μA·cm-2) 0.782 muA cm higher than CG1 and CG2 respectively-2And 0.362. mu.A. cm-2Further reduction of contact resistance is reflected, and test data of EG can reflect electrochemical performance of selected zinc-based alloy test pieces.
Experimental example 2
In order to verify the effectiveness and repeatability of the zinc-based working electrode obtained in the embodiment of the invention, the working electrode EG obtained in the embodiment 1 is subjected to two repeatability tests: and in the second repeated test, aiming at the EG1 electrode subjected to the polarization curve test, the corrosion layer of the electrode is completely wiped off by using sand paper, a smooth and clean working surface is re-ground, so that the EG2 electrode is obtained, and the technical curve test is carried out. The results of Tafel curves for EG electrode, EG1 electrode, EG2 electrode are detailed in FIG. 6.
In fig. 6, the EG electrode, EG1 electrode, EG2 electrode correspond to curve D, E, F, respectively, and it can be seen from the figure that all three curves have distinct Tafel regions, and E of the three curvescorrAre all around-1.119V (± 0.011V interval), where E of EGcorrE as-1.131V, EG1corrE as-1.119V, EG2corrat-1.107V, which may be caused by non-homogeneity between the working surfaces of the cylindrical electrodes and other environmental factors, E was obtained from three testscorrThe coefficient of variation, CV, of the values was about 0.011, within a reasonable range. The prepared electrode of the method can ensure the effectiveness and repeatability of the test result.
Compared with the electrode manufactured by the traditional scheme, the zinc-based alloy working electrode manufactured by the invention has good sealing performance and better conductivity, avoids the influence of high temperature on the performance of a test piece, can ensure the stability of an electrochemical test system, obtains a Tafel curve with obvious characteristics and effective performance parameters, has high experimental repeatability, and can meet the test requirement on the electrochemical corrosion performance of a zinc-based alloy material.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The zinc-based alloy working electrode is characterized by specifically comprising a zinc-based alloy test piece, a lead, a conductive layer and an insulating layer;
the wire comprises a multi-strand conductive wire part with an insulating shell part and without the insulating shell part;
the conducting layer is formed by overlapping a plurality of conducting metal wires without an insulating shell conducting wire part and two layers of double-sided copper adhesive tapes in a layered and crossed manner, and the conducting metal wires are dispersed on the side and the top of the zinc-based alloy test piece and are fixed by the copper adhesive tapes;
the insulating layer is a cold embedding agent and is coated outside the conductive layer by a cold embedding method, and the conducting wire part with the insulating shell is positioned at the top of the zinc-based alloy and penetrates through the insulating layer to be communicated with a test circuit.
2. The zinc-based alloy working electrode according to claim 1, wherein the cold setting agent is a mixture of crystal glue and a curing agent, and the mass ratio of the crystal glue to the curing agent is 10-20: 1.
3. A zinc-based alloy working electrode according to claim 2, wherein the crystal glue is polyurethane PU glue or epoxy resin.
4. A zinc-based alloy working electrode according to claim 2, wherein the curing agent is p-hydroxybenzene sulfonic acid.
5. The preparation method of the zinc-based alloy working electrode is characterized by specifically comprising the following steps of:
s1, uniformly dispersing the conductive wires of the wire part without the insulating shell on the side and the top of the time, and winding and fixing the conductive wires by adopting a copper adhesive tape to obtain a conductive assembly;
s2, preparing a cold embedding agent, placing the conductive assembly in a flat-mouth round-bottom soft test tube mold and fixing, adding the cold embedding agent into the mold and carrying out cold embedding for 20-30min to obtain a cold embedding working electrode;
s3, taking out the cold-embedding working electrode, cutting off redundant cold-embedding agent at the bottom of the zinc-based alloy test piece, and then solidifying for 20-30 min;
and S4, grinding the bottom of the working electrode obtained in the step S3 with sand paper for multiple times, polishing with diamond polishing solution, ultrasonically cleaning with alcohol, and cold-blowing to dry to obtain the zinc-based working electrode.
6. The method of claim 5, wherein the plurality of sanding operations of step S4 specifically include:
successively adopting 100# Al2O3Sandpaper, 1000# SiC sandpaper and 1500# Al2O3And (5) polishing with sand paper.
7. The method for preparing a zinc-based alloy working electrode according to claim 5, wherein the diamond micro powder of the diamond polishing solution has a particle size of 3 μm.
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