CN111781256B - Universal electrolytic cell for electrochemical test - Google Patents
Universal electrolytic cell for electrochemical test Download PDFInfo
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- CN111781256B CN111781256B CN202010699017.6A CN202010699017A CN111781256B CN 111781256 B CN111781256 B CN 111781256B CN 202010699017 A CN202010699017 A CN 202010699017A CN 111781256 B CN111781256 B CN 111781256B
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- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
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Abstract
The invention relates to the technical field of electrochemical electrolytic cells, in particular to a universal electrolytic cell for electrochemical tests, which comprises an electrolytic cell, wherein the upper end of the electrolytic cell is fixedly connected with a support frame, the lower end of the electrolytic cell is fixedly connected with a base, the surface of a bottom plate of the electrolytic cell is provided with a first hole, the lower end of the first hole is communicated with a first mounting groove, a working electrode is arranged in the first mounting groove, an electrode clamp is arranged outside the working electrode and fixed at the lower end of the bottom plate, and a drain hole is formed at the position, adjacent to the side wall of the electrolytic cell, of the bottom plate; the support frame is provided with an adjusting stud and four guide posts, the guide posts are detachably and fixedly connected to the support frame, the lower ends of the guide posts are propped against the upper end of the bottom plate, and the lower ends of the adjusting studs are connected with an auxiliary electrode clamp through an adjusting mechanism; the invention can ensure that the working electrode and the auxiliary electrode can be aligned when the current electrolytic cell is used for electrochemical test, and the position of the auxiliary electrode and the distance between the two electrodes can be adjusted, thereby obtaining more accurate electrochemical test results.
Description
Technical Field
The invention relates to the technical field of electrochemical electrolytic cells, in particular to a general electrolytic cell for electrochemical tests.
Background
The electrolytic cell is a necessary experimental device for metal corrosion electrochemical test. Commonly used electrolytic cells include glass cup type and H-type glass electrolytic cells, which are convenient to use but require sample sealing treatment on samples. The sample preparation method for the electrochemical test is a common sample preparation method for sealing the metal by using epoxy resin. However, the sample preparation step using resin is complicated, and the electrochemical test result is affected by crevice corrosion between the resin and the sample. In addition, after the electrochemical test, the working electrode of the epoxy resin sealed sample is inconvenient for subsequent material analysis of the same sample (such as observing the surface appearance of the sample by using a scanning electron microscope, determining the components and structure of corrosion products, and the like), and a sample needs to be prepared additionally for analysis, so that the electrochemical test result and the material analysis result are inconsistent due to different samples.
In order to reduce the above experimental errors, researchers tend to use a box-type integrated electrolytic cell (Zhou Xianliang, guo Wenting, she Zhiguo, etc., a three-electrode system electrochemical test apparatus, national intellectual property office, patent No. 201020257142.3) composed of a box body, a cover plate and a jig holding a working electrode. By adopting the clamp, the working electrode can be fixed on the outer side of the electrolyte containing box body, and the contact between the testing surface of the working electrode and the solution is realized through the hole on the side wall of the box body. By adopting the electrolytic cell, the electrochemical experiment can be carried out without carrying out sample sealing treatment on the working electrode. In addition, the invention patents (Tian Yimei, liu Xingfei, guo Hao, etc., application number: 201510018238.1) entitled "electrochemical experimental apparatus for metal corrosion in flowing corrosive medium" also adopt similar electrolytic cell structures. The electrolytic cell with the box-type integrated structure can overcome the defects of glass cup type and H-type glass electrolytic cells, the working electrode does not need to be sealed, and subsequent material analysis can be continuously carried out after electrochemical test.
The electrochemical test of the electrolytic cell with the box-type integrated structure has the advantages that the experimental steps can be simplified, more importantly, the position of the working electrode can be fixed, and the consistency of the working electrode is ensured. However, such an apparatus does not consider the position of the auxiliary electrode and the distance between the working electrode and the auxiliary electrode, and an experiment is performed by merely inserting the auxiliary electrode into the solution. In fact, the spatial position and the geometry of the auxiliary electrode as cathode in the electrochemical three-electrode system are also very important. This is because, above all, the auxiliary electrode is the carrier for electron transfer when the circuit is turned on and electrochemical reverse reaction occurs, and its structure and position greatly affect the electrochemical results (especially the corrosion study when the auxiliary electrode and the working electrode are made of the same material). In general, the auxiliary electrode should have a large surface area so that externally applied polarization mainly acts on the working electrode, and the auxiliary electrode should have a small resistance so as not to be easily polarized. Secondly, the auxiliary electrode is generally opposite to the working electrode, and the position and the distance from the working electrode cause different solution resistances, thereby leading to different experimental results. However, in the current three-electrode system, the auxiliary electrode is usually directly inserted into the electrolyte from the opening at the upper end of the electrolytic cell, on one hand, the insertion depth is not fixed, so that the auxiliary electrode cannot be guaranteed to be always over against the working electrode, on the other hand, the distance between the auxiliary electrode and the working electrode is not adjustable, and a large error may exist in the electrochemical result due to an improper position.
Disclosure of Invention
The object of the present invention is to provide a universal electrolytic cell for electrochemical tests that solves the problems set forth in the background above.
In order to achieve the purpose, the invention provides the following technical scheme: a universal electrolytic cell for electrochemical testing comprises an electrolytic cell, wherein the upper end of the electrolytic cell is fixedly connected with a support frame, the lower end of the electrolytic cell is fixedly connected with a base, the surface of a bottom plate of the electrolytic cell is provided with a first hole, the lower end of the first hole is communicated with a first mounting groove, a working electrode is arranged in the first mounting groove, an electrode clamp is arranged outside the working electrode and fixed at the lower end of the bottom plate, and a drain hole is formed in the position, adjacent to the side wall of the electrolytic cell, of the bottom plate; the adjusting stud is in threaded connection with the support frame, the upper end of the adjusting stud is fixedly connected with a handle, and the lower end of the adjusting stud is connected with an auxiliary electrode clamp through an adjusting mechanism.
Preferably, the support frame is provided with an adjusting stud and four guide posts, the guide posts are detachably and fixedly connected to the support frame, and the lower ends of the guide posts are propped against the upper end of the bottom plate.
Preferably, the electrode clamp comprises a baffle and a screwed bolt, the baffle is fixedly connected to the lower end of the bottom plate, the screwed bolt is in threaded connection with the baffle, the upper end of the screwed bolt is attached to the working electrode, and the working electrode is attached to the lower end of the hole.
Preferably, the auxiliary electrode clamp comprises a connecting sleeve, an adjusting plate, a sample upper support, a sample lower support, an auxiliary electrode and a locking bolt; the lower extreme of adapter sleeve connects gradually sample upper support and regulating plate through the bolt, four slide holes, four have been seted up on the surface of regulating plate the guide post runs through in a slide hole respectively, support and sample under bracing threaded connection on the sample, the temple lower extreme of sample under bracing is equipped with mounting groove two, the porose two of lower extreme intercommunication of mounting groove two, auxiliary electrode is located the inside of mounting groove two and auxiliary electrode is located the upper end of hole two, locking bolt threaded connection supports on the sample, just locking bolt laminates in auxiliary electrode's upper end, working electrode and auxiliary electrode set up relatively, the middle part of regulating plate is equipped with the mounting hole, support on the sample and be located the mounting hole.
Preferably, the opening part of electrolysis trough is equipped with auxiliary support plate, the macropore has been seted up at auxiliary support plate's middle part, two at least apertures have been seted up around the macropore, the size of regulating plate is less than auxiliary support plate's macropore size.
Preferably, a sealing washer is arranged in front of the working electrode and the bottom plate, the sealing washer is arranged between the auxiliary electrode and the lower sample support, the sealing washer is arranged between the upper sample support and the lower sample support in threaded fit, and the sealing washer is arranged between the upper sample support and the connecting sleeve.
Preferably, the adjusting mechanism comprises a thrust bearing, a bearing seat, a sleeve and a locking nut, the bearing seat is connected with the upper end of the connecting sleeve through a bolt, a third hole is formed in the shoulder part of the bearing seat, and the locking bolt can be connected with a wire penetrating through the third hole.
Preferably, the adjusting stud, the adjusting mechanism, the connecting sleeve, the locking bolt, the supporting central hole on the sample, the mounting hole of the adjusting plate, the second hole, the first hole and the screwing bolt are coaxial, and the adjusting stud, the locking bolt and the screwing bolt are made of metal materials; the positions of the working electrode and the auxiliary electrode can be interchanged.
Preferably, the working electrode and the auxiliary electrode may have a circular, square, pentagonal or hexagonal shape.
Preferably, the electrolytic cell, the guide post, the auxiliary supporting plate, the connecting sleeve, the adjusting plate, the sample upper supporting plate and the sample lower supporting plate are in direct contact with the electrolyte and made of insulating materials, such as acrylic materials and polytetrafluoroethylene materials.
Preferably, when the auxiliary electrode is a working electrode, a sealing gasket is arranged between the auxiliary electrode and the sample lower support, so that good sealing of the working electrode is ensured.
Preferably, the auxiliary support plate and the opening on the auxiliary support plate can be provided with a reference electrode, a thermometer and a pH meter.
Preferably, the lowest position of the auxiliary electrode can be descended to the bottom plate of the electrolytic cell to be in contact with the upper end of the bottom plate, the working electrode is replaced under the condition that electrolyte is not discharged, and the highest position of the auxiliary electrode can be ascended to be higher than the auxiliary supporting plate, so that the auxiliary electrode can be conveniently replaced.
Preferably, the adjusting mechanism can be replaced by a sliding screw formed between the adjusting stud and the connecting sleeve.
Preferably, the adjusting mechanism consisting of the adjusting stud and the adjusting mechanism can be replaced by a screw-nut pair.
Preferably, the electrolytic cell and the support frame can be connected by a stud and a nut or by joggle joint, and the top end of the vertical part of the support frame is inserted into a hole arranged at the corresponding position of the electrolytic cell.
Preferably, the drain hole is positioned on the bottom plate.
Preferably, the supporting frame can be made into a plate shape or a lath shape, so that four or two guide posts can be arranged.
Compared with the prior art, the invention has the beneficial effects that:
the universal electrolytic cell for electrochemical tests can realize the rapid assembly of the working electrode and the auxiliary electrode; when an electrochemical experiment is carried out, the distance between the auxiliary electrode and the working electrode can be adjusted according to different test metals, the auxiliary electrode and the working electrode are just opposite, and the accuracy of an electrochemical experiment result is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced 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 that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an overall structural view of an electrolytic cell of the present invention;
FIG. 2 is a schematic view of a working electrode holder according to the present invention;
FIG. 3 is a schematic structural view of an auxiliary electrode holder according to the present invention;
in the drawings, the components represented by the respective reference numerals are listed below:
the device comprises an electrolytic cell 1, a support frame 2, a base 3, an electrode clamp 4, a working electrode 5, a guide post 6, an adjusting stud 7, an auxiliary electrode clamp 8, an adjusting mechanism 9, a bottom plate 11, a first hole 12, a drain hole 13, an auxiliary support plate 14, a baffle plate 41, a tightening bolt 42, a connecting sleeve 81, an adjusting plate 82, a sample upper support 83, a sample lower support 84, an auxiliary electrode 85, a locking bolt 86, a second hole 87, a thrust bearing 91, a bearing seat 92, a sleeve 93, a locking nut 94 and a third hole 95.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides the following technical solutions:
a general electrolytic cell for electrochemical testing comprises an electrolytic cell 1, wherein the upper end of the electrolytic cell 1 is fixedly connected with a support frame 2, the lower end of the electrolytic cell 1 is fixedly connected with a base 3, a bottom plate 11 of the electrolytic cell 1 is provided with a first hole 12, the lower end of the first hole 12 is communicated with a first mounting groove, a working electrode 5 is arranged in the first mounting groove, an electrode clamp 4 is arranged outside the working electrode 5, the electrode clamp 4 is fixed at the lower end of the bottom plate 11, and a drain hole 13 is formed in the position, adjacent to the side wall of the electrolytic cell 1, of the bottom plate 11; an adjusting stud 7 is installed on the support frame 2, the adjusting stud 7 is in threaded connection with the support frame 2, a handle is fixedly connected to the upper end of the adjusting stud 7, and an auxiliary electrode clamp 8 is connected to the lower end of the adjusting stud 7 through an adjusting mechanism 9.
Wherein, install adjusting stud 7 and four guide posts 6 on the support frame 2, guide post 6 can be dismantled fixed connection and on support frame 2, and the lower extreme top of guide post 6 is in the upper end of bottom plate 11.
The electrode clamp 4 comprises a baffle plate 41 and a screwing bolt 42, the baffle plate 41 is fixedly connected to the lower end of the bottom plate 11, the screwing bolt 42 is in threaded connection with the baffle plate 41, the upper end of the screwing bolt 42 is attached to the working electrode 5, and the working electrode 5 is attached to the lower end of the first hole 12.
The auxiliary electrode clamp 8 comprises a connecting sleeve 81, an adjusting plate 82, a sample upper support 83, a sample lower support 84, an auxiliary electrode 85 and a locking bolt 86; the lower extreme of adapter sleeve 81 passes through bolt and connects gradually sample upper support 83 and regulating plate 82, four slide holes have been seted up on the surface of regulating plate 82, four guide post 6 run through respectively in a slide hole, sample upper support 83 and sample lower support 84 threaded connection, the temple lower extreme of sample lower support 84 is equipped with mounting groove two, the porose two 87 of lower extreme intercommunication of mounting groove two, auxiliary electrode 85 is located the inside of mounting groove two and auxiliary electrode 85 is located the upper end of hole two 87, locking bolt 86 threaded connection supports 83 on the sample, and the laminating of locking bolt 86 is in auxiliary electrode 85's upper end, working electrode 5 and auxiliary electrode 85 are just to setting up, the middle part of regulating plate 82 is equipped with the mounting hole, support 83 is located the mounting hole on the sample.
Wherein, the opening of the electrolytic bath 1 is provided with an auxiliary supporting plate 14, the middle part of the auxiliary supporting plate 14 is provided with a large hole, the periphery of the large hole is provided with at least two small holes, and the size of the adjusting plate 82 is smaller than that of the large hole of the auxiliary supporting plate 14.
Wherein, a sealing gasket is arranged in front of the working electrode 5 and the bottom plate 11, a sealing gasket is arranged between the auxiliary electrode 85 and the sample lower support 84, a sealing gasket is arranged between the sample upper support 83 and the sample lower support 84 which are in threaded fit, and a sealing gasket is arranged between the sample upper support 83 and the connecting sleeve 81.
The adjusting mechanism 9 comprises a thrust bearing 91, a bearing seat 92, a sleeve 93 and a locking nut 94, the bearing seat 92 is in threaded connection with the upper end of the connecting sleeve 81, the shoulder of the bearing seat 92 is provided with three holes 95, and the locking bolt 86 can be connected with a lead passing through the three holes 95 and is communicated with the electrochemical workstation.
The adjusting stud 7, the adjusting mechanism 9, the connecting sleeve 81, the locking bolt 86, the central hole of the sample upper support 83, the mounting hole of the adjusting plate 82, the second hole 87, the first hole 12 and the tightening bolt 42 are coaxial, and the adjusting stud 7, the locking bolt 86 and the tightening bolt 42 are made of metal materials; the positions of the working electrode 5 and the auxiliary electrode 85 may be interchanged.
Principle of operation
When an electrochemical test is carried out, the positions and the distances of a working electrode 5 and an auxiliary electrode 85 are fixed and adjusted, the working electrode 5 is tightly pressed on a bottom plate 11 by screwing a bolt 42, a hole 12 is in a seamless sealing state, the auxiliary electrode 85 is tightly locked by a locking bolt 86 penetrating through a threaded hole in the center of a sample upper support 83, and an auxiliary electrode clamp 8 below a rotary stud 7 is moved up and down by rotating a handle of the rotary stud 7 so as to adjust the distance between the working electrode 5 and the auxiliary electrode 85; if a reference electrode is needed, the reference electrode is inserted into the electrolyte in the access slot 1 from a small hole on the auxiliary support plate 14, and the electrode is connected to an electrochemical workstation through a lead wire, so that an electrochemical experiment can be carried out.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (4)
1. A general electrolytic cell for electrochemical test comprises an electrolytic cell (1), wherein the upper end of the electrolytic cell (1) is fixedly connected with a support frame (2), and the lower end of the electrolytic cell (1) is fixedly connected with a base (3), and is characterized in that a first hole (12) is formed in the surface of a bottom plate (11) of the electrolytic cell (1), the lower end of the first hole (12) is communicated with a first mounting groove, a working electrode (5) is arranged in the first mounting groove, an electrode clamp (4) is arranged outside the working electrode (5), the electrode clamp (4) is fixed at the lower end of the bottom plate (11), and a drain hole (13) is formed at the position where the bottom plate (11) is adjacent to the side wall of the electrolytic cell (1); an adjusting stud (7) is mounted on the support frame (2), the adjusting stud (7) is in threaded connection with the support frame (2), a handle is fixedly connected to the upper end of the adjusting stud (7), the lower end of the adjusting stud (7) is connected with an auxiliary electrode clamp (8) through an adjusting mechanism (9), and four guide posts (6) are further mounted on the support frame (2);
the auxiliary electrode clamp (8) comprises a connecting sleeve (81), a regulating plate (82), a sample upper support (83), a sample lower support (84), an auxiliary electrode (85) and a locking bolt (86); the lower end of the connecting sleeve (81) is sequentially connected with a sample upper support (83) and an adjusting plate (82) through bolts, a mounting hole is formed in the middle of the adjusting plate (82), the sample upper support (83) is located in the mounting hole, four sliding holes are formed in the surface of the adjusting plate (82), four guide posts (6) penetrate through one sliding hole respectively, the sample upper support (83) is in threaded connection with a sample lower support (84), a mounting groove II is formed in the lower end of the temporal part of the sample lower support (84), the lower end of the mounting groove II is communicated with a hole II (87), an auxiliary electrode (85) is located inside the mounting groove II, an auxiliary electrode (85) is located at the upper end of the hole II (87), a locking bolt (86) is in threaded connection with the sample upper support (83), the locking bolt (86) is attached to the upper end of the auxiliary electrode (85), and the working electrode (5) and the auxiliary electrode (85) are arranged oppositely;
an auxiliary supporting plate (14) is arranged at the opening of the electrolytic cell (1), a large hole is formed in the middle of the auxiliary supporting plate (14), at least two small holes are formed around the large hole, and the size of the adjusting plate (82) is smaller than that of the large hole of the auxiliary supporting plate (14);
be equipped with seal ring between working electrode (5) and bottom plate (11), be equipped with seal ring between auxiliary electrode (85) and sample under bracing (84), be equipped with seal ring on screw-thread fit's the sample between support (83) and sample under bracing (84), be equipped with seal ring on the sample between support (83) and adapter sleeve (81).
2. The universal electrolytic cell for electrochemical tests according to claim 1, characterized in that said guide posts (6) are removably and fixedly connected to the support frame (2), the lower ends of said guide posts (6) resting on the upper end of the bottom plate (11).
3. The general electrolytic cell for electrochemical tests according to claim 1 or 2, characterized in that the electrode clamp (4) comprises a baffle plate (41) and a tightening bolt (42), the baffle plate (41) is fixedly connected to the lower end of the bottom plate (11), the tightening bolt (42) is in threaded connection with the baffle plate (41), the upper end of the tightening bolt (42) is attached to the working electrode (5), and the working electrode (5) is attached to the lower end of the first hole (12).
4. The universal electrolytic cell for electrochemical tests as claimed in claim 1, characterized in that the adjusting mechanism (9) comprises a thrust bearing (91), a bearing seat (92), a sleeve (93) and a lock nut (94), the bearing seat (92) is connected with the upper end of the connecting sleeve (81) through a bolt, and the shoulder of the bearing seat (92) is provided with a hole III (95).
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