CN110988063A - Electrochemical test electrode system for realizing deep-sea high-pressure high-flow-rate aqueous solution system - Google Patents
Electrochemical test electrode system for realizing deep-sea high-pressure high-flow-rate aqueous solution system Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 70
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 38
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 38
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention relates to the field of electrochemical testing of deep-sea high-pressure high-flow-rate aqueous solution systems, in particular to an electrode system for realizing electrochemical testing of deep-sea high-pressure high-flow-rate aqueous solution systems. The working electrode is designed into a tubular structure suitable for an electrochemical testing device in a deep-sea high-flow-rate and high-pressure environment, and the size of the working electrode is adjusted according to the flow rate requirement. The connecting member includes: the device comprises a connecting flange, a sealing washer, an insulating sealing pipe, a copper connecting rod, a locking screw, a connecting nut, a compression washer, a compression nut, a compression sleeve, a working electrode, a sleeve, a welding short section, a conical transition section and the like; the counter and reference electrode core components include: the electrode assembly comprises a counter electrode body, a reference electrode body, an anti-scouring component and a sealing component. The invention meets the requirements of the sealing performance of the testing environment and the electrochemical testing precision, and is used for researching the corrosion process and mechanism in the deep-sea high-flow-rate and high-pressure environment.
Description
Technical Field
The invention relates to the field of electrochemical testing of deep-sea high-pressure high-flow-rate aqueous solution systems, in particular to an electrode system for realizing electrochemical testing under a deep-sea high-pressure high-flow-rate aqueous solution system.
Background
Abundant resources are stored in the deep sea, and the development and utilization of the deep sea resources have wide development prospect. With the detection and development of marine resources, the deep sea environment has higher and higher requirements on the performance of materials, wherein the corrosion resistance of the materials under the high flow speed and high pressure environment is an important performance index for the design of the materials for the deep sea. The evaluation of the corrosion performance of the material under the environment of simulating high flow velocity and high pressure in deep sea becomes a key problem to be solved urgently.
The electrochemical testing technology can monitor the corrosion process of the metal material in the environment in situ and evaluate the corrosion resistance of the metal material at the same time. However, the high flow rate and high pressure water environment conditions are harsh, so that the online electrochemical test in the test section is difficult to realize, and the requirements on the design of the three-electrode test section and the preparation process of each electrode are high, so that the realization is difficult. At present, the problem that most of domestic research equipment medium-high water pressure high flow rate test sections generally face is that in-situ electrochemical test can not be carried out, and the problem that the test sections generally face simultaneously is that sealing performance is poor, can not guarantee the test stability under the higher pressure, more can not carry out the stable work under the environment such as high flow rate, long-time.
Disclosure of Invention
The invention aims to provide an electrode system for realizing electrochemical test under a high-pressure high-flow-rate aqueous solution system for simulating a deep sea environment, solves the problem of in-situ electrochemical test of metal and a coating under the high-pressure high-flow-rate aqueous solution environment, and is suitable for electrochemical test of metal by coating in-situ corrosion behavior analysis.
The technical scheme of the invention is as follows:
an electrochemical test electrode system for realizing deep sea high-pressure high-flow-rate aqueous solution system, which comprises: the counter electrode, the reference electrode, the working electrode and the connecting part are matched with equipment to operate; wherein, the connecting part includes: seal ring A, pressure washer, lock screw, sleeve pipe, insulating seal tube, pressure sleeve pipe A, gland nut, coupling nut, welding nipple joint A, copper connective bar, welding nipple joint B, welding nipple joint C, seal ring B, pressure sleeve pipe B, concrete structure is as follows:
a sleeve is arranged on the outer side of a horizontally arranged tubular working electrode, a gap is reserved between the working electrode and the sleeve, insulating sealing pipes are respectively arranged between the working electrode and two ends of the sleeve, the working electrode and the sleeve are connected with and can be detached from the insulating sealing pipes, and the working electrode is fixed together with the insulating sealing pipes through the sleeve;
the two connecting nuts are symmetrically arranged at two ends of the sleeve, the center of each connecting nut is provided with a columnar hole with the middle diameter smaller than the diameters of the two sides, the columnar hole with the smaller middle diameter is opposite to the central hole of the tubular working electrode and has the same diameter, and the inner threads are respectively arranged on the inner side walls of the columnar holes with the larger diameters of the two sides; the two ends of the sleeve are provided with external threads matched with the connecting nuts, one end of each connecting nut is respectively connected with the external threads at one end of the sleeve through internal threads, and the connecting nuts, the sleeve and the insulating sealing tube are in sealing connection with the working electrode;
a compression washer is arranged in a columnar hole with a larger diameter at the other end of the connecting nut, a compression sleeve A is inserted and tightly contacted with the compression washer, the compression nut is tightly installed between the inner side wall of the columnar hole and the compression sleeve A, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut through internal threads, a flange is arranged at one end of the compression sleeve A extending into the columnar hole, and the end of the compression nut extending into the columnar hole compresses the flange to fix one end of the compression sleeve A and is hermetically connected with the connecting nut through the compression washer, the compression sleeve A and the compression nut;
a compression washer is arranged in a columnar hole with a larger diameter at the other end of the connecting nut, a compression sleeve B is inserted and tightly contacted with the compression washer, the compression nut is tightly installed between the inner side wall of the columnar hole and the compression sleeve B, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut through internal threads, a flange is arranged at one end of the compression sleeve B extending into the columnar hole, and the end of the compression nut extending into the columnar hole compresses the flange to fix one end of the compression sleeve B and is hermetically connected with the connecting nut through the compression washer, the compression sleeve B and the compression nut;
the middle opening of the side face of the sleeve is upward, a welding platform is arranged around the opening, a welding short section A is welded on the welding platform, and the port of the welding short section A is downward and is opposite to the central opening of the side face of the sleeve and is welded; the locking screw is of a tubular structure, internal threads are arranged on the inner side wall of the locking screw, and the copper connecting rod extends into the locking screw and is connected with the locking screw through threads; the inner side wall of the welding short section A is provided with internal threads, the outer pipe wall of the locking screw is provided with external threads, and the locking screw extends into the welding short section A and is in threaded connection with the welding short section A;
two holes are formed in the lower portion of the side face of the compression sleeve B, a welding platform is arranged around each hole, and a welding short section B and a welding short section C are welded on the welding platforms respectively; a sealing washer B is arranged in the welding short section C, the counter electrode extends into the welding short section C and is tightly contacted with the sealing washer B, the counter electrode is connected with the inner side wall of the welding short section C through threads, and the sealing between the counter electrode and the pressing sleeve B is realized through the sealing washer B; set up seal ring A in the welding nipple joint B, the reference electrode extends in the welding nipple joint B and with seal ring A in close contact with, the reference electrode passes through threaded connection with the inside wall of welding nipple joint B, realizes sealing through seal ring A between reference electrode and the compression sleeve pipe B.
The electrochemical test electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system comprises a counter electrode, a counter electrode and a counter electrode, wherein the counter electrode comprises a copper wire, a 316L locking screw, an anti-scouring net, a platinum sheet and epoxy resin, and the counter electrode has the following specific structure: a platinum sheet is welded at one end of a copper conducting wire serving as a counter electrode, the copper conducting wire and the platinum sheet extend into a central hole of the 316L locking screw, the copper conducting wire, the platinum sheet and the central hole are sealed through epoxy resin, the platinum sheet is located near one end of the central hole, and the platinum sheet and the 316L locking screw are kept insulated; an anti-scouring net is arranged at one end of the central hole, and a gap is reserved between the platinum sheet and the anti-scouring net correspondingly; wherein, the platinum sheet is used as a counter electrode main body as a reference electrode main body, and the anti-scouring net and the epoxy resin are respectively used as an anti-scouring part and a sealing part;
the reference electrode comprises a copper wire, a 316L locking screw, an anti-scouring net, a solid Ag/AgCl electrode plate and epoxy resin, and the reference electrode has the following specific structure: the reference electrode is a copper wire, one end of the copper wire is connected with a solid Ag/AgCl electrode plate, the copper wire and the solid Ag/AgCl electrode plate extend into a central hole of the 316L locking screw, the copper wire, the solid Ag/AgCl electrode plate and the central hole are sealed through epoxy resin, the solid Ag/AgCl electrode plate is located near one end of the central hole, and the solid Ag/AgCl electrode plate and the 316L locking screw are insulated; an anti-scouring net is arranged at one end of the central hole, and a gap is reserved between the solid Ag/AgCl electrode plate and the anti-scouring net correspondingly; wherein, the solid Ag/AgCl electrode slice is used as a reference electrode main body, and the anti-scouring net and the epoxy resin are respectively used as an anti-scouring part and a sealing part.
The electrochemical test electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system is characterized in that a conical transition section is arranged in an inner cavity at one end of a compression sleeve A, a conical hole is formed in the center of the conical transition section, one end of the conical hole is opposite to a columnar hole with a smaller middle diameter and has the same diameter, and the diameter of the other end of the conical hole is the same as the inner diameter of the compression sleeve A; mounting a flange at the other end of the compression sleeve A as a connecting flange;
a conical transition section is arranged in an inner cavity at one end of the compression sleeve B, a conical hole is formed in the center of the conical transition section, one end of the conical hole is opposite to the columnar hole with a smaller middle diameter and has the same diameter, and the diameter of the other end of the conical hole is the same as the inner diameter of the compression sleeve B; and installing a flange at the other end of the compression sleeve B as a connecting flange.
The electrochemical test electrode system under the deep-sea high-pressure high-flow-rate aqueous solution system is realized, the upper part of the copper connecting rod is cylindrical, and the surface of the copper connecting rod is provided with external threads; the lower end of the copper connecting rod is in an arch bridge shape and is attached to the outer wall of the working electrode.
According to the electrochemical testing electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system, the welding short section A, the welding short section B and the welding short section C are all tubular structures with the inner diameter of 20mm, the outer diameter of 24mm and the height of 24mm, and the distances between the welding short section B and the welding short section C and the vertical center of the working electrode are respectively 30mm and 40 mm; meanwhile, the sealing planes with the widths of 4mm are processed at the bottoms of the welding short section B and the welding short section C, so that sealing with the sealing washer A and the sealing washer B is facilitated.
The electrochemical test electrode system under the deep-sea high-pressure high-flow-rate aqueous solution system is realized, the welding short section A, the welding short section B and the welding short section C are made of 316L stainless steel which is the same as the sleeve and the compression sleeve B.
The electrochemical test electrode system under the deep sea high-pressure high-flow-rate aqueous solution system is realized, the sealing washer A and the sealing washer B are made of temperature-resistant fluororubber sealing rings, and the specification and the size are as follows: the outer diameter is 20mm, the inner diameter is 17mm, and the thickness is 3 mm.
The electrochemical test electrode system under the deep sea high-pressure high-flow-rate aqueous solution system is realized, the insulating sealing tube is made of polyether-ether-ketone, the compression washer is made of tetrafluoroethylene, the copper connecting rod is made of pure copper, and the locking screw is made of polytetrafluoroethylene.
The invention has the advantages and beneficial effects that:
the invention has simple structure and convenient installation, has very strong universality for the circulation type simulation equipment, the design of the working electrode can well match with circulation type high-flow-rate and high-pressure equipment, and the design of a three-electrode system can realize in-situ electrochemical measurement in deep sea high-flow-rate and high-pressure environment. The invention meets the requirements of testing environment tightness and electrochemical testing resolution and can be used for researching corrosion processes and mechanisms in deep sea high-flow-rate and high-pressure environments.
Drawings
FIG. 1 is a schematic structural view of an electrochemical test electrode system according to the present invention. In the figure, 1, a counter electrode; 2. a reference electrode; 3. sealing washer A; 4. a compression washer; 5. locking screws; 6. a working electrode; 7. a sleeve; 8. an insulating seal tube; 9. compressing the sleeve A; 10. a flange; 11. a compression nut; 12. a connecting nut; 13. welding a short section A; 14. a copper connecting rod; 15. a tapered transition section; 16. welding a short section B; 17. welding a short section C; 18. a sealing washer B; 19. compressing the sleeve B.
FIGS. 2 a-2 b are schematic diagrams of a counter electrode (FIG. 2a) and a reference electrode (FIG. 2b), respectively, of an electrochemical test electrode system of the invention. In the figure, 20 copper wires; 21.316L locking screw; 22. an anti-scouring net; 23. a platinum sheet; 24. an epoxy resin; 25. solid Ag/AgCl electrode plate.
FIG. 3 is a graph of Q235 potential versus time at a pressure of 3MPa and various flow rates. In the figure, the abscissa Time represents the Time(s) and the ordinate E (V vs Ag/AgCl) represents the open circuit potential of the test material Q235.
FIGS. 4 a-4 b are Nernst (Nyquist) and Bode (FIG. 4b) spectra of the electrochemical impedance spectrum of Q235 at different times under the condition of a pressure of 3MPa and a flow rate of 3 m/s. In FIG. 4a, the abscissa Z' represents the real part of the impedance (Ω. cm)2) The ordinate-Z' represents the imaginary impedance (Ω · cm)2). In FIG. 4b, the Frequency (Hz) is represented by the abscissa Frequency, and the modulus of the impedance (Ω. cm) is represented by the left ordinate | Z |2) The right ordinate Phase angle represents the Phase angle (deg.) of the impedance.
Detailed Description
As shown in figure 1, the electrochemical test electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system mainly comprises: the counter electrode 1, the reference electrode 2, the working electrode 6 and the connecting part are matched with equipment to operate; wherein, the connecting part is provided with: sealing washer A3, pressure washer 4, lock screw 5, sleeve pipe 7, insulating sealed tube 8, pressure sleeve pipe A9, flange 10, gland nut 11, coupling nut 12, welding nipple A13, copper connective bar 14, toper changeover portion 15, welding nipple B16, welding nipple C17, sealing washer B18, pressure sleeve pipe B19 etc. specific structure is as follows:
the working electrode 6 (working section) is designed into a tubular shape suitable for an electrochemical testing device in a high flow speed and high pressure environment, and the inner diameter, the outer diameter and the length of the working electrode 6 are respectively 6mm, 12mm and 60 mm.
The sleeve 7 is arranged on the outer side of the horizontally arranged tubular working electrode 6, a gap is reserved between the working electrode 6 and the sleeve 7, the insulating sealing pipes 8 are respectively arranged between the two ends of the working electrode 6 and the sleeve 7, the insulating sealing pipes 8 are made of polyether-ether-ketone PEEK, certain plastic deformation is guaranteed to guarantee sealing, certain rigidity and insulating property are guaranteed, the working electrode 6, the sleeve 7 and the insulating sealing pipes 8 are connected in a sealing mode and can be detached, the working electrode 6 is fixed together with the insulating sealing pipes 8 through the sleeve 7, and therefore the working electrode can be guaranteed to be insulated from a simulation system when an electrochemical test is carried out.
Two connecting nuts 12 are symmetrically arranged at two ends of the sleeve 7, a columnar hole with the middle diameter smaller than the diameters of two sides is arranged in the center of each connecting nut 12, the columnar hole with the smaller middle diameter is opposite to the central hole of the tubular working electrode 6 and has the same diameter, and internal threads are respectively arranged on the inner side walls of the columnar holes with the larger diameters of two sides; the both ends of sleeve pipe 7 are equipped with the external screw thread that can match with coupling nut 12, and every coupling nut 12 one end is passed through the internal thread and is connected with the external screw thread of sleeve pipe 7 one end respectively, through coupling nut 12, sleeve pipe 7, insulating sealed tube 8 and working electrode 6 sealing connection.
A compression washer 4 is arranged in a columnar hole with a larger diameter at the other end of the connecting nut 12, a compression sleeve A9 is inserted and tightly contacted with the compression washer 4, a compression nut 11 is tightly arranged between the inner side wall of the columnar hole and the compression sleeve A9, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut 11 through internal threads, a flange is arranged at one end of the compression sleeve A9 extending into the columnar hole, the flange is compressed at one end of the compression nut 11 extending into the columnar hole, so that one end of the compression sleeve A9 is fixed, the compression washer 4 (made of tetrafluoroethylene), the compression sleeve A9 and the compression nut 11 are in sealing connection with the connecting nut 12, and the compression washer 4 mainly plays a sealing role. Set up toper changeover portion 15 in compressing tightly sleeve pipe A9's the one end inner chamber, reduce the local flow state change that the reducing caused through the toper type changeover portion, toper 15 center formation taper hole, the one end of taper hole is relative and the diameter is the same with the less column hole of middle diameter, the other end diameter of taper hole is the same with compressing tightly sleeve pipe A9's internal diameter. And mounting the flange 10 at the other end of the compression sleeve A9, and selecting the flange 10 with the diameter of 120mm as a connecting flange.
A compression washer 4 is arranged in a columnar hole with a larger diameter at the other end of the connecting nut 12, a compression sleeve B19 is inserted and tightly contacted with the compression washer 4, a compression nut 11 is tightly arranged between the inner side wall of the columnar hole and the compression sleeve B19, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut 11 through internal threads, a flange is arranged at one end of the compression sleeve B19 extending into the columnar hole, the flange is compressed at one end of the compression nut 11 extending into the columnar hole, so that one end of the compression sleeve B19 is fixed, the compression washer 4 (made of tetrafluoroethylene), the compression sleeve B19 and the compression nut 11 are in sealing connection with the connecting nut 12, and the compression washer 4 mainly plays a sealing role. The pressing sleeve B19 is characterized in that a conical transition section 15 is arranged in an inner cavity of one end of the pressing sleeve B19, a conical hole is formed in the center of the conical transition section 15, one end of the conical hole is opposite to a cylindrical hole with a small middle diameter, the diameter of the cylindrical hole is the same as that of the cylindrical hole, and the diameter of the other end of the conical hole is the same as that of the inner diameter of the pressing sleeve B19. And mounting the flange 10 at the other end of the compression sleeve B19, and selecting the flange 10 with the diameter of 120mm as a connecting flange.
The pipeline connecting parts of the pressing sleeve A9, the pressing sleeve B19 and the working electrode 6 are provided with a conical transition section 15, the conical transition section 15 is designed to be an inclined plane with a certain gradient (15 degrees) through simulation calculation, so that the influence of the flow state rapid change generated after the pipeline is reduced on the test is relieved, the conical transition section 15 can be changed into different gradients and diameters according to the test requirement, and the pipe diameters of the connecting parts of the pressing sleeve A9 and the pressing sleeve B19 and the working electrode 6 are the same through the conical transition section 15.
Welding nipple A13, welding nipple B16, welding nipple C17 are internal diameter 20mm, external diameter 24mm, high 24 mm's tubular structure, and the material of welding nipple A13, welding nipple B16, welding nipple C17 is selected and is pressed down the same steel 316L stainless steel of sleeve pipe 7 and the same steel 316L stainless steel of sleeve pipe B19, wherein:
the trompil up in the middle of the side of sleeve pipe 7 to make 2mm high welded platform around the trompil, the welding has welded nipple joint A13 on the welded platform, and the port of welded nipple joint A13 is relative and the welding with the central trompil of sleeve pipe 7 side down. The locking screw 5 is of a tubular structure, internal threads are arranged on the inner side wall of the locking screw, and the copper connecting rod 14 extends into the locking screw 5 and is connected with the locking screw 5 through threads; the inside wall of welding nipple joint A13 is equipped with the internal thread, and locking screw 5's outer pipe wall is equipped with the external screw thread, and locking screw 5 extends in welding nipple joint A13 to with welding nipple joint A13 threaded connection.
The copper connecting rod 14 is made of pure copper, the upper end of the copper connecting rod 14 is designed into a protruding cylinder, the surface of the copper connecting rod is threaded, an electrochemical testing device is convenient to connect, the lower end of the copper connecting rod is designed into an arch bridge shape and is attached to the outer wall of the working electrode 6, in order to reduce the influence of contact resistance on testing, the contact area between the lower end of the copper connecting rod and the working electrode 6 is as large as possible, and the contact resistance between the working electrode 6 and the copper connecting rod 14 is detected after connection is completed and is smaller than 0.3 omega; the material of locking screw 5 is polytetrafluoroethylene, and the inside perpendicular punching (diameter 6mm) of locking screw 5 guarantees that copper connective bar 14 can insert inside locking screw 5, also guarantees the compactness of copper connective bar 14 and working electrode 6 contact simultaneously.
Two holes are formed in the lower portion of the side face of the pressing sleeve B19, a welding platform with the height of 2mm is arranged around each hole, a welding short section B16 and a welding short section C17 are respectively welded on the welding platform, and sealing planes with the width of 4mm are machined at the bottoms of the welding short section B16 and the welding short section C17; a sealing washer B18 is arranged in the welding short section C17, the counter electrode 1 extends into the welding short section C17 and is tightly contacted with the sealing washer B18, the counter electrode 1 is connected with the inner side wall of the welding short section C17 through threads, and the sealing between the counter electrode 1 and the pressing sleeve B19 is realized through the sealing washer B18; a sealing washer A3 is arranged in the welding short section B16, the reference electrode 2 extends into the welding short section B16 and is in close contact with the sealing washer A3, the reference electrode 2 is in threaded connection with the inner side wall of the welding short section B16, and the sealing between the reference electrode 2 and the pressing sleeve B19 is achieved through the sealing washer A3. Wherein, the material of seal ring A3, seal ring B18 is rubber, and its specification and size is: the outer diameter is 20mm, the inner diameter is 17mm, and the thickness is 3 mm. The welding short joint B16 and the welding short joint C17 are respectively 30mm and 40mm away from the vertical center of the working electrode 6 (namely the central axis of the copper connecting rod 14). Meanwhile, the sealing planes with the widths of 4mm are machined at the bottoms of the welding short section B16 and the welding short section C17, so that good sealing is formed between the sealing planes and the sealing gaskets A3 and B18.
As shown in fig. 2a, the counter electrode includes a copper wire 20, a 316L locking screw 21, an anti-erosion mesh 22, a platinum sheet 23, an epoxy resin 24, and the like, and the specific structure is as follows: one end of the copper wire 20 is welded with a platinum sheet 23, the copper wire 20 and the platinum sheet 23 extend into a central hole of the 316L locking screw 21, the copper wire 20, the platinum sheet 23 and the central hole are sealed through epoxy resin 24, the platinum sheet 23 is located near one end of the central hole, and the platinum sheet 23 and the 316L locking screw 21 are kept insulated. An anti-scouring net 22 is arranged at one end of the central hole, and a gap is reserved between the platinum sheet 23 and the anti-scouring net 22 correspondingly. The platinum sheet 23 is used as a counter electrode main body, and the erosion prevention net 22 and the epoxy resin 24 are an erosion prevention component and a sealing component, respectively.
As shown in fig. 2b, the reference electrode comprises a copper wire 20, a 316L locking screw 21, an anti-scouring mesh 22, a solid Ag/AgCl electrode sheet 25, epoxy resin 24 and the like, and the specific structure is as follows: one end of the copper lead 20 is welded with a solid Ag/AgCl electrode plate 25, the copper lead 20 and the solid Ag/AgCl electrode plate 25 extend into a central hole of the 316L locking screw 21, the copper lead 20, the solid Ag/AgCl electrode plate 25 and the central hole are sealed through epoxy resin 24, the solid Ag/AgCl electrode plate 25 is located near one end of the central hole, and the solid Ag/AgCl electrode plate 25 and the 316L locking screw 21 are kept insulated. An anti-scouring net 22 is arranged at one end of the central hole, and a gap is reserved between the solid Ag/AgCl electrode slice 25 and the anti-scouring net 22 correspondingly. Wherein, the solid Ag/AgCl electrode slice 25 is used as a reference electrode main body, and the anti-scouring net 22 and the epoxy resin 24 are respectively used as an anti-scouring part and a sealing part.
The manufacturing requirements of the electrode are as follows: the platinum sheet 23 with the diameter of 10mm, the thickness of 2mm and the purity of 99 wt% is selected for the electrodes of the counter electrode, the platinum sheet 23 is welded with the copper lead 20 with the length of 20cm, the copper lead 20 is ensured to be in the center of the platinum sheet 23, contact with other metals is avoided when the copper lead is sealed by epoxy resin 24, and the connection resistance is as small as possible. The welded platinum electrode (platinum sheet 23) is vertically placed into a 316L locking screw 21, the front end of the 316L locking screw 21 is sealed by a sealing sheet with the thickness of 3mm and the diameter of 10mm, then epoxy resin 24 is poured into the center hole of the 316L locking screw 21, the platinum sheet 23 and the copper lead 20 are sealed and fixed, the sealing sheet is removed after a sealing box is dried for 48h, and a metal platinum sheet is exposed; in order to prevent the platinum sheet 23 from being washed by the test medium during the test, an anti-scouring net 22 made of nylon with the thickness of 2mm is fixed above the platinum sheet 23, and the platinum sheet 23 is not in contact with the anti-scouring net 22.
The manufacturing requirements of the reference electrode are as follows: the reference electrode is characterized in that Ag sheets with the diameter of 9mm, the thickness of 2mm and the purity of 99 wt% are selected as electrodes of the reference electrode, AgCl powder is coated outside the reference electrode and is subjected to hot-pressing sintering to form a solid Ag/AgCl electrode piece 25, the solid Ag/AgCl electrode piece is welded with a copper wire 20 with the length of 20cm (holes are formed in the Ag/AgCl electrode piece, the copper wire 20 is only welded with metal silver), the copper wire 20 is ensured to be in the middle position of the solid Ag/AgCl electrode piece 25, contact with other metals when the solid Ag/AgCl electrode piece is sealed by epoxy resin 24 is avoided. The welded reference electrode (solid Ag/AgCl electrode plate 25) is vertically placed in a 316L locking screw 21, the front end of the 316L locking screw 21 is sealed by a sealing plate with the thickness of 3mm and the diameter of 10mm, then epoxy resin 24 is poured into a center hole of the 316L locking screw 21, the solid Ag/AgCl electrode plate 25 and a copper wire 20 are sealed and fixed, the sealing plate is removed after a sealing box is dried for 48 hours, and the solid Ag/AgCl electrode is exposed; in order to prevent the solid Ag/AgCl electrode plate 25 from being washed by a test medium during the test, an anti-scouring net 22 made of nylon with the thickness of 2mm is fixed above the solid Ag/AgCl electrode plate 25, and the solid Ag/AgCl electrode plate 25 is not in contact with the anti-scouring net 22.
The invention is further illustrated by the following figures and examples, which are not intended to limit the invention in any way.
The working electrode used in the following examples was a Q235 low carbon steel meeting the national standard, and was carried out under simulated seawater with a mass fraction of 3.5 wt% NaCl.
Example 1
In this example, Q235 steel with an inner diameter of 6mm, an outer diameter of 12mm, and a length of 61mm was used as a working electrode, the inner diameter of the tube of the working electrode was polished, the surface was polished with 120#, 240#, 400#, 600# and 800# sandpaper, and then washed with deionized water and absolute ethanol and dried. The test solution is simulated seawater of 3.5 wt% NaCl, the test temperature is 25 ℃, the test pressure is 3MPa, the flow rates are 3, 5 and 9m/s respectively, and the electrochemical open-circuit potential monitoring is carried out for 6 hours.
The test results are shown in fig. 3, and it can be seen from fig. 3 that there is a decreasing process of the open-circuit potential of Q235 under different flow rates, because the oxide on the surface of the material is rapidly damaged by the fluid, so that the potential decreases to different degrees, and the degree of the potential decrease is observed to be larger as the flow rate increases. With the prolonging of the scouring time, after the open-circuit potential of the Q235 rises slightly under the condition of low flow rate (3m/s and 5m/s) under the pressure of 3MPa, the open-circuit potential tends to be in a stable state, which indicates that corrosion products are gradually formed on the surface of the Q235 under the condition of low flow rate, a relatively stable rust layer and a double electric layer structure are formed, and the corrosion potential also tends to be stable; and under the condition of high flow rate (9m/s), the open-circuit potential of the Q235 shows a two-stage descending trend and finally tends to be stable, wherein the descending speed is slow in the time period of 0-9000 s and the descending speed is rapid in the time period of 9000-13000 s, which indicates that the corrosion product formed on the surface of the Q235 under the condition of high flow rate is difficult, and the stable open-circuit potential can be formed in a long time. The open circuit potential of the material can reflect the corrosion tendency of the material under the environment to a certain extent, namely the corrosion tendency of Q235 under the condition of low flow rate (3m/s and 5m/s) is low under the condition of higher flow rate, wherein the corrosion tendency is severe.
Example 2
In this example, Q235 steel with an inner diameter of 6mm, an outer diameter of 12mm, and a length of 61mm was used as a working electrode, the inner diameter of the tube of the working electrode was polished, the surface was polished with 120#, 240#, 400#, 600# and 800# sandpaper, and then washed with deionized water and absolute ethanol and dried. The test solution is 3.5 wt% NaCl aqueous solution, the test temperature is 25 ℃, the test pressure is 3MPa, the flow rates are respectively 3m/s, and the electrochemical impedance spectroscopy test for 8h is carried out.
The test results are shown in FIG. 4, and it can be seen from FIG. 4a that under the conditions of pressure of 3MPa and flow rate of 3m/s, the capacitive arc is slightly increased with the increase of the test time from the Nyquist plot of the electrochemical impedance spectrum of Q235 at different times, which indicates that the corrosion products are gradually formed on the surface of the sample but in a smaller amount. From fig. 4b, it can be seen that, from Bode plot of electrochemical impedance spectrum of Q235 at different times, the impedance modulus value is slightly increased with the increase of the test time, which indicates that the surface formation part corrosion product hinders the further occurrence of corrosion with the increase of the scouring time, and this phenomenon is consistent with the condition that the surface corrosion product increases with the increase of the test time to play a certain protection role on the substrate.
Claims (8)
1. An electrochemical test electrode system for realizing deep sea high-pressure high-flow-rate aqueous solution system is characterized by comprising: the counter electrode, the reference electrode, the working electrode and the connecting part are matched with equipment to operate; wherein, the connecting part includes: seal ring A, pressure washer, lock screw, sleeve pipe, insulating seal tube, pressure sleeve pipe A, gland nut, coupling nut, welding nipple joint A, copper connective bar, welding nipple joint B, welding nipple joint C, seal ring B, pressure sleeve pipe B, concrete structure is as follows:
a sleeve is arranged on the outer side of a horizontally arranged tubular working electrode, a gap is reserved between the working electrode and the sleeve, insulating sealing pipes are respectively arranged between the working electrode and two ends of the sleeve, the working electrode and the sleeve are connected with and can be detached from the insulating sealing pipes, and the working electrode is fixed together with the insulating sealing pipes through the sleeve;
the two connecting nuts are symmetrically arranged at two ends of the sleeve, the center of each connecting nut is provided with a columnar hole with the middle diameter smaller than the diameters of the two sides, the columnar hole with the smaller middle diameter is opposite to the central hole of the tubular working electrode and has the same diameter, and the inner threads are respectively arranged on the inner side walls of the columnar holes with the larger diameters of the two sides; the two ends of the sleeve are provided with external threads matched with the connecting nuts, one end of each connecting nut is respectively connected with the external threads at one end of the sleeve through internal threads, and the connecting nuts, the sleeve and the insulating sealing tube are in sealing connection with the working electrode;
a compression washer is arranged in a columnar hole with a larger diameter at the other end of the connecting nut, a compression sleeve A is inserted and tightly contacted with the compression washer, the compression nut is tightly installed between the inner side wall of the columnar hole and the compression sleeve A, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut through internal threads, a flange is arranged at one end of the compression sleeve A extending into the columnar hole, and the end of the compression nut extending into the columnar hole compresses the flange to fix one end of the compression sleeve A and is hermetically connected with the connecting nut through the compression washer, the compression sleeve A and the compression nut;
a compression washer is arranged in a columnar hole with a larger diameter at the other end of the connecting nut, a compression sleeve B is inserted and tightly contacted with the compression washer, the compression nut is tightly installed between the inner side wall of the columnar hole and the compression sleeve B, the inner side wall of the columnar hole is respectively connected with the external thread of the compression nut through internal threads, a flange is arranged at one end of the compression sleeve B extending into the columnar hole, and the end of the compression nut extending into the columnar hole compresses the flange to fix one end of the compression sleeve B and is hermetically connected with the connecting nut through the compression washer, the compression sleeve B and the compression nut;
the middle opening of the side face of the sleeve is upward, a welding platform is arranged around the opening, a welding short section A is welded on the welding platform, and the port of the welding short section A is downward and is opposite to the central opening of the side face of the sleeve and is welded; the locking screw is of a tubular structure, internal threads are arranged on the inner side wall of the locking screw, and the copper connecting rod extends into the locking screw and is connected with the locking screw through threads; the inner side wall of the welding short section A is provided with internal threads, the outer pipe wall of the locking screw is provided with external threads, and the locking screw extends into the welding short section A and is in threaded connection with the welding short section A;
two holes are formed in the lower portion of the side face of the compression sleeve B, a welding platform is arranged around each hole, and a welding short section B and a welding short section C are welded on the welding platforms respectively; a sealing washer B is arranged in the welding short section C, the counter electrode extends into the welding short section C and is tightly contacted with the sealing washer B, the counter electrode is connected with the inner side wall of the welding short section C through threads, and the sealing between the counter electrode and the pressing sleeve B is realized through the sealing washer B; set up seal ring A in the welding nipple joint B, the reference electrode extends in the welding nipple joint B and with seal ring A in close contact with, the reference electrode passes through threaded connection with the inside wall of welding nipple joint B, realizes sealing through seal ring A between reference electrode and the compression sleeve pipe B.
2. The system for realizing the electrochemical test electrode under the deep-sea high-pressure high-flow-rate aqueous solution system as claimed in claim 1, wherein the counter electrode comprises a copper wire, a 316L locking screw, an anti-scouring net, a platinum sheet and epoxy resin, and the specific structure is as follows: a platinum sheet is welded at one end of a copper conducting wire serving as a counter electrode, the copper conducting wire and the platinum sheet extend into a central hole of the 316L locking screw, the copper conducting wire, the platinum sheet and the central hole are sealed through epoxy resin, the platinum sheet is located near one end of the central hole, and the platinum sheet and the 316L locking screw are kept insulated; an anti-scouring net is arranged at one end of the central hole, and a gap is reserved between the platinum sheet and the anti-scouring net correspondingly; wherein, the platinum sheet is used as a counter electrode main body as a reference electrode main body, and the anti-scouring net and the epoxy resin are respectively used as an anti-scouring part and a sealing part;
the reference electrode comprises a copper wire, a 316L locking screw, an anti-scouring net, a solid Ag/AgCl electrode plate and epoxy resin, and the reference electrode has the following specific structure: the reference electrode is a copper wire, one end of the copper wire is connected with a solid Ag/AgCl electrode plate, the copper wire and the solid Ag/AgCl electrode plate extend into a central hole of the 316L locking screw, the copper wire, the solid Ag/AgCl electrode plate and the central hole are sealed through epoxy resin, the solid Ag/AgCl electrode plate is located near one end of the central hole, and the solid Ag/AgCl electrode plate and the 316L locking screw are insulated; an anti-scouring net is arranged at one end of the central hole, and a gap is reserved between the solid Ag/AgCl electrode plate and the anti-scouring net correspondingly; wherein, the solid Ag/AgCl electrode slice is used as a reference electrode main body, and the anti-scouring net and the epoxy resin are respectively used as an anti-scouring part and a sealing part.
3. The system for realizing the electrochemical test electrode in the deep-sea high-pressure high-flow-rate aqueous solution system according to claim 1, wherein a conical transition section is arranged in an inner cavity at one end of the pressing sleeve A, a conical hole is formed in the center of the conical transition section, one end of the conical hole is opposite to the columnar hole with a smaller middle diameter and has the same diameter, and the diameter of the other end of the conical hole is the same as the inner diameter of the pressing sleeve A; mounting a flange at the other end of the compression sleeve A as a connecting flange;
a conical transition section is arranged in an inner cavity at one end of the compression sleeve B, a conical hole is formed in the center of the conical transition section, one end of the conical hole is opposite to the columnar hole with a smaller middle diameter and has the same diameter, and the diameter of the other end of the conical hole is the same as the inner diameter of the compression sleeve B; and installing a flange at the other end of the compression sleeve B as a connecting flange.
4. The system for realizing the electrochemical test electrode in the deep-sea high-pressure high-flow-rate aqueous solution system according to claim 1, wherein the upper part of the copper connecting rod is cylindrical, and the surface of the copper connecting rod is provided with external threads; the lower end of the copper connecting rod is in an arch bridge shape and is attached to the outer wall of the working electrode.
5. The electrochemical test electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system according to claim 1, wherein the welding short section A, the welding short section B and the welding short section C are all tubular structures with the inner diameter of 20mm, the outer diameter of 24mm and the height of 24mm, and the distances between the welding short section B and the welding short section C and the vertical center of the working electrode are respectively 30mm and 40 mm; meanwhile, the sealing planes with the widths of 4mm are processed at the bottoms of the welding short section B and the welding short section C, so that sealing with the sealing washer A and the sealing washer B is facilitated.
6. The electrochemical test electrode system for realizing the deep-sea high-pressure high-flow-rate aqueous solution system according to claim 1 or 5, wherein the welding short section A, the welding short section B and the welding short section C are made of 316L stainless steel which is the same as the sleeve and the compression sleeve B.
7. The system for realizing the electrochemical test electrode under the deep-sea high-pressure high-flow-speed aqueous solution system according to claim 1, wherein the sealing gaskets A and B are made of temperature-resistant fluororubber sealing rings and have the specification and size as follows: the outer diameter is 20mm, the inner diameter is 17mm, and the thickness is 3 mm.
8. The system for realizing the electrochemical test electrode in the deep-sea high-pressure high-flow-rate aqueous solution system according to claim 1, wherein the insulating sealing tube is made of polyether ether ketone, the compression washer is made of tetrafluoroethylene, the copper connecting rod is made of pure copper, and the locking screw is made of polytetrafluoroethylene.
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