CN111323365A - Three-electrode corrosion sensor and manufacturing method thereof - Google Patents
Three-electrode corrosion sensor and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to the field of metal corrosion monitoring, and provides a three-electrode corrosion sensor and a manufacturing method thereof. The sensor includes: the device comprises a substrate, a first substrate and a second substrate, wherein a through hole is formed in the substrate; the reference electrode and the counter electrode are arranged on the front surface of the substrate and form a ring surrounding the through hole; the guard ring electrode is arranged on the front surface of the substrate and surrounds the reference electrode and the counter electrode; and the metal connecting sheet to be detected is arranged on the reverse side of the substrate and is used for connecting the sensor and the metal to be detected. The sensor has the advantages of convenient operation, good consistency and low manufacturing cost, and is suitable for industrial large-scale production.
Description
Technical Field
The invention relates to the field of metal corrosion monitoring, in particular to a three-electrode corrosion sensor and a manufacturing method thereof.
Background
The metal corrosion refers to a phenomenon that a metal material is damaged by a change of state caused by the action of a medium and a transformation into a new phase. Each year, metal corrosion causes significant economic losses, either directly or indirectly. According to statistics, the quantity of the metal scrapped due to corrosion in the world every year is equal to 1/4-1/3 of the annual yield of the metal. Therefore, monitoring of atmospheric corrosion of metals is very important. The traditional metal atmospheric corrosion monitoring method is a hanging piece method, and a sample piece made of metal to be evaluated is exposed in the atmosphere, the ocean and the soil environment and is taken back and weighed regularly. The method needs to establish exposure experiment station groups located in various regions, and has the problems of long data acquisition time interval, few data points, poor data consistency and stability, high data cost and the like.
The corrosion of metal is mostly the electrochemical corrosion process of metal in the electrolytic bath environment, which conforms to the general rule of electrochemistry. The method is characterized in that a metal to be tested is used as an anode of a primary battery, an inert electrode is used as a reference electrode and a counter electrode, and a linear polarization resistance is tested to calculate corrosion current under the environment of an electrolytic cell in which the metal to be tested is located. The linear polarization method is used for measuring the metal corrosion rate, has the advantages of high detection speed, high sensitivity, less limitation by objective conditions and the like, and is a nondestructive metal corrosion detection method.
Fig. 1 is a measurement schematic diagram of a three-electrode sensor in the prior art. As shown in fig. 1, a metal of the same material as the material to be measured is used as a Working Electrode (WE), a silver/silver chloride electrode or a saturated calomel electrode is used as a Reference Electrode (RE), a platinum electrode is used as a Counter Electrode (CE), and the three electrodes are placed in soil or water simulating a real environment for measurement. The method is a laboratory test method, the monitoring result can only be used as reference or for accelerated test, and the corrosion condition of the metal to be tested cannot be directly fed back.
Disclosure of Invention
The invention aims to provide a three-electrode corrosion sensor and a manufacturing method thereof, and aims to solve the technical problems in the prior art.
In one aspect, an embodiment of the present invention provides a three-electrode corrosion sensor, including: the device comprises a substrate, a first substrate and a second substrate, wherein a through hole is formed in the substrate; the reference electrode and the counter electrode are arranged on the front surface of the substrate and form a ring surrounding the through hole; the guard ring electrode is arranged on the front surface of the substrate and surrounds the reference electrode and the counter electrode; and the metal connecting sheet to be detected is arranged on the reverse side of the substrate and is used for connecting the sensor and the metal to be detected.
On the other hand, the embodiment of the invention also provides a manufacturing method of the sensor, and the manufacturing method is one of an etching method, a pressing method, an ink jet printing method and a sputtering method.
The invention has the beneficial effects that: the metal to be detected is used as a working electrode, a three-electrode system is formed by matching a reference electrode and a counter electrode of the sensor, the potentials of the counter electrode and the guard ring electrode are the same through a peripheral circuit, the current outside the sensor can not reach a current electrode, the electrode area of the metal to be detected is determined, the detection sensitivity is high, and the metal to be detected can be used outdoors for a long time. The sensor can be directly attached to the surface of metal for use, is convenient to operate, good in consistency and low in manufacturing cost, and is suitable for industrial large-scale production.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed for the embodiments or the prior art descriptions 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 diagram of a three-electrode sensor in the prior art
Fig. 2(a) is a front view of a circular hole three-electrode corrosion sensor provided by an embodiment of the present invention.
Fig. 2(b) is a back view of a circular hole three-electrode corrosion sensor provided by an embodiment of the invention.
The corrosion sensor comprises a three-electrode corrosion sensor 1, a substrate 2, a through hole 3, a reference electrode 4, a counter electrode 5, a counter electrode 6, a guard ring electrode 7 and a metal connecting sheet to be detected.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a three-electrode corrosion sensor. Fig. 2(a) and 2(b) are front and back views, respectively, of a circular aperture three-electrode corrosion sensor. Taking fig. 2(a) and 2(b) as an example, the sensor includes: the device comprises a substrate 2, wherein a through hole 3 is formed in the substrate 2; a reference electrode 4 and a counter electrode 5 which are arranged on the front surface of the substrate 2 and form a ring surrounding the through hole 3; a guard ring electrode 6 disposed on the front surface of the substrate 2 and surrounding the reference electrode 4 and the counter electrode 5; and the metal connecting sheet 7 to be detected is arranged on the reverse side of the substrate 2 and is used for connecting the sensor 1 and the metal to be detected.
Optionally, the through hole 3 is circular, the reference electrode 4 and the counter electrode 5 form a circular ring, and the reference electrode 4 is located at the opening of the counter electrode 5; the ring angle of the reference electrode 4 is less than or equal to 60 DEG, and the ring angle of the counter electrode 5 is the same as that of the guard ring electrode 6.
Optionally, the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected are made of inert metal or graphite.
Optionally, the substrate 2 is made of a flexible insulating material.
Optionally, the metal connecting sheet 7 to be detected is fixed on the back surface of the substrate 2 through a back adhesive, and the back adhesive is made of acrylate.
The embodiment of the invention also provides a manufacturing method of any one of the sensors, which is one of an etching method, a pressing method, an ink-jet printing method and a sputtering method.
Optionally, the etching method comprises the steps of: pressing inert metal or graphite on the substrate 2; and etching the inert metal or graphite by using an acid solution to form the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected.
Optionally, the pressing method comprises the following steps: manufacturing the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected; and the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected are pressed and integrated with the substrate 2 through a pressing process.
Optionally, the inkjet printing method comprises the steps of: printing a nano gold, nano silver or graphite material solution on the surface of the substrate 2 by adopting an ink jet printing mode according to the preset positions and shapes of the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected on the substrate 2; and drying the substrate 2 to obtain the sensor 1.
Optionally, the sputtering method comprises the steps of: covering a mask on the surface of the substrate 2 by adopting a photoetching method, wherein the mask is reserved at the positions of the reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected; placing the substrate 2 in a small sputtering instrument, and sputtering inert metal or graphite on the surface of the substrate 2 by the small sputtering instrument; the mask is washed away, resulting in the sensor 1.
The invention provides a three-electrode corrosion sensor 1, which comprises a substrate 2 with a hole 3, a reference electrode 4, a counter electrode 5, a guard ring electrode 6 and a metal connecting sheet 7 to be detected. The substrate 2 is made of flexible insulating material, polyimide or poly terephthalic acid plastic or glass fiber with the thickness of 0.005-0.05 mm is preferable, and different thicknesses and materials can be selected according to different measuring environments. The substrate 2 is provided with a back adhesive, the preferable thickness of the back adhesive is 0.005-0.05 mm, and the back adhesive material is preferably acrylate. The through hole 3 can be round or rectangular, and can be drilled by laser or by a cutting die. The reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected are positioned on the front surface of the base material 2 and are made of inert metals such as gold, silver, copper, platinum and the like or graphite and the like; the ring composed of the reference electrode 4 and the counter electrode 5 can be tightly attached to the through hole 3 or kept at a certain distance from the through hole 3 according to the actual use environment. For example, in an atmospheric environment, a liquid film formed by moisture in the atmosphere is very thin, is estimated to be about 10-500 μm, and needs to be tightly attached to the through hole 3 at this time, so that a continuous liquid film is formed; in a soil environment, the soil acts as an electrolyte and may be kept at a distance from the through-hole 3.
The sensor 1 can be directly attached to the surface of a metal to be detected for use, the metal to be detected is connected through a metal connecting sheet to be detected, the metal to be detected is used as a working electrode, and a reference electrode 4 and a counter electrode 5 of the sensor 1 are matched to form a three-electrode system. The corrosion rate of the metal to be detected is reflected by detecting the open circuit potential of the working electrode and the reference electrode 4 in the electrolyte environment and measuring the linear polarization resistance by scanning the potential. The sensor has high detection sensitivity, can directly reflect the actual corrosion condition of the detected metal, has quick preparation method, low cost and strong controllability, and is suitable for industrial large-scale production.
In addition, the distance between the counter electrode 5 and the working electrode is the sum of the thickness of the sensor substrate and the thickness of the sensor back adhesive, the thickness of the substrate 2 and the thickness of the back adhesive are uniform and controllable, different thicknesses can be adopted in different environments, and an electrolytic cell is formed by utilizing the actual environment of the metal to be detected. For example, the substrate and the back glue thickness of 10 μm in the atmosphere and the substrate and the back glue thickness of 0.2mm in the soil can reflect the corrosion rate of the measured object in real time. Meanwhile, the guard ring electrode 6 on the sensor 1 can prevent the corrosion current outside the sensor from flowing to the counter electrode 5, namely, only the corrosion current of the exposed part of the measured metal in the sensor 1 can reach the counter electrode 5, and the corrosion area of the measured metal can be confirmed.
The above is the core idea of the present invention, and the three-electrode corrosion sensor and the manufacturing method thereof will be described in detail below with reference to specific examples.
Example 1: three-electrode sensor for monitoring atmospheric corrosion
Example 1 provides a three electrode sensor for monitoring atmospheric corrosion. As shown in fig. 2(a) and 2(b), the substrate 2 is a polyimide insulating film with a thickness of 5 μm, and has a rectangular shape of 50 × 60mm, and a circular through hole 3(Φ 15mm) is formed in the center of the substrate 2; the reference electrode 4 and the counter electrode 5 form a ring shape (the inner diameter phi is 15mm, the outer diameter phi is 21mm) which is tightly attached to the through hole 3 and is concentric with the through hole 3, the ring angle of the reference electrode 4 is 30 degrees, and the ring angle of the counter electrode 5 is 320 degrees; the guard ring electrode 6 is in a ring shape (inner diameter phi 35mm, outer diameter phi 41mm) concentric with the through hole 3. The metal connecting sheet 7 to be measured is arranged on the back surface of the substrate 2, is positioned 10mm below the central point of the through hole 3 and is rectangular with the shape of 10 x 5 mm. The reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected are all made of copper materials, and the thickness of the copper materials is 5 micrometers.
The three-electrode corrosion sensor 1 is manufactured by an etching method. The sensor 1 is formed by first laminating a 5 μm polyimide film with a 5 μm copper metal film and then etching with acid to leave the desired portions of the reference electrode 4, counter electrode 5, guard ring electrode 6 and metal tab 7 to be measured.
Example 2: three-electrode sensor for monitoring marine corrosion
Example 2 provides a three-electrode sensor for monitoring marine corrosion. As shown in fig. 2(a) and 2(b), the substrate 2 is a polyimide insulating film with a thickness of 20 μm, and has a rectangular shape of 60 × 80mm, and a circular through hole 3(Φ 16mm) is formed in the center of the substrate 2; the reference electrode 4 and the counter electrode 5 form a concentric ring (with the inner diameter phi of 20mm and the outer diameter phi of 26mm) which is 2mm away from the through hole 3, the ring angle of the reference electrode 4 is 20 degrees, and the ring angle of the counter electrode 5 is 330 degrees; the guard ring electrode 6 is in a ring shape (inner diameter phi 36mm, outer diameter phi 42mm) concentric with the through hole 3. The metal connecting sheet 7 to be measured is arranged on the back surface of the substrate 2, is positioned 10mm below the central point of the through hole 3 and is a rectangle with 10 x 5 mm. The reference electrode 4, the counter electrode 5, the guard ring electrode 6 and the metal connecting sheet 7 to be detected are all made of metal gold.
The three-electrode corrosion sensor 1 is prepared by a sputtering method. Firstly, covering a mask on a polyimide insulating film with the thickness of 20 mu m by using a photoetching method, and reserving gaps at the positions of a required reference electrode 4, a required counter electrode 5, a required guard ring electrode 6 and a required metal connecting sheet 7; the substrate 2 is then placed in a small sputtering apparatus, metallic gold is sputtered onto the substrate 2 by the small particle sputtering apparatus, and the mask is washed away, forming the sensor 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A three-electrode corrosion sensor (1), comprising:
the device comprises a substrate (2), wherein a through hole (3) is formed in the substrate (2);
the reference electrode (4) and the counter electrode (5) are arranged on the front surface of the substrate (2) and form a ring surrounding the through hole (3);
a guard ring electrode (6) arranged on the front surface of the substrate (2) and surrounding the reference electrode (4) and the counter electrode (5);
and the metal connecting sheet (7) to be detected is arranged on the reverse side of the substrate (2) and is used for connecting the sensor (1) and the metal to be detected.
2. The sensor (1) according to claim 1,
the through hole (3) is circular, the reference electrode (4) and the counter electrode (5) form a circular ring, and the reference electrode (4) is positioned at the opening of the counter electrode (5);
the ring angle of the reference electrode (4) is less than or equal to 60 degrees, and the ring angle of the counter electrode (5) is the same as that of the guard ring electrode (6).
3. The sensor (1) according to claim 1, wherein the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connection piece (7) to be measured are made of inert metal or graphite.
4. A sensor (1) according to claim 1, wherein the substrate (2) is made of a flexible insulating material.
5. The sensor (1) according to claim 1, wherein the metal connection pad (7) to be tested is fixed on the back of the substrate (2) by a back adhesive, and the back adhesive is made of acrylate.
6. A method of manufacturing a sensor (1) according to any of claims 1-5, characterized in that the manufacturing method is one of etching, pressing, ink-jet printing and sputtering.
7. The method of claim 6, wherein the etching comprises the steps of:
pressing inert metal or graphite on the substrate (2);
and etching the inert metal or graphite by using an acidic solution to form the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connecting sheet (7) to be detected.
8. The method of manufacture of claim 6, wherein the compression method comprises the steps of:
manufacturing the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connecting sheet (7) to be detected;
and the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connecting sheet (7) to be detected are pressed into a whole with the substrate (2) through a pressing process.
9. The method of manufacturing according to claim 6, wherein the inkjet printing method comprises the steps of:
printing a nano gold, nano silver or graphite material solution on the surface of the substrate (2) by adopting an ink jet printing mode according to the preset positions and shapes of the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connecting sheet (7) to be detected on the substrate (2);
and drying the substrate (2) to obtain the sensor (1).
10. The method of manufacturing of claim 6, wherein the sputtering method comprises the steps of:
covering a mask on the surface of the substrate (2) by adopting a photoetching method, wherein the mask is reserved at the positions of the reference electrode (4), the counter electrode (5), the guard ring electrode (6) and the metal connecting sheet (7) to be detected;
placing the substrate (2) in a small sputtering instrument, and sputtering inert metal or graphite on the surface of the substrate (2) through the small sputtering instrument;
and washing off the mask to obtain the sensor (1).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112964629A (en) * | 2021-02-24 | 2021-06-15 | 江苏师范大学 | Metal structure corrosion monitoring device |
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