CN210401309U - Miniature chloride ion sensor based on Fick diffusion law - Google Patents
Miniature chloride ion sensor based on Fick diffusion law Download PDFInfo
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- CN210401309U CN210401309U CN201920424071.2U CN201920424071U CN210401309U CN 210401309 U CN210401309 U CN 210401309U CN 201920424071 U CN201920424071 U CN 201920424071U CN 210401309 U CN210401309 U CN 210401309U
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Abstract
The utility model discloses a Fick diffusion law-based micro chloride ion sensor, which comprises a polyimide thin sheet substrate, an auxiliary electrode, a sensing electrode, a reference electrode and a counter electrode, which are not in contact with each other; the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode all comprise a sensitive element, a lead and a welding spot connected with the sensitive element through the lead; the sensitive element of the sensing electrode is arranged in the groove of the sensitive element of the auxiliary electrode; the sensitive elements of the auxiliary electrode, the sensing electrode and the reference electrode all comprise a Ti adhesion layer, a Pt electrode layer and an Au thin film layer from bottom to top; the sensitive element of the counter electrode comprises a Ti adhesion layer and a Pt electrode layer from bottom to top; the sensitive elements of the auxiliary electrode, the sensing electrode and the reference electrode are plated with Ag thin film layers, and the Ag thin film layers are plated with AgCl thin film layers. The utility model discloses small, structural stability is good, the reliability is high, the leakproofness is good, can be applied to aircraft salt fog corruption and protection, improves aircraft life.
Description
Technical Field
The utility model relates to a chloride ion sensor field especially relates to a miniature chloride ion sensor based on Fick diffusion law.
Background
Corrosion is one of the major forms of structural damage in aircraft, accounting for 20% of total structural damage. Aircraft structural corrosion is the cumulative chemical loss and destruction of components through chemical or electrochemical action in an atmospheric corrosive micro-liquid film environment. In the initial stage of corrosion, the corrosion site is difficult to detect, and when the corrosion site is not controlled after the initiation, the corrosion site will develop faster and more seriously than other damages. The corrosion damage of the aircraft directly affects the attendance rate of the aircraft and more seriously affects the life safety of pilots. Therefore, active precautions must be taken to predict early aircraft corrosion levels to reduce aircraft maintenance costs and avoid tragedies.
In the east coastal region of China, whether civil or military aircraft, because flight tasks are executed in severe and complex environments such as high salt fog, high humidity and the like for a long time, the surface of the aircraft, even the inner part of a cockpit, is not subjected to various corrosions all the time. These corrosions are generally not observable to the naked eye of a human in the early stages of their occurrence, and the aircraft surfaces have suffered severe corrosion by the time they are discovered, which greatly reduces the service life of the aircraft and seriously threatens the life safety of the pilot.
At present, the corrosion protection of China on aircrafts is mainly based on the periodical inspection of sealed water-proof and airframe, the traditional detection mode has low efficiency and high cost, and although the corrosion conditions of aircrafts and the like are evaluated by the technologies of ultrasound, infrared imaging and the like, the methods detect the corrosion parts under the condition that the aircrafts are corroded seriously, the efficiency is low and the cost is high. At present, the corrosion inspection of the domestic aircrafts mainly takes pH value as a main part, and because the corrosion rate of chloride ions to the aircrafts is lower than that of hydrogen ions to the aircrafts, the corrosion protection of chloride ions at home and abroad is not researched, but the corrosion rate of chloride ions to the aircrafts is almost multiplied in high-salt, high-humidity and weak-acid environments such as coastal environments and island environments, and a sensor for monitoring the concentration of chloride ions is urgently needed in the aircrafts.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that to the defect that involves in the background art, provide a miniature chloride ion sensor based on Fick diffusion law.
The utility model discloses a solve above-mentioned technical problem and adopt following technical scheme:
the micro chloride ion sensor based on Fick diffusion law comprises a polyimide sheet substrate, an auxiliary electrode, a sensing electrode, a reference electrode and a counter electrode;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are all arranged on the polyimide sheet substrate and respectively comprise a sensitive element, a lead and a welding spot connected with the sensitive element through the lead;
the sensitive elements of the sensing electrode are in an interdigital shape; the sensitive element of the auxiliary electrode is rectangular, and a groove for placing the sensitive element of the sensing electrode is arranged on the sensitive element of the auxiliary electrode; the sensitive element of the sensing electrode is arranged in the groove of the sensitive element of the auxiliary electrode;
the sensitive elements of the reference electrode and the counter electrode are strip-shaped, are respectively arranged on two sides of the sensitive element of the auxiliary electrode and are parallel to the edges on two sides of the sensitive element of the auxiliary electrode, and are vertical to the length direction of an interdigital of the sensitive element of the single sensing machine;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode all comprise a Ti adhesion layer, a Pt electrode layer and an Au thin film layer from bottom to top; the sensitive element of the counter electrode comprises a Ti adhesion layer and a Pt electrode layer from bottom to top;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode are plated with Ag thin film layers, and the Ag thin film layers are plated with AgCl thin film layers;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are not in contact with each other.
As a further optimization scheme of the miniature chloride ion sensor based on Fick diffusion law, the sensing electrode has the sensitive element with the fork index of 3, the width of the fork of 5 mu m, the distance between the forks of 1mm and the length of the fork of 3 mm; the wire width of the sensing electrode is 70 μm, and the welding spot of the sensing electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the auxiliary electrode is a rectangle with 8 x 4 mm; the distance between the auxiliary electrode sensitive element and the sensing electrode sensitive element is 5 mu m; the wire width of the auxiliary electrode is 70 μm, and the auxiliary electrode welding spot is a rectangle with 1 x 1.5 mm;
the sensitive element of the reference electrode is a rectangle with 70 x 3000 mu m; the distance between the reference electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the reference electrode lead is 70 mu m, and the welding spot of the reference electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the counter electrode is a rectangle of 70 x 3000 mu m; the distance between the counter electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the counter electrode lead is 70 mu m, and the counter electrode welding spot is a rectangle with the length of 1 x 1.5 mm.
As a further optimization scheme of the miniature chloride ion sensor based on Fick diffusion law, the miniature chloride ion sensor also comprises a first connector, a second connector, a third connector and a fourth connector;
one end of each of the first connector, the second connector, the third connector, the fourth connector and the reference electrode are respectively connected with welding points of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode, and the other ends of the first connector, the second connector and the third connector are respectively connected with the outside;
and insulating layers are arranged on the wires and welding spots of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode.
The utility model adopts the above technical scheme to compare with prior art, have following technological effect:
the utility model discloses stability is high, the sensitivity is good, can carry out real-time supervision to chloride ion in the faintly acid salt fog environment, has solved present atmosphere monitoring and has used traditional monitoring website as leading, the website is few, coverage area is few, data update real-time is poor, can not truly reflect the problem of the true air quality information of people's personal contact.
Drawings
Fig. 1 is the overall structure schematic diagram of the micro chloride ion sensor provided by the present invention.
FIG. 2 is an enlarged view of a portion of FIG. 1 at A;
FIG. 3 is a schematic diagram of a sputtering and photolithography scheme of the micro chloride ion sensor provided by the present invention;
FIG. 4 is a connection diagram of a chloride ion sensor test circuit provided by the present invention;
FIG. 5 is a pulse current function diagram of the micro chloride ion sensor provided by the present invention;
fig. 6 is a graph of the theoretical potential of the micro chloride ion sensor Nernst provided by the present invention;
FIG. 7 is a graph showing the relationship between the potential value and the time obtained by signal processing under the conditions of 0.1, 0.3, 0.5, 0.7 and 1mol/L chloride ion concentration micro-liquid membrane of the micro-chloride ion sensor according to the embodiment of the present invention;
FIG. 8 is a graph showing the results of the test of the micro chloride ion sensor according to the embodiment of the present invention under the micro liquid film conditions of chloride ion concentration of 0.1, 0.3, 0.5, 0.7, 1mol/L, respectively;
fig. 9 is a comparison graph of the transition time calibration curve and the theoretical equation obtained by ten times of tests performed on the micro chloride ion sensor under the conditions of 0.1, 0.3, 0.5, 0.7 and 1mol/L chloride ion concentration micro liquid film, respectively.
In the figure, 1-sensitive element of counter electrode, 2-conducting wire of counter electrode, 3-welding point of counter electrode, 4-sensitive element of auxiliary electrode, 5-conducting wire of auxiliary electrode, 6-welding point of auxiliary electrode, 7-sensitive element of sensing electrode, 8-conducting wire of sensing electrode, 9-welding point of sensing electrode, 10-sensitive element of reference electrode, 11-conducting wire of reference electrode, 12-welding point of reference electrode, and 13-polyimide thin sheet substrate.
Detailed Description
The technical scheme of the utility model is further explained in detail with the attached drawings as follows:
the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, components are exaggerated for clarity.
As shown in figure 1, the utility model discloses a micro chloride ion sensor based on Fick's diffusion law, comprising a polyimide thin slice substrate, an auxiliary electrode, a sensing electrode, a reference electrode and a counter electrode;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are all arranged on the polyimide sheet substrate and respectively comprise a sensitive element, a lead and a welding spot connected with the sensitive element through the lead;
as shown in fig. 2, the sensing elements of the sensing electrode are interdigital; the sensitive element of the auxiliary electrode is rectangular, and a groove for placing the sensitive element of the sensing electrode is arranged on the sensitive element of the auxiliary electrode; the sensitive element of the sensing electrode is arranged in the groove of the sensitive element of the auxiliary electrode;
the sensitive elements of the reference electrode and the counter electrode are strip-shaped, are respectively arranged on two sides of the sensitive element of the auxiliary electrode and are parallel to the edges on two sides of the sensitive element of the auxiliary electrode, and are vertical to the length direction of an interdigital of the sensitive element of the single sensing machine;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode all comprise a Ti adhesion layer, a Pt electrode layer and an Au thin film layer from bottom to top; the sensitive element of the counter electrode comprises a Ti adhesion layer and a Pt electrode layer from bottom to top;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode are plated with Ag thin film layers, and the Ag thin film layers are plated with AgCl thin film layers;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are not in contact with each other.
As a further optimization scheme of the miniature chloride ion sensor based on Fick diffusion law, the sensing electrode has the sensitive element with the fork index of 3, the width of the fork of 5 mu m, the distance between the forks of 1mm and the length of the fork of 3 mm; the wire width of the sensing electrode is 70 μm, and the welding spot of the sensing electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the auxiliary electrode is a rectangle with 8 x 4 mm; the distance between the auxiliary electrode sensitive element and the sensing electrode sensitive element is 5 mu m; the wire width of the auxiliary electrode is 70 μm, and the auxiliary electrode welding spot is a rectangle with 1 x 1.5 mm;
the sensitive element of the reference electrode is a rectangle with 70 x 3000 mu m; the distance between the reference electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the reference electrode lead is 70 mu m, and the welding spot of the reference electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the counter electrode is a rectangle of 70 x 3000 mu m; the distance between the counter electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the counter electrode lead is 70 mu m, and the counter electrode welding spot is a rectangle with the length of 1 x 1.5 mm.
As a further optimization scheme of the miniature chloride ion sensor based on Fick diffusion law, the miniature chloride ion sensor also comprises a first connector, a second connector, a third connector and a fourth connector;
one end of each of the first connector, the second connector, the third connector, the fourth connector and the reference electrode are respectively connected with welding points of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode, and the other ends of the first connector, the second connector and the third connector are respectively connected with the outside;
and insulating layers are arranged on the wires and welding spots of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode.
The utility model also discloses a preparation method of this miniature chloride ion sensor based on Fick diffusion law contains following step:
step A), sputtering a Ti adhesion layer and a Pt electrode layer on a polyimide sheet substrate in sequence by adopting a magnetron sputtering method;
step B), performing line pattern transfer on the polyimide sheet substrate sputtered with the Ti adhesion layer and the Pt electrode layer by adopting a photoetching-based technology to form patterns of a reference electrode, a sensing electrode, an auxiliary electrode and a counter electrode on the Ti adhesion layer and the Pt electrode layer;
step C), electroplating Au on the Pt electrode layers of the patterns of the reference electrode, the sensing electrode and the auxiliary electrode by adopting an electroplating method to form an Au thin film layer;
step D), electroplating Ag on the Au thin film layers of the reference electrode, the sensing electrode and the auxiliary electrode by adopting an electroplating method to form an Ag thin film layer;
and E), electroplating AgCl on the Ag thin film layers of the reference electrode, the sensing electrode and the auxiliary electrode by adopting an electroplating method to form AgCl thin film layers.
The polyimide sheet substrate is a rectangular parallelepiped substrate of 15 × 10 × 1 mm. The Polyimide sheet substrate is made of Polyimide (PI), and the Polyimide (PI) has the advantages of high temperature resistance (up to 400 ℃), excellent mechanical properties, high irradiation resistance, good acid-base chemical stability, good flexibility and the like. The polyimide is used as the substrate material of the chloride ion sensor, so that the use temperature range of the sensor can be enlarged, the influence of the external corrosion environment on the chloride ion sensor is reduced, and the stability and the reliability of the sensor in a complex environment are improved. In addition, the polyimide is a flexible material, and the application field and the application range of the chloride ion sensor can be widened.
Fig. 3 is a schematic diagram of the sputtering and photolithography schemes of the micro chloride ion sensor provided by the present invention.
The invention also discloses a measuring method using the miniature chloride ion sensor based on Fick diffusion law, which comprises the following steps:
step 1), as shown in fig. 4, a current source, a function generator and a potential measuring device are arranged, wherein the control end of the current source is connected with the function generator, constant pulse constant current is generated through the function generator, the positive electrode of the current source is connected with the welding point of the counter electrode, and the negative electrode of the current source is connected with the welding point of the auxiliary electrode; the positive electrode of the potential measuring device is connected with the welding spot of the sensing electrode, and the negative electrode of the potential measuring device is connected with the welding spot of the reference electrode;
step 2), measuring by a potential measuring device to obtain a potential curve of a sensing electrode in the miniature chloride ion sensor;
step 3), derivation is carried out on the potential curve to obtain a derivative curve of the potential curve, and the time corresponding to the peak value of the derivative curve is made to be the transition time tau;
step 4), calculating the chloride ion concentration C measured by the micro chloride ion sensor according to the following formula* O：
In the formula, DOThe diffusion coefficient of chloride ions, A the surface area of the auxiliary electrode, F the Faraday coefficient, and I the current applied by the current source.
FIG. 5 is a pulse current function diagram of the micro chloride ion sensor provided by the present invention; referring to fig. 5, the pulse current is a direct current signal and has the same time variation rule; when the pulse current is positive, the sensor starts to measure to obtain an S-shaped curve of the potential changing along with the time, the software calculates through a test interface to obtain a corresponding transition time, when the pulse current is negative, the sensor is in a stagnation state, and the potential gradually returns to zero value to fluctuate;
fig. 6 is a graph of the theoretical potential of the micro chloride ion sensor Nernst provided by the present invention; referring to fig. 6, τ is the transition time of the chloride ion concentration, and theoretically when t ═ τ, the potential is infinite, and is shown as the measurement device potential threshold;
FIG. 7 is a graph showing the relationship between the potential value and the time obtained by signal processing under the conditions of 0.1, 0.3, 0.5, 0.7 and 1mol/L chloride ion concentration micro-liquid membrane of the micro-chloride ion sensor according to the embodiment of the present invention; referring to fig. 7, a potential time curve measured by the sensor in a micro-liquid film environment is an S-shaped curve, and the S-shaped curve gradually moves backwards with the increase of concentration, and the curve is smoother the higher the concentration is, and the inflection point (transition time) of the curve is clearer;
FIG. 8 is a graph showing the results of the test of the micro chloride ion sensor according to the embodiment of the present invention under the micro liquid film conditions of chloride ion concentration of 0.1, 0.3, 0.5, 0.7, 1mol/L, respectively; referring to fig. 8, the sensor has obvious peak values of derivative curves under the conditions of 0.1, 0.3, 0.5, 0.7 and 1mol/L chloride ion concentration micro liquid film, and the peak values of the derivative curves can be obtained through an automatic peak searching function, wherein the peak values are transition time values;
FIG. 9 is a comparison graph of the transition time calibration curve and the theoretical equation obtained by ten times of tests performed on the micro chloride ion sensor according to the embodiment of the present invention under the micro liquid film conditions of chloride ion concentration of 0.1, 0.3, 0.5, 0.7, and 1mol/L, respectively; referring to fig. 9, a transition time calibration curve obtained by the sensor through multiple measurements is the same as a theoretical equation rule, and the stability is good.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The above-mentioned embodiments further describe the objects, technical solutions and advantages of the present invention in detail, it should be understood that the above description is only the embodiments of the present invention, and is not intended to limit the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. The micro chloride ion sensor based on Fick diffusion law is characterized by comprising a polyimide sheet substrate, an auxiliary electrode, a sensing electrode, a reference electrode and a counter electrode;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are all arranged on the polyimide sheet substrate and respectively comprise a sensitive element, a lead and a welding spot connected with the sensitive element through the lead;
the sensitive elements of the sensing electrode are in an interdigital shape; the sensitive element of the auxiliary electrode is rectangular, and a groove for placing the sensitive element of the sensing electrode is arranged on the sensitive element of the auxiliary electrode; the sensitive element of the sensing electrode is arranged in the groove of the sensitive element of the auxiliary electrode;
the sensitive elements of the reference electrode and the counter electrode are strip-shaped, are respectively arranged on two sides of the sensitive element of the auxiliary electrode and are parallel to the edges on two sides of the sensitive element of the auxiliary electrode, and are vertical to the length direction of an interdigital of the sensitive element of the single sensing machine;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode all comprise a Ti adhesion layer, a Pt electrode layer and an Au thin film layer from bottom to top; the sensitive element of the counter electrode comprises a Ti adhesion layer and a Pt electrode layer from bottom to top;
the sensitive element of the auxiliary electrode, the sensitive element of the sensing electrode and the sensitive element of the reference electrode are plated with Ag thin film layers, and the Ag thin film layers are plated with AgCl thin film layers;
the auxiliary electrode, the sensing electrode, the reference electrode and the counter electrode are not in contact with each other.
2. The Fick diffusion law-based micro chloride ion sensor according to claim 1, wherein the sensitive element of the sensing electrode has a fork index of 3, a fork width of 5 μm, a fork pitch of 1mm, and a fork length of 3 mm; the wire width of the sensing electrode is 70 μm, and the welding spot of the sensing electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the auxiliary electrode is a rectangle with 8 x 4 mm; the distance between the auxiliary electrode sensitive element and the sensing electrode sensitive element is 5 mu m; the wire width of the auxiliary electrode is 70 μm, and the auxiliary electrode welding spot is a rectangle with 1 x 1.5 mm;
the sensitive element of the reference electrode is a rectangle with 70 x 3000 mu m; the distance between the reference electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the reference electrode lead is 70 mu m, and the welding spot of the reference electrode is a rectangle with 1 x 1.5 mm;
the sensitive element of the counter electrode is a rectangle of 70 x 3000 mu m; the distance between the counter electrode sensitive element and the auxiliary electrode sensitive element is 70 μm; the line width of the counter electrode lead is 70 mu m, and the counter electrode welding spot is a rectangle with the length of 1 x 1.5 mm.
3. A Fick's diffusion law based micro chloride ion sensor as claimed in claim 1, further comprising first to fourth connectors;
one end of each of the first connector, the second connector, the third connector, the fourth connector and the reference electrode are respectively connected with welding points of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode, and the other ends of the first connector, the second connector and the third connector are respectively connected with the outside;
and insulating layers are arranged on the wires and welding spots of the auxiliary electrode, the sensing electrode, the reference electrode and the Pt counter electrode.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018215A (en) * | 2019-04-01 | 2019-07-16 | 南京航空航天大学 | Miniature chloride ion sensor and its method based on Fick diffusion law |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018215A (en) * | 2019-04-01 | 2019-07-16 | 南京航空航天大学 | Miniature chloride ion sensor and its method based on Fick diffusion law |
| CN110018215B (en) * | 2019-04-01 | 2023-09-29 | 南京航空航天大学 | Fick diffusion law-based miniature chloride ion sensor and method thereof |
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