CN113063995B - Carbon-based conductive polymer film underwater electric field sensor - Google Patents
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Abstract
The invention relates to a carbon-based conductive polymer film underwater electric field sensor. The carbon-based conductive polymer film underwater electric field sensor is composed of two paired electrodes, wherein each electrode in the paired electrodes comprises: the device comprises a carbon-based material, a conductive polymer film, a microporous protective sleeve, a sealing cavity and a lead; one end of the carbon-based material is connected with the lead and forms a connecting part; the connecting part is arranged in the sealing cavity; the conductive polymer film uniformly covers the surface of the carbon-based material to form a carbon-based conductive polymer film electrode; the carbon-based conductive polymer membrane electrode sealing device is packaged in the sealing cavity and in the cavity formed by the micropore protective sleeve. A single electrode pair of the same potential is used to probe the underwater electric field. The invention improves the sensitivity and stability of the underwater electric field sensor, reduces the preparation cost and can be effectively used for measuring underwater low-frequency weak electric field signals.
Description
Technical Field
The invention relates to the field of underwater electric field sensors, in particular to a carbon-based conductive polymer film underwater electric field sensor.
Background
The ocean not only contains abundant oil gas and mineral resources, but also provides wide space for human beings. With the emphasis of human beings on oceans and the development of marine geoscience and technology, the development of human beings on seabed resources is continuously increased, and the marine electromagnetic method also becomes human explorationAnd an important means of exploiting the seabed. However, due to the special environment of the ocean, the electromagnetic field in the ocean is mainly a very low frequency weak signal. Therefore, the preparation of an underwater electric field sensor with high sensitivity, high stability and low noise aiming at low-frequency weak signals becomes one of important research contents of marine electromagnetic detection. The electric field sensors are used in pairs, and electric field changes in the sea are detected by voltage changes between the paired sensors. At present, electrodes of an underwater electric field sensor are generally divided into two types, namely a reversible electrode and an inert electrode. The reversible electrode comprises Hg/Hg 2 Cl 2 、Pb/PbCl 2 And Ag/AgCl electrodes and the like, the metal insoluble salt electrodes are nonpolarized electrodes, and the electrode potential and insoluble salt anions in the solution have a response relation and conform to the Nernst electrochemical equation. At present, the most used electrode is an Ag/AgCl electrode which has better stability, higher precision, lower self-noise and good response performance. However, ag/AgCl electrodes also have some disadvantages, such as high manufacturing cost, short service life, and transportation and storage with brine.
Another class is the inert electrodes represented by carbon fiber electrodes, which also include titanium, gold, graphite, carbon aerogel electrodes, and the like. The electrode does not generate chemical reaction, the change of a surface double electric layer is mainly utilized to convert an external electric field into an electric signal, the polarizability of the electrode is generally utilized, and the electrode potential is sensitive to the surface charge density. However, the electrodes generally have poor stability and high self-noise, and have large low-frequency capacitive reactance, so that the sensitivity is reduced, and the electrodes are difficult to detect low-frequency weak signals.
Therefore, there is a need to develop a new underwater electric field sensor, which can reduce the manufacturing, storage and transportation costs of the sensor while maintaining the high sensitivity electric field response performance.
Disclosure of Invention
The invention aims to provide a carbon-based conductive polymer film underwater electric field sensor, which improves the sensitivity and stability of the underwater electric field sensor, reduces the preparation cost and can be effectively used for measuring underwater low-frequency weak electric field signals.
In order to achieve the purpose, the invention provides the following scheme:
a carbon-based conductive polymer film underwater electric field sensor, said carbon-based conductive polymer film underwater electric field sensor comprising two paired electrodes, each of said electrodes comprising: the device comprises a carbon-based material, a conductive polymer film, a microporous protective sleeve, a sealing cavity and a lead;
one end of the carbon-based material is connected with the lead and forms a connecting part; the connecting part is arranged in the sealing cavity;
the conductive polymer film uniformly covers the surface of the carbon-based material to form a carbon-based conductive polymer film electrode;
the carbon-based conductive polymer membrane electrode sealing device is packaged in the sealing cavity and in a cavity formed by the microporous protective sleeve.
The carbon-based conductive polymer film underwater electric field sensors are used in pairs, and the change of the underwater electric field is reflected by measuring the induced voltage between a pair of carbon-based conductive polymer film electrodes.
Optionally, the carbon-based material is carbon rod, carbon fiber, carbon cloth, carbon felt or carbon foam.
Optionally, the length of the carbon-based material is 10 cm-20 cm.
Optionally, the mass of the carbon-based material is 0.5g.
Optionally, the conductive polymer film is polypyrrole, polyaniline or polythiophene.
Optionally, the method further includes: and sealing the connection point of one end of the carbon-based material and the lead in the sealing cavity by using epoxy resin.
Optionally, the method further includes: and generating the conductive polymer film by in-situ polymerization on the surface of the carbon-based material by using an electrochemical polymerization method.
Optionally, the method of electrochemical polymerization comprises: galvanostatic polymerization, potentiostatic polymerization or cyclic voltammetric polymerization.
Optionally, the distance between the two paired electrodes ranges from 10cm to 100cm.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the carbon-based conductive polymer film underwater electric field sensor provided by the invention is prepared by taking a low-cost carbon material as a conductive base material, electrochemically polymerizing the carbon material on the surface of the conductive base material to generate a conductive polymer film to form a carbon-based conductive polymer film electrode, and leading out, sealing and pairing through a lead, and has high sensitivity response to underwater electric field signals. The carbon-based conductive polymer film underwater electric field sensor converts underwater electric field change into a measurable electric signal by measuring induced voltage between paired electrodes. The carbon-based conductive polymer film underwater electric field sensor provided by the invention has the characteristics of high sensitivity, good stability, low self-noise, adjustable performance and low cost, and can be effectively used for measuring low-frequency weak electric field signals in ocean or river water areas.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of an underwater electric field sensor with a carbon-based conductive polymer film according to the present invention;
FIG. 2 is a schematic view of a carbon-based conductive polymer membrane electrode;
FIG. 3 is a schematic diagram of a potential change curve of a polyaniline and polypyrrole underwater electric field sensor continuously recording for one week in filtered seawater;
FIG. 4 is a diagram of an electric field response testing apparatus;
FIG. 5 is a schematic diagram of the response of a paired polypyrrole and polyaniline underwater electric field sensor to a 0.01Hz,1mV sinusoidal electric field signal in seawater;
FIG. 6 is a schematic diagram of the response of a paired polypyrrole and polyaniline underwater electric field sensor to a sinusoidal electric field signal of 0.1Hz,100mV in seawater;
FIG. 7 is a schematic diagram of the response of a paired carbon-based conductive polymer film underwater electric field sensor to a 0.01Hz,1mV sinusoidal electric field signal in seawater with a paired Ag/AgCl underwater electric field sensor;
FIG. 8 is a graph showing the response of a carbon-based conductive polymer film paired underwater electric field sensor to a 0.1Hz,100mV sinusoidal electric field signal in seawater, in comparison with an Ag/AgCl paired underwater electric field sensor.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a carbon-based conductive polymer film 4 underwater electric field sensor, which improves the sensitivity and stability of the underwater electric field sensor, reduces the preparation cost and can be effectively used for measuring underwater low-frequency weak electric field signals.
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description thereof.
Fig. 1 is a schematic structural view of an underwater electric field sensor of a carbon-based conductive polymer film 4 according to the present invention, and as shown in fig. 1, the underwater electric field sensor of a carbon-based conductive polymer film 4 according to the present invention includes two paired electrodes, each of the electrodes includes: carbon-based material 3, conductive polymer film 4, microporous protection sleeve 5, sealed cavity 6 and lead 1. The carbon-based material 3 is carbon rod, carbon fiber, carbon cloth, carbon felt or foam carbon. The conductive polymer film 4 is polypyrrole, polyaniline or polythiophene.
One end of the carbon-based material 3 is connected with the lead 1 and forms a connecting part; said connection being arranged in said sealed chamber 6. The length of the carbon-based material 3 is 10 cm-20 cm. The mass of the carbon-based material 3 was 0.5g (carbon fiber). Specifically, if carbon fibers are used as the carbon-based material, the mass of the carbon-based material is about 0.5g, and if other carbon materials are used, the mass of the carbon-based material is more than 0.5g, taking a carbon rod of the same size as an example.
Specifically, a connection point 7 between one end of the carbon-based material 3 and the lead 1 is sealed in the sealing cavity 6 by using epoxy resin.
The conductive polymer film 4 is uniformly covered on the surface of the carbon-based material 3 to form the carbon-based conductive polymer film electrode.
And generating the conductive polymer film 4 by in-situ polymerization on the surface of the carbon-based material 3 by using an electrochemical polymerization method.
Wherein the electrochemical polymerization method comprises the following steps: galvanostatic polymerization, potentiostatic polymerization or cyclic voltammetric polymerization.
The carbon-based conductive polymer membrane electrode sealing device is packaged in a cavity formed by the sealing cavity 6 and the microporous protection sleeve 5.
Fig. 4 is a schematic diagram of an apparatus for measuring an underwater electric field signal by using an underwater electric field sensor of a carbon-based conductive polymer film 4 provided by the invention. As shown in fig. 4, the device for measuring underwater electric field signals by the carbon-based conductive polymer film 4 underwater electric field sensor comprises: the device comprises a carbon-based conductive polymer film matched underwater electric field sensor 17, filtered seawater 16 contained in a container, an electric field signal transmitter 13, a transmitting electrode 15 and a data acquisition instrument 14.
The electric field signal transmitter 13 and the transmitting electrode 15 work together to simulate the underwater electric field signal change.
The data acquisition instrument 14 is used for recording the induced voltage between the paired carbon-based conductive polymer film underwater electric field sensors 17.
The paired carbon-based conductive polymer film underwater electric field sensors 17 are arranged at a certain interval.
The invention is further illustrated below by means of a number of specific embodiments.
Example 1
As shown in fig. 1, the invention designs a high-sensitivity carbon-based conductive polymer film 4 underwater electric field sensor structure: the conductive polymer film 4 plated on a certain area of the surface of the carbon rod is a response unit, the carbon rod is connected with the lead 1, and the connection point 7 is sealed in the special sealing cavity 2 by epoxy resin; the micropore protective sleeve 5 is in threaded connection with the bottom of the sealing cavity 2, and the preparation of the conductive carbon-based polymer film underwater electric field sensor is completed.
Example 2
As shown in fig. 1, the invention designs a high-sensitivity carbon-based conductive polymer film 4 underwater electric field sensor structure: the conductive polymer film 4 plated on a certain area of the surface of the carbon fiber is a response unit, the carbon fiber is connected with the lead 1, and the connection point 7 is sealed in the special sealing cavity 2 by epoxy resin; the micropore protective sleeve 5 is connected to the bottom of the sealed cavity 2 to complete the preparation of the conductive carbon-based polymer film underwater electric field sensor.
Example 3
As shown in fig. 2, the present invention prepares a carbon-based conductive polymer membrane electrode: a sealed carbon-based electrode 11 is used as a working electrode to construct a three-electrode system (a saturated calomel electrode is used as a reference electrode 9, a platinum sheet electrode is used as a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% of aniline monomer (conductive polymer monomer solution 12) is introduced, an electrochemical workstation 8 is used for adopting a constant current polymerization method, the current is set to be 0.1A, the polymerization time is 10min, in order to ensure that the thickness of a conductive polymer film 4 is uniform, a plurality of counter electrodes 10 can be adopted to uniformly surround the working electrode, finally, the polymerized electrode is repeatedly washed by a large amount of deionized water until the solution is neutral, and the solution is dried for later use.
Example 4
As shown in fig. 2, the present invention prepares a carbon-based conductive polymer membrane electrode: a sealed carbon-based electrode 11 is used as a working electrode to construct a three-electrode system (a saturated calomel electrode is used as a reference electrode 9, a platinum sheet electrode is used as a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% aniline monomer is introduced, a constant potential polymerization method is adopted by an electrochemical workstation 8, the set potential is 0.7V, and the polymerization electric quantity is 50℃ In order to ensure the uniform thickness of a conductive polymer film 4, a plurality of counter electrodes 10 can be adopted to uniformly surround the working electrode, and finally, the electrode after polymerization is repeatedly washed by a large amount of deionized water until the solution is neutral, and is dried for later use.
Example 5
As shown in fig. 3, the present invention prepares a carbon-based conductive polymer membrane electrode: a three-electrode system is constructed by taking a sealed carbon-based electrode 11 as a working electrode (a saturated calomel electrode is a reference electrode 9, a platinum sheet electrode is a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% aniline monomer is introduced, polymerization is carried out by using an electrochemical workstation 8 through a cyclic voltammetry method, the set potential is 0.2V-1.0V, the sweep rate is 10mV/s, and 20 cycles are carried out.
Example 6
As shown in fig. 2, the present invention prepares a carbon-based conductive polymer membrane electrode: a sealed carbon-based electrode 11 is used as a working electrode to construct a three-electrode system (a saturated calomel electrode is used as a reference electrode 9, a platinum sheet electrode is used as a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% of pyrrole monomers are introduced, a constant current polymerization method is adopted by an electrochemical workstation 8, the current is set to be 0.1A, the polymerization time is 5min, in order to ensure that the thickness of a conductive polymer film 4 is uniform, a plurality of counter electrodes 10 can be adopted to uniformly surround the working electrode, finally, the polymerized electrode is repeatedly washed by a large amount of deionized water until the solution is neutral, and the electrode is dried for later use.
Example 7
As shown in fig. 2, the present invention prepares a carbon-based conductive polymer membrane electrode: a sealed carbon-based electrode 11 is used as a working electrode to construct a three-electrode system (a saturated calomel electrode is used as a reference electrode 9, a platinum sheet electrode is used as a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% of pyrrole monomers are introduced, an electrochemical workstation 8 is used for adopting a constant potential polymerization method, the set potential is 0.8V, and the polymerization electric quantity is 50℃ In order to ensure that the thickness of a conductive polymer film 4 is uniform, a plurality of counter electrodes 10 can be adopted to uniformly surround the working electrode, finally, the polymerized electrode is repeatedly washed by a large amount of deionized water until the solution is neutral, and is dried for later use.
Example 8
As shown in fig. 2, the present invention prepares a carbon-based conductive polymer membrane electrode: a sealed carbon-based electrode 11 is used as a working electrode to construct a three-electrode system (a saturated calomel electrode is used as a reference electrode 9, a platinum sheet electrode is used as a counter electrode 10, 0.5mol/L HCl solution is selected as an electrolyte, 5% of pyrrole monomer is introduced, polymerization is carried out by using an electrochemical workstation 8 through a cyclic voltammetry method, the potential is set to be 0.4V-1.2V, the sweep rate is 10mV/s, and 25 circles of circulation are carried out, in order to ensure that the thickness of a conductive polymer film 4 is uniform, a plurality of counter electrodes 10 can be adopted to uniformly surround the working electrode, finally, the electrode which is polymerized is repeatedly washed by a large amount of deionized water until the solution is neutral, and is dried for later use.
Example 9
As shown in figure 3, a single carbon-based conductive polymer film 4 underwater electric field sensor is completely immersed in a container containing filtered seawater 16, a data acquisition instrument 14 is used for continuously recording the potential change of the conductive polymer electrode within one circle, and the prepared carbon-based conductive polymer film 4 underwater electric field sensor has better potential stability (the potential drift is less than 90 MuV/24 h)
Example 10
As shown in fig. 4 and 5, a paired carbon-based conductive polymer film underwater electric field sensor 17 (with an electrode spacing of 10 cm) is completely immersed in a container containing filtered seawater 16, an electric field signal emitter 13 is connected to a transmitting electrode 15, and a data acquisition instrument 14 is used to record voltage signal changes between the pair of carbon-based conductive polymer film 4 underwater electric field sensors; the output signal of the electric field signal transmitter 13 is set to a sinusoidal electric field signal of 0.01Hz, 1mV. The prepared conductive polymer underwater electric field sensor can better reduce the law of low-frequency weak electric field signals emitted by the electric field signal emitter 13 and has higher sensitivity.
Example 11
As shown in fig. 4 and 6, a paired carbon-based conductive polymer film underwater electric field sensor 17 (with an electrode spacing of 10 cm) is completely immersed in a container containing filtered seawater 16, an electric field signal transmitter 13 is connected to a transmitting electrode 15, and a data acquisition instrument 14 is used to record a voltage signal change between the pair of carbon-based conductive polymer film 4 underwater electric field sensors; the output signal of the electric field signal transmitter 13 is set to a sinusoidal electric field signal of 0.1hz, 100mv. The prepared carbon-based conductive polymer film 4 underwater electric field sensor can better reduce the law of electric field signals emitted by the electric field signal emitter 13 and has a wider amplitude-frequency range.
Example 12
As shown in fig. 4 and 7, a paired carbon-based conductive polymer film underwater electric field sensor 17 (with an electrode spacing of 10 cm) and a paired Ag/AgCl underwater electric field sensor (with an electrode spacing of 10 cm) are completely immersed in a container containing filtered seawater 16, an electric field signal transmitter 13 is connected to a transmitting electrode 15, and a data acquisition instrument 14 is used to record the voltage signal change between the paired underwater electric field sensors; the output signal of the electric field signal transmitter 13 is set to a sinusoidal electric field signal of 0.01Hz, 1mV. In the low-frequency electric field signal response, the prepared carbon-based conductive polymer film 4 underwater electric field sensor can more stably reduce the electric field signal rule transmitted by the electric field signal transmitter 13 than an Ag/AgCl underwater electric field sensor.
Example 13
As shown in fig. 4 and 8, a paired carbon-based conductive polymer film underwater electric field sensor 17 (with an electrode spacing of 10 cm) and a paired Ag/AgCl underwater electric field sensor (with an electrode spacing of 10 cm) are completely immersed in a container containing filtered seawater 16, an electric field signal emitter 13 is connected to an emitter electrode 15, and a data acquisition instrument 14 is used to record voltage signal changes between the pair of underwater electric field sensors; the output signal of the electric field signal transmitter 13 is set to a sinusoidal electric field signal of 0.1hz, 100mv. The response amplitude of the prepared carbon-based conductive polymer film 4 underwater electric field sensor is higher than that of an Ag/AgCl underwater electric field sensor.
The underwater electric field sensor obtained by the invention starts with obtaining a novel underwater electric field sensor with low cost, easy storage and high performance, adopts a cheap carbon material as a conductive base material, and generates a conductive polymer film 4 on the surface of the conductive base material, aiming at providing the low-cost and high-performance electric field sensor for measuring underwater low-frequency weak electric field signals; the beneficial effects are as follows:
1. the material is various, the carbon-based material 3 comprises carbon rods, carbon fibers, carbon cloth, carbon felt and foam carbon, and the conductive polymer comprises polypyrrole, polyaniline and polythiophene.
2. The performance can be regulated, and the thickness and the appearance of the conductive polymer film 4 can be regulated and controlled by regulating the polymerization current and the polymerization voltage.
3. The underwater electric field sensor has low cost, the substrate material of the underwater electric field sensor is a carbon material, the functional material is a conductive polymer, the material has wide sources and low cost, and the industrial production is mature.
4. The underwater electric field sensor is convenient to store and transport, can be stored in seawater 16 or tap water or directly stored in a dry mode, and does not need to be processed in a dark place.
5. The carbon-based material 3 and the conductive polymer functional material have stable physical and chemical properties, no consumption in use and long service life.
6. The prepared underwater electric field sensor has good tightness and can normally work in a deep pressure environment.
7. The underwater electric field sensor has higher stability, and the potential drift amount is less than or equal to 90 MuV within 24 hours.
8. The underwater electric field sensor is used after being paired, has high sensitivity response and wide-amplitude frequency response, and has better response to electric field signals above 0.001Hz and 1mV.
9. The underwater electric field sensor is used after being paired, has low self-noise, and the self-noise is less than or equal to 5nV/rtHz @1Hz at a frequency point of 1Hz.
10. The underwater electric field sensor has wide application range and is used for electric field detection in oceans or rivers.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (8)
1. An underwater carbon-based conductive polymer film electric field sensor comprising two paired electrodes, each of the electrodes comprising: the device comprises a carbon-based material, a conductive polymer film, a microporous protective sleeve, a sealing cavity and a lead;
one end of the carbon-based material is connected with the lead and forms a connecting part; the connecting part is arranged in the sealing cavity;
the conductive polymer film uniformly covers the surface of the carbon-based material to form a carbon-based conductive polymer film electrode; generating the conductive polymer film by in-situ polymerization on the surface of the carbon-based material by using an electrochemical polymerization method;
the carbon-based conductive polymer membrane electrode is packaged in a cavity formed by the sealing cavity and the microporous protective sleeve;
by measuring the induced voltage between the paired electrodes, the underwater electric field change is converted into a measurable electric signal.
2. The carbon-based conductive polymer film underwater electric field sensor according to claim 1, wherein the carbon-based material is carbon rod, carbon fiber, carbon cloth, carbon felt or carbon foam.
3. The carbon-based conductive polymer film underwater electric field sensor according to claim 1, wherein the carbon-based material has a length of 10cm to 20cm.
4. The underwater electric field sensor of claim 1, wherein the carbon-based material has a mass of 0.5g.
5. The underwater electric field sensor of claim 1, wherein the conductive polymer film is polypyrrole, polyaniline, or polythiophene.
6. The carbon-based conductive polymer film underwater electric field sensor of claim 1, further comprising: and sealing the connection point of one end of the carbon-based material and the lead in the sealing cavity by using epoxy resin.
7. The carbon-based conductive polymer film underwater electric field sensor according to claim 6, wherein the electrochemical polymerization method comprises: galvanostatic polymerization, potentiostatic polymerization or cyclic voltammetric polymerization.
8. The carbon-based conductive polymer film underwater electric field sensor of claim 1, wherein the distance between the two paired electrodes is in a range of 10cm to 100cm.
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| JPH06118107A (en) * | 1992-10-06 | 1994-04-28 | Nippon Telegr & Teleph Corp <Ntt> | Production of electric field sensor |
| WO2012064179A1 (en) * | 2010-11-12 | 2012-05-18 | Mimos Berhad | Ph sensor |
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| CN113063995A (en) | 2021-07-02 |
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