CN107576699B - A kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam - Google Patents
A kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam Download PDFInfo
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Abstract
A kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam, the electrode is using high-specific surface area foamy carbon as basis material, it is first that the foamy carbon for connecting carbon plate is shaped, activated, cleaning and drying process, then foamy carbon surface electrochemistry preplating metallic copper or nickel, by the method deposited metal silver of chemical silvering, is thickeied by plating and form uniform silver layer, method for electrodeposition is recycled to generate silver chloride layer in silver surface；Finally the carbon-based Ag/AgCl electrode of foam is installed in microporous pipe, filler is filled by the carbon plate extraction wire being connected with foamy carbon and obtains foamy carbon base-height ratio surface area Ag/AgCl electric field electrode.The electrode has high-specific surface area, high stability and low potential drift value, and the potential difference between two identical electrodes is small, self noise is low, can be preferably using the monitoring of Yu Haiyang's wide frequency domain electric field signal and anti-corrosion of metal field.
Description
Technical field
The present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation methods of high-specific surface area foam, and in particular to a kind of
The carbon-based Ag/AgCl electric field electrode system of high-specific surface area foam of the detection of ocean wide frequency domain electric field signal and metal corrosion potential test
Preparation Method.
Background technique
With the progress of science and technology, during ocean exploitation, electric field signal measurement applies valence with important
Value.Electric field signal has obtained important application in the physics electric field on naval vessel and the detection of seabottom geology structure.
Marine water flowing, cutting earth magnetic field can generate corresponding induction field, these electric field signals can reflect ocean
The multiple information of environment.Since naval vessel is mostly different metal structure composition, different types of metal can generate different corrosion electricity
Position, therefore when two kinds of different metals impregnate in the seawater together, it just will form corrosion loop, generate corrosion current.In addition, in order to
Naval vessel anti-corrosion need to manually apply cathodic protection current.These electric currents are eventually since the effect of seawater flows to propeller, then from spiral shell
It revolves paddle and returns to ship shell, forming circuit due to the rotation of propeller, causes the cyclically-varying of resistance in circuit, thus
Alternating electric field signal is formed in the seawater.In addition, different geologic structures have different electric field responses to electric field signal in seabed.According to
Principle like this actively emits a kind of known electric field signal to seabed, observes the changing rule of electric field signal after its reflection, Ji Kefen
The geologic structure in seabed is precipitated.But electric field signal is decayed quickly in the seawater, and mostly based on low frequency signal, and therefore, ocean
The good electrode of monitoring needs high sensitivity, the stability of electric field signal.In corrosion-resistant field, metal material protection is improper easily to be occurred
Corrosion, corrosion can be more violent and serious especially in briny environment, all causes huge economic losses to the world every year.It is accurate to survey
It is most important in corrosion-resistant field with the protection electric current of control corrosion rate guard system to determine material corrosion current potential, this is also required to high stability
And the reference electrode of low self noise.
Type of electrodes currently used for electric field monitoring and corrosion monitoring mainly has: copper/copper sulfate electrode, lead/lead chloride electricity
Pole, silver/silver chloride electrode etc..The principle that these three electrodes monitor electric field is identical, relies primarily on different reversible reactions, works as surrounding
Electric field signal when changing, the charged ion in reversible reaction is moved by the effect of electric field, leads to reversible reaction
It is broken, electrode potential is caused to change.Monitoring electrode potential variation counter can push away the situation of change of electric field signal.Wherein copper/sulfuric acid
Copper electrode to very poor larger, is mainly used for the monitoring of land electric field to, lead/chlorination lead electrode；Silver/silver chloride electrode is mainly led at present
Cross it is powder sintered be made, compare copper/copper sulfate electrode and lead/chlorination lead electrode, powder sintered silver/silver chloride electrode have electrode
The advantages that performance stabilization, long service life, but its ohmic internal resistance is big, anti-polarizability is poor, and current potential easily drifts about, and both influences electric field
Measurement influences corrosion monitoring again.In view of silver it is expensive, it is at high cost, how can improve electrode stability, reduce noise and
Cost can be reduced, is always the target that people pursue.Electrode specific surface area is bigger, and electrode stability will significantly improve, this will
Advantageous Yu Haiyang's electrical field test and corrosion monitoring, the service performance for improving whole system are of great significance.Foam is carbon-based
On the one hand the preparation of Ag/AgCl electric field electrode uses high, cheap, light weight the foamy carbon of specific surface area as matrix material
Material, it is this on the other hand by, using chemistry and electrochemical method deposition silver, obtaining silver layer in homogeneous thickness in foam carbon surface
Method can be such that the usage amount of silver reduces so as to reduce preparation cost.Meanwhile the carbon-based Ag/AgCl electric field electrode of foam has high ratio
Surface area, high stability and low noise, thus in ocean wideband electric field signal monitoring and corrosion monitoring field its have it is very high
Application value.
Summary of the invention
In view of the above problems, the present invention is prepared for a kind of carbon-based Ag/AgCl electric field electrode of high-specific surface area foam.To realize
The purpose of the present invention, the carbon-based Ag/AgCl electric field electrode structure of high-specific surface area foam are as shown in Figure 1.Preparation method is as follows:
The foamy carbon for connecting carbon plate is shaped.
Pretreatment: activation, cleaning, drying.
Foam carbon surface electrochemistry preplating metallic copper or nickel first, then surface chemistry is silver-plated, and electroplated thickening forms equal
Even silver layer.
Foam carbon surface silver generates silver chloride layer using method for electrodeposition.
The carbon-based Ag/AgCl electrode of foam is installed in microporous pipe, filler is filled, passes through the carbon plate being connected with foamy carbon
Extraction wire.
Electrode method is prepared to describe it for foamy carbon electroplate in the content of present invention, with prior art phase
Than gain effect of the invention is:
The carbon-based Ag/AgCl electric field electrode good conductivity of high-specific surface area foam, surface area are big, significantly improve the stabilization of electrode
Property.
High-specific surface area foamy carbon makes Ag/AgCl electric field electrode anti-polarization performance with higher.
Foamy carbon substrate quality is light, reduces electrode weight.
Foamy carbon is cheap, significantly reduces electrode cost.
The carbon-based Ag/AgCl electric field electrode of high-specific surface area foam has high stability, is conducive to accurately measure corrosion potential,
Be conducive to the accurate control that electric current is protected erosion prevention system.
The carbon-based Ag/AgCl electric field electrode of high-specific surface area foam enables the accurate controlling potential of erosion prevention system, extends system
It unites the service life.
Microporous pipe outside electrode is advantageously implemented exchange of seawater, prevents ocean current from influencing.
Microporous pipe outside electrode can be realized the carbon-based Ag/AgCl electric field electrode of foam and be kept in dark place.
The carbon-based Ag/AgCl electric field electrode potential difference (very poor) of high-specific surface area foam is small, and stability is high, is conducive to pairwise testing
External electrical field.
The carbon-based Ag/AgCl electric field electrode of high-specific surface area foam has high stability, low self noise, to extraneous electric field energy spirit
Quick response is conducive to the precision for improving electrical field test.
Detailed description of the invention
Fig. 1 is the carbon-based Ag/AgCl electrode structure schematic diagram of high-specific surface area foam
Wherein: 1, conducting wire 2, filler 3, end cap 4, microporous pipe 5, Ag/AgCl layer 6, foamy carbon
Specific embodiment:
The present invention is further described below according to Figure of description and embodiment, following embodiment is only used for clearer
Ground illustrates design scheme of the invention, and cannot be limited the scope of the invention with this.
Embodiment 1
As shown in Figure 1, the present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam,
The foamy carbon finished product 6 for connecting carbon plate being processed into the shape that shape is cylindrical body, wherein 5 mm of radius, length is 5 cm, activate,
After cleaning and drying process, foam carbon surface carries out electrochemistry preplating metal nickel layer, then the method deposition one for passing through chemical silvering
Layer metallic silver, then plating thickeies silver layer, recycles the method for electrolytic deposition in the electrolytically generated silver chlorate 5 of silver layer surface, then will
The carbon-based Ag/AgCl electrode of foam is installed in microporous pipe 4, fills quartz sand filler 2, draws silver wire 1.
Embodiment 2
As shown in Figure 1, the present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam,
The foamy carbon finished product 6 for connecting carbon plate is processed into the shape that shape is cylindrical body, wherein 10 mm of radius, length is 15 cm, living
Change, after cleaning and drying process, foam carbon surface carries out electrochemistry preplating metal nickel layer, then is deposited by the method for chemical silvering
One layer of metallic silver, then plating thickeies silver layer, recycles the method for electrolytic deposition in the electrolytically generated silver chlorate 5 of silver layer surface, then
The carbon-based Ag/AgCl electrode of foam is installed in microporous pipe 4, quartz sand filler 2 is filled, draws silver wire 1.
Embodiment 3
As shown in Figure 1, the present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam,
The foamy carbon finished product 6 for connecting carbon plate is processed into the shape that shape is cylindrical body, wherein 15 mm of radius, length is 50 cm, living
Change, after cleaning and drying process, foam carbon surface carries out electrochemistry preplating metal copper layer, then is deposited by the method for chemical silvering
One layer of metallic silver, then plating thickeies silver layer, recycles the method for electrolytic deposition in the electrolytically generated silver chlorate 5 of silver layer surface, then
The carbon-based Ag/AgCl electrode of foam is installed in microporous pipe 4, quartz sand filler 2 is filled, draws silver wire 1.
Embodiment 4
As shown in Figure 1, the present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam,
The foamy carbon finished product 6 for connecting carbon plate is processed into the shape that shape is cuboid, wherein 10 mm of length, 5 mm of width, height 30
Mm, after activation, cleaning and drying process, foam carbon surface carries out electrochemistry preplating metal copper layer, then the side for passing through chemical silvering
Method deposits one layer of metallic silver, and thickening silver layer can so be electroplated, recycle the method for electrolytic deposition in the electrolytically generated chlorination of silver layer surface
Silver 5, then the carbon-based Ag/AgCl electrode of foam is installed in microporous pipe 4, quartz sand filler 2 is filled, silver wire 1 is drawn.
Embodiment 5
As shown in Figure 1, the present invention relates to a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam,
The foamy carbon finished product 6 for connecting carbon plate is processed into the shape that shape is cylindrical body, wherein 5 mm of radius, length is 50 cm, living
Change, after cleaning and drying process, foam carbon surface carries out electrochemistry preplating metal copper layer, then is deposited by the method for chemical silvering
One layer of metallic silver, then plating thickeies silver layer, recycles the method for electrolytic deposition in the electrolytically generated silver chlorate 5 of silver layer surface, then
The carbon-based Ag/AgCl electrode of foam is installed in microporous pipe 4, tripolite filling material 2 is filled, draws silver wire 1.
Embodiment 6
In the corrosion potential experiment of the measurement high NiCr alloy coat of 40Cr carbon steel, using LK2005B electrochemical workstation,
Three-electrode system, the electrode wherein the 40Cr carbon steel of high NiCr alloy coat is worked, platinum electrode are done to electrode, successively select saturation
Calomel electrode and the carbon-based Ag/AgCl electric field electrode of foam do reference electrode, test corrosion potential, comparison hair using potentiostatic method
Existing, when doing reference electrode test using the carbon-based Ag/AgCl electric field electrode of foam, obtained potential curve is steady, corrosion potential value
It is more accurate.
Embodiment 7
The carbon-based Ag/AgCl electric field electrode of foam is inside cuboid glass container and fixed to putting into parallel vertically, to glass
Natural sea-water is added in glass container, makes the carbon-based Ag/AgCl electric field electrode of foam to being completely immersed in seawater；With data collecting instrument
Voltage channel records the carbon-based Ag/AgCl electric field electrode of foam to the voltage change at both ends, has recorded the very poor variation of 90 hours
Situation.Very poor drift value is 18 μ V or so in such the carbon-based Ag/AgCl electric field electrode of foam 24 hours, with high very poor steady
It is qualitative.
Embodiment 8
By the carbon-based Ag/AgCl electric field electrode of foam to putting into parallel vertically inside cuboid glass container and fixed, Xiang Qi
Middle addition natural sea-water makes the carbon-based Ag/AgCl electric field electrode of foam to being completely immersed in seawater；It is put into emission electrode (carbon plate),
And be connected with signal generator, emission electrode and the carbon-based Ag/ of foam are recorded respectively with two voltage channels of data collecting instrument
Voltage change of the AgCl electric field electrode to both ends.The output signal of signal generator is arranged are as follows: 1 mHz, 50 mV.Foamy carbon
Base Ag/AgCl electric field electrode is accurately monitored the electric field signal of signal generator transmitting.
Embodiment 9
The carbon-based Ag/AgCl electric field electrode of a pair of of foam is placed on to inside cuboid glass container and fixed, string in parallel vertically
Resistance box on connection connects DC power supply, with very poor variation between data logger voltage channel recording electrode pair.Pass through when test
DC power supply applies 924.8 nA continuous currents, and polarize 1min.It is computed, the carbon-based Ag/AgCl electric field electrode of foam is to 924.8
The polarization resistance R generated when nA constant current 1 min of polarizationPolarization=△ the Ω of U/I=25.81, polarization resistance is small, and anti-polarization performance is good.
Embodiment 10
By the carbon-based Ag/AgCl electric field electrode of foam to putting into parallel vertically inside cuboid glass container and fixed, Xiang Qi
Middle addition natural sea-water makes the carbon-based Ag/AgCl electric field electrode of foam to being completely immersed in seawater；It is put into emission electrode (carbon plate),
And be connected with signal generator, emission electrode and the carbon-based Ag/ of foam are recorded respectively with two voltage channels of data collecting instrument
AgCl electric field electrode records the current signal in circuit with data logger current channel to the voltage change at both ends.Signal is sent out
The output signal frequency of raw device is set as 10 mHz, and amplitude is respectively 1 mV, 5 mV, 10 mV, 50 mV, 100 mV, is calculated
Its linearity reflects that the carbon-based Ag/AgCl electric field electrode of foam can accurately respond electric field signal less than 0.1% out.
Embodiment 11
By the carbon-based Ag/AgCl electric field electrode of foam to being placed in parallel into plastic containers vertically, 3.5%NaCl solution is added, it will
Electrode pair is connected with low-noise amplifier and data collecting instrument and is put into screened room.After electrode is to 24 h is impregnated, Acquisition Instrument
Start the open-circuit voltage of measuring electrode pair, sample frequency 2kHz, measurement range is -10 mV of mV~+10, obtains electrode and surveys
Aggregate system noise is measured, measuring system intrinsic noise is subtracted, this electric-field sensor can be found out and made an uproar in 1Hz frequency point power spectrum root mean square
Sound.It is computed, self noise numerical value is 1.6 nV/@1Hz。
Claims (1)
1. a kind of carbon-based Ag/AgCl electric field electrode preparation method of high-specific surface area foam, which is characterized in that the electric field electrode benefit
Use high-specific surface area foamy carbon as basis material, preparation step is as follows:
Step (1), the foamy carbon for connecting carbon plate is shaped, activated, cleaning and drying process；
Step (2), in step (1) treated foamy carbon surface electrochemistry preplating metallic copper or nickel；
Step (3), the foam carbon surface of preplating metallic copper or nickel is deposited by the method for chemical silvering in step (2)
Metallic silver, then electroplated thickening forms uniform silver layer, and method for electrodeposition is recycled to generate silver chloride layer in silver surface, is made
The carbon-based Ag/AgCl electrode of foam；
The carbon-based Ag/AgCl electrode of foam made from step (3) is installed in microporous pipe by step (4), is filled filler, is passed through
The carbon-based Ag/AgCl electric field electrode of high-specific surface area foam is made in the carbon plate extraction wire being connected with foamy carbon.
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| CN113063995B (en) * | 2021-03-16 | 2022-12-16 | 中国海洋大学 | Carbon-based conductive polymer film underwater electric field sensor |
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| CN103616529A (en) * | 2013-12-13 | 2014-03-05 | 国家海洋技术中心 | Expendable type electromagnetic ocean current profile measuring probe |
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