CN108827868A - A kind of coating failure monitoring probe and live coating failure quick monitoring method - Google Patents
A kind of coating failure monitoring probe and live coating failure quick monitoring method Download PDFInfo
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Abstract
The present invention relates to a kind of coating failure monitoring probe and live coating failure quick monitoring methods, the coating failure monitoring probe include pop one's head in cavity, positioned at probe chamber it is intracorporal probe inner core, positioned at probe cavity lower end base bottom plate and outer guide line, pop one's head in cavity upper end opening;The probe inner core is made of working electrode, reference electrode and auxiliary electrode, working electrode, reference electrode and auxiliary electrode bottom end are arranged on bottom plate, it is equipped with insulated enclosure layer between three electrode gap settings and adjacent electrode, the top of three electrodes forms a working face at cavity upper end opening.The monitoring probe structure is simple, response sensitivity is high, the service life is long, high reliablity.The fast slowdown monitoring sensor of live coating failure of the invention uses electrochemical impedance principle, coating failure monitoring probe combine ac impedance measurement instrument, detection parameters are more, response sensitivity is high, it can be achieved that carrying out real time monitoring in commission coating aging state and aging speed.
Description
Technical field
The present invention relates to corrosion monitoring and protection technology field more particularly to a kind of coating failure monitoring probe and scenes
Coating failure quick monitoring method.
Background technique
In order to preferably prevent and reduce the influence of corrosion, many engineerings and project use coating protection technology.Coating meeting
It is influenced by factors such as moisture absorption, climate change, external force damage, constructional deficiencies, these corrosion-inhibiting coatings can be with the time
There is the phenomenon that ageing failure in passage, and antiseptic property is caused to decline, final overall structure failure.Equipment is also resulted in when serious
It Deng being destroyed, or even can also cause serious burst accident, economic asset even casualties be caused, to production, life band
To lose or inconvenient.Therefore, it is very necessary for taking scientific and effective safeguard procedures.
Method in existing invention about coating aging failure monitor is related to the fields such as sound, light, electricity, needs into one
Step development and improvement.Wherein, main method one of of the electrochemical impedance spectroscopy (EIS) as assessment, many researchers incited somebody to action
Its protection field for applying coating.It is by traditional three-electrode system by a sine wave shaped voltage (electric current)
When the disturbance of AC signal, 10-2~105Corresponding electric current (voltage) response signal of measurement in the frequency range of Hz, by these
Signal calculates the impedance of available electrode again.By Equivalent Circuit Fitting, parameter can be handled by professional's digital simulation
Out, for assessing coating performance.But this method needs coating to immerse the electrode in electrolyte, stable reference electricity
Pole, it is accordingly required in particular to the analysis tool of a set of profession.Therefore, inconvenient to the site inspection of vehicle or aircraft coating.
Summary of the invention
For the technical problems in the prior art, the object of the present invention is to provide a kind of monitorings of coating failure
Probe and the fast slowdown monitoring sensor of live coating failure, realize coating real-time monitoring, can learn painting by electrochemical analysis
The protective performance of layer improves the protective action of coating to optimize to coating.
To achieve the above object, the present invention is achieved by the following technical solutions:
Present invention firstly provides a kind of coating failure monitoring probe, the coating failure monitoring probe includes probe chamber
Body, positioned at probe chamber it is intracorporal probe inner core, positioned at probe cavity lower end base bottom plate and outer guide line, the probe chamber
Body upper end opening;The probe inner core is made of working electrode, reference electrode and auxiliary electrode, working electrode, reference electrode
It is arranged on bottom plate with auxiliary electrode bottom end, is equipped with insulated enclosure layer between three electrode gap settings and adjacent electrode;Three
The top of a electrode forms a working face at cavity upper end opening;The working electrode, reference electrode and auxiliary electrode are equal
It is made of metal material;The outer guide line connection probe inner core simultaneously stretches out probe cavity.
Further, the probe cavity is made of ABS resin material.
Further, the working electrode is cylindrical tube shape, and reference electrode and auxiliary electrode are ring-type, the work
Electrode, reference electrode and auxiliary electrode are highly identical and are coaxially disposed, and working electrode is internally positioned, reference electrode is covered and worked
Electrode exterior, auxiliary electrode cover outside reference electrode, and the upper surface of three electrodes forms a work at cavity upper end opening
Make face.
Further, the radial distance of the working electrode and reference electrode is less than 0.5mm, reference electrode and auxiliary electricity
Pole radial distance is less than 0.5mm.
Further, the gap between two neighboring electrode is filled with ABS with the isolation that is electrically insulated.
Further, the outer guide line is quad, and the quad includes the work electricity for connecting working electrode
Polar conductor, the reference electrode conducting wire for connecting reference electrode, the auxiliary electrode conducting wire for connecting auxiliary electrode and GND ground line.
Further, several magnetic parts are set on the bottom plate, and the magnetic part is for adsorbing coating monitoring probe
In metal surface to be measured.
Further, it is packaged between the magnetic part and bottom plate with ABS resin.
Second object of the present invention is to provide a kind of live coating failure fast slowdown monitoring sensor, the sensor
Including coating failure monitoring probe described in any of the above embodiments, coating failure monitoring probe passes through the connection exchange resistance of outer guide line
Anti- tester.
Third object of the present invention is to provide a kind of live coating failure quick monitoring method, and the method is logical
The fast slowdown monitoring sensor of the live coating failure crossed includes the following steps come what is realized:
(1) initial impedance modulus value and starting phase angle are obtained:Initial time is monitored, it will be identical with metal coating to be measured
New coating is coated on the working face of coating failure monitoring probe, and ac impedance measurement instrument applies the 10- of a fixed frequency
The sine wave signal of 30mV forms current loop in detecting head surface, is calculated, obtained by IV conversion circuit and phase correlation method
The initial impedance modulus value and starting phase angle of the lower initial time of certain fixed frequency;
(2) the measurement impedance magnitude and measured phase angle at certain measurement moment are obtained:Certain measurement moment, ac impedance measurement
Instrument applies one and step (1) identical sine wave signal, forms current loop in detecting head surface, by IV conversion circuit and
Phase correlation method calculates, and obtains the measurement impedance magnitude and measured phase angle at certain lower measurement moment of certain fixed frequency;
(3) it is calculated by initial impedance modulus value and starting phase angle and obtains initial characteristics frequency and initial specific capacitance, passed through
It measures impedance magnitude and measured phase angle calculates and obtains measurement characteristic frequency and measurement specific capacitance;And according to initial impedance modulus value
Aging coefficient is calculated with measurement impedance magnitude;
(4) coating is evaluated according to impedance value, phase angle, four indexs of characteristic frequency and specific capacitance and aging coefficient
Aging conditions.
The working principle of the invention:
The principle of the present invention is based on microelectric technique, using the method for electrochemical impedance (EIS) to coating aging degree
It is assessed.The present invention proposes five key index relevant to EIS phase angles (θ), characteristic frequency (fb), specific capacitance (C),
Impedance modulus (Z) and aging coefficient (δ), for assessing the degree of aging of coating.Principle is specifically described as follows:
Before introducing coating aging monitoring signals, it is necessary to first introduce the calculation method of coating capacitor and resistance.
1. for coating capacitor:
CC=ε ε0A/d (1)
CCCoating capacitor is represented, A is coating area, and d is coating layer thickness, and ε represents dielectric constant, ε0It is initial dielectric constant
It is 8.86 × 10-14F/cm。
Coating resistance is related to the porosity in coating:
Wherein ρ represents hole resistivity, Ad coating stripping area,It is coating initial resistance.
The calculation formula of impedance magnitude Z such as equation:
Wherein ω is angular frequency, RsSolution resistance, RcAnd CcRespectively represent coating resistance and coating capacitor.
2. phase angle θ is defined as
Wherein ZImAnd ZReRespectively represent the imaginary part and real part of impedance.
For intact coating, resistance is larger, capacitor very little, and coating is equivalent to a capacitor, therefore electric current
Be by this capacitor, phase angle in intermediate frequency to high frequency very wide range close to 90 °, but due to coating itself soak process, electricity
Appearance is gradually increased, and resistance reduces, and portion of electrical current is by resistance, and phase angle can be gradually reduced at this time, and when coating water suction reaches
After saturation, coating capacitor variation is smaller, and resistance will continue to reduce at this time, therefore phase angle can also reduce significantly,
The variation at phase angle can reaction coating resistance and capacitance variations, can choose under the conditions of determining frequency corresponding phase angle under 10Hz
θ10HzAs potential coating aging monitoring signals.
3. being the corresponding frequency when phase angle is 45 ° for characteristic frequency, it is believed that it is related with the peeling area of coating,
And usually in high band, the processing of unwanted complexity can be extracted from impedance data, therefore can be very good as monitoring
Signal.
When θ=- 45 °,
2πfbRCCC=1 (5)
Bringing equation (2) and (3) into can obtain,
fb=1/2 π RCCC=Ad/2πρεε0A (6)
It is the frequency that coating integrally falls off.
Therefore it can be found that fbIt is, when coating intact f related with fall off area of the coating in matrixbIt is smaller, work as coating
After the area that falls off in ageing process is gradually increased, fbAlso increasing.
4. for the imaginary part of impedance:
When frequency is higher, equation can convert, therefore can quickly calculate coating capacitor C in high frequency pointsc。
CC=1/2 π fZIm (9)
5. the degree of aging of coating can be calculated according to following formula:
δ-aging coefficient (Degradation coefficiency), R0Initial impedance modulus value under certain fixed frequency, RtCertain fixed frequency
Under it is a certain when the impedance magnitude inscribed, the degree of aging of coating can be calculated by the formula.
During actual monitoring, coating monitoring probe combination electrochemical impedance tester can be obtained intuitively by test
The impedance magnitude at a certain moment under certain fixed frequency and phase angle, and according to calculating it can be concluded that characteristic frequency (fb), specific capacitance
(C) and aging coefficient δ.The value that different industries define the critical aging coefficient of coating failure is different;Same industry, aging coefficient
Value is bigger, and the degree of coating failure is higher;In conjunction with impedance magnitude, phase angle, characteristic frequency (fb) and specific capacitance (C) four
The variation of index, comprehensive assessment coating aging state.
Compared with prior art, the beneficial effects of the present invention are:
(1) coating failure monitoring probe structure provided by the invention is simple, response sensitivity is high, the service life is long, reliability
Height, probe uses the fixed form of adsorbing metal coating, easy to operate and can play good fixed effect, is live
Test offers convenience.
(2) the live fast slowdown monitoring sensor of coating failure provided by the invention uses electrochemical impedance principle, will be of the invention
Coating failure monitoring probe combine ac impedance measurement instrument, detection parameters are more, response sensitivity is high, can be achieved at the same time to clothes
Coating aging state and aging speed in labour carry out real time monitoring, especially suitable for bridge, marine facility, aircraft
Deng service safety carry out long-term follow monitoring.For more comprehensively, more reliably evaluating and testing device security and coating military service longevity
Life has highly important practical significance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the coating failure monitoring probe of embodiment 1;
Fig. 2 is the sectional view of the coating failure monitoring probe of embodiment 1;
Fig. 3 is the Z of the portable coating probe of three kinds of differences in embodiment 30.1HzChange under salt fog acceleration environment at any time
Change schematic diagram;
Fig. 4 is the f of the portable coating probe of three kinds of differences in embodiment 3bIt changes with time under salt fog acceleration environment
Schematic diagram;
Fig. 5 is the θ of the different portable coating probes of kind in embodiment 310HzIt changes with time under salt fog acceleration environment
Schematic diagram.
Specific embodiment
It shows that example illustrates certain embodiments of the present invention, and should not be construed as limiting model of the invention
It encloses.Present disclosure can be improved from material, method and reaction condition simultaneously, all these improvement should all
It falls within spirit and scope of the invention.
Electrochemical AC impedance method (EIS) disturbs tested electrode using AC signal by a small margin, will not cause serious
Concentration polarization or electrode surface state change, and avoid strong polarization method and cross large disturbances to what electrode system generated.Pass through synchronization
The electric potential signal of measuring electrode and corresponding current-responsive, the exchange of tested electrode is calculated by means of correlation analysis algorithm
Impedance spectrum finally obtains polarization resistance and dielectric resistance using Equivalent Circuit Fitting.EIS measurement result stabilization, anti-interference ability
By force, corrode high resolution, the variation of coating can be reflected by obtained impedance spectrum, to learn the protective performance of coating.
Embodiment 1:
Fig. 1 is a kind of specific structure of coating failure monitoring probe that combination electrochemical AC impedance principle uses, in conjunction with
Fig. 1 and Fig. 2, the coating failure monitoring probe include probe cavity 4, are located at the intracorporal probe inner core of probe chamber, are located at probe chamber
The bottom plate of body bottom and outer guide line 5,4 upper end opening of cavity, bottom plate is preferably stainless steel plate.The outer connection of guide line 5 probe
Inner core simultaneously stretches out probe cavity 4.
Cavity 4 is made of ABS resin shell, which is cylindrical tube shape structure, and longitudinally middle position is in probe
Core.The probe inner core is using electrochemistry three-electrode system defined in, including working electrode 1, reference electrode 2 and auxiliary
Electrode 3, three kinds of electrodes are all by 7075 aluminium alloys (weight %:Cu 1.72, Fe 0.31, Si 0.09, Mn 0.33, Cr
0.15, Ti 0.03, Al surplus) it is made, working electrode 1, reference electrode 2 and the coaxial arrangement of auxiliary electrode 3 and three electrode height
Spend identical, wherein working electrode 1 is that cylindrical tube shape is located at center, and reference electrode 2 is cyclic annular close to working electrode, auxiliary electricity
Pole 3 is also cyclic annular be located on the outside of reference electrode.In the present embodiment, the diameter of internal work electrode 1 is 11.3mm, intermediate reference
The internal diameter of electrode 2 is 12.2mm, outer diameter 16.7mm, and the internal diameter of external auxiliary electrode 3 is 17.6mm, outer diameter 21mm, is protected
The radial distance for demonstrate,proving working electrode and reference electrode is less than 0.5mm, and reference electrode and auxiliary electrode radial distance are less than 0.5mm,
It is filled with ABS with the isolation that is electrically insulated in gap between each adjacent two electrode.The top of three electrodes shown in FIG. 1 is in cavity
A working face is formed at upper end opening.Outer guide line is quad, is drawn from the inner core of probe, can be with electrification
Learn testing impedance connection.Wherein quad is respectively the working electrode conducting wire 6 of welding electrode, welding reference electrode
Reference electrode conducting wire 7, the auxiliary electrode conducting wire 8 for welding auxiliary electrode and GND ground line 9.The setting of stainless steel plate upper peripheral
There are four permanent magnetism metal trough, place permanent magnet respectively and be used to be adsorbed on metal surface to be measured to fix probe, permanent magnet with
And it is encapsulated around stainless steel plate with ABS resin.In the present invention, other magnetic parts that can play suction-operated be also can
With, it is not limited to permanent magnet.
It should be further noted that the distance between annular electrode need to be within 0.5mm.During coating aging,
Coating itself may be considered that there is one layer very thin electrolyte layer water on surface after absorbing trace water.As ionic current (H+, Cl-
Deng) migrated between the working electrode 1 and annular auxiliary electrode 3 of coating when, electric current will along in working electrode 1 and auxiliary electricity
The surface of pole 3.Obviously, it is uniform to can be regarded as horizontal distribution for electric current.Therefore, coating sensor probe is substantially one
Planar capacitor.In addition, the current distribution on two electrode surfaces is uniform, it is desirable that auxiliary electrode 3 and working electrode 1 have
There is identical surface area.So coating sensor is very sensitive in conjunction with EIS technology, absorb water especially for coating degradation to coating
The monitoring in stage.
The working face of probe uses 200# sand paper to polish first, is then polished with 600# sand paper, is then washed and done with hexane
It is dry to be finally stored in the container with nitrogen.
Embodiment 2:
Four conducting wires of the monitoring probe in the present embodiment are connected on ac impedance measurement instrument, that is, are constituted a kind of existing
The fast slowdown monitoring sensor of sound coating failure.The sensor is using ac impedance technology come field monitoring coating failure degree, tool
Body method is:
(1) initial impedance modulus value and starting phase angle are obtained:Initial time is monitored, it will be identical with metal coating to be measured
New coating is coated on the working face of coating failure monitoring probe, and ac impedance measurement instrument applies the 10- of a fixed frequency
The sine wave signal of 30mV forms current loop in detecting head surface, is calculated, obtained by IV conversion circuit and phase correlation method
The initial impedance modulus value and starting phase angle of the lower initial time of certain fixed frequency;
(2) the measurement impedance magnitude and measured phase angle at certain measurement moment are obtained:Certain measurement moment, ac impedance measurement
Instrument applies one and step (1) identical sine wave signal, forms current loop in detecting head surface, by IV conversion circuit and
Phase correlation method calculates, and obtains the measurement impedance magnitude and measured phase angle at certain lower measurement moment of certain fixed frequency;
(3) it is calculated by initial impedance modulus value and starting phase angle and obtains initial characteristics frequency and initial specific capacitance, passed through
It measures impedance magnitude and measured phase angle calculates and obtains measurement characteristic frequency and measurement specific capacitance;And according to initial impedance modulus value
Aging coefficient is calculated with measurement impedance magnitude;
(4) coating is evaluated according to impedance value, phase angle, four indexs of characteristic frequency and specific capacitance and aging coefficient
Aging conditions.
Embodiment 3:
Salt fog accelerated test is carried out using the portable coating probe (A-PU, F-PU, PU) of three kinds of differences.According to ISO7253
Standard carries out neutral salt spray test to accelerate coating aging, and all samples are exposed to 5% NaCl (pH=7), temperature 35
It is carried out in ± 2 DEG C of salt spray chamber.Salt spray test is set as 60 minutes spraying intermittent sprayings and 60 minutes drying rooms and hands over every to simulate
Drying and wet processes in tubing flow displacement mist marine environment.Simultaneously under real-time testing difference ageing time coating electrochemical impedance.
Testing impedance parameter:Alternating-current magnitude 20mV, range of scanned frequencies 100kHz~0.01Hz, log scan, 10 points/10 frequencys multiplication.
When test result shows that portable coating probe (A-PU, the F-PU, PU) salt fog of three kinds of differences accelerates, with the time
Passage, the diameter length of capacitive reactance arc reduces, and there is decreasing trend at phase angle.Fig. 3~Fig. 5 is that the portable coating of three kinds of differences is visited
The Z of head (A-PU, F-PU, PU)0.1Hz、fb、θ10HzChanging with time under salt fog acceleration environment.Based on the above content point
Analysis, once Z0.1Hz<106Ω·cm2, fb>100Hz or θ10Hz<20 °, it is believed that the complete aging of coating and gold cannot be protected
Belong to substrate, it means that the barrier properties of coating deteriorate, and this portable coating probe sensor will greatly contribute to examine in early days
Coating failure is measured, risk that may be present is prevented.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited to
This, anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention
And its inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of coating failure monitoring probe, which is characterized in that the coating failure monitoring probe includes probe cavity, is located at and visits
Head cavity it is intracorporal probe inner core, positioned at probe cavity lower end base bottom plate and outer guide line, the probe cavity upper end opening;
The probe inner core is made of working electrode, reference electrode and auxiliary electrode, working electrode, reference electrode and auxiliary electrode bottom
End is arranged on bottom plate, is equipped with insulated enclosure layer between three electrode gap settings and adjacent electrode;The top of three electrodes
A working face is formed at cavity upper end opening;The working electrode, reference electrode and auxiliary electrode are metal material system
At;The outer guide line connection probe inner core simultaneously stretches out probe cavity.
2. a kind of coating failure monitoring probe according to claim 1, which is characterized in that the probe cavity is by ABS tree
Rouge material is made.
3. a kind of coating failure monitoring probe according to claim 1, which is characterized in that the working electrode is cylindrical drum
Shape, reference electrode and auxiliary electrode are ring-type, and the working electrode, reference electrode and auxiliary electrode are highly identical and coaxially set
It sets, working electrode is internally positioned, reference electrode covers outside working electrode, auxiliary electrode covers outside reference electrode, three electricity
The upper surface of pole forms a working face at cavity upper end opening.
4. a kind of coating failure monitoring probe according to claim 3, which is characterized in that the working electrode and reference electricity
The radial distance of pole is less than 0.5mm, and reference electrode and auxiliary electrode radial distance are less than 0.5mm.
5. a kind of coating failure monitoring probe according to claim 3, which is characterized in that between two neighboring electrode
Gap is filled with ABS with the isolation that is electrically insulated.
6. a kind of coating failure monitoring probe according to claim 1, which is characterized in that the outer guide line is that four cores are led
Line, the quad include the working electrode conducting wire for connecting working electrode, the reference electrode conducting wire for connecting reference electrode, connection
The auxiliary electrode conducting wire and GND of auxiliary electrode are grounded.
7. a kind of coating failure monitoring probe according to claim 1, which is characterized in that several are arranged on the bottom plate
Magnetic part, the magnetic part are used to coating monitoring probe being adsorbed on metal surface to be measured.
8. a kind of coating failure monitoring probe according to claim 7, which is characterized in that between the magnetic part and bottom plate
It is packaged with ABS resin.
9. a kind of fast slowdown monitoring sensor of scene coating failure, which is characterized in that the sensor includes claim 1-8 any
Coating failure monitoring probe described in, coating failure monitoring probe connect ac impedance measurement instrument by outer guide line.
10. a kind of scene coating failure quick monitoring method, which is characterized in that the method is by as claimed in claim 9
The live fast slowdown monitoring sensor of coating failure includes the following steps come what is realized:
(1) initial impedance modulus value and starting phase angle are obtained:Initial time is monitored, it will new coating identical with metal coating to be measured
On working face coated in coating failure monitoring probe, ac impedance measurement instrument is applying the 10-30mV of a fixed frequency just
String wave signal forms current loop in detecting head surface, is calculated by IV conversion circuit and phase correlation method, obtains at the beginning of under certain fixed frequency
The initial impedance modulus value and starting phase angle at moment beginning;
(2) the measurement impedance magnitude and measured phase angle at certain measurement moment are obtained:Certain measurement moment, ac impedance measurement instrument apply
One and step (1) identical sine wave signal form current loop in detecting head surface, related to phase by IV conversion circuit
Method calculates, and obtains the measurement impedance magnitude and measured phase angle at certain lower measurement moment of certain fixed frequency;
(3) it is calculated by initial impedance modulus value and starting phase angle and obtains initial characteristics frequency and initial specific capacitance, pass through measurement
Impedance magnitude and measured phase angle, which calculate, obtains measurement characteristic frequency and measurement specific capacitance;And according to initial impedance modulus value and measurement
Impedance magnitude calculates aging coefficient;
(4) the aging feelings of coating are evaluated according to impedance value, phase angle, four indexs of characteristic frequency and specific capacitance and aging coefficient
Condition.
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