CN106198375B - A kind of deep-sea multichannel corrosion electrochemistry in-situ testing device and its test method - Google Patents
A kind of deep-sea multichannel corrosion electrochemistry in-situ testing device and its test method Download PDFInfo
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Abstract
The present invention provides a kind of deep-sea multichannel corrosion electrochemistry in-situ test system and its test method, belong to metal and organic coating coating material corrosion electrochemistry original position field of automatic testing in deep-marine-environment, the device uses oil reservoir logging high pressure sealing technology, by power supply, precision analog and digital circuit, the function element such as memory and electrochemical sensor are sealed in pressure hull, form the deep-sea corrosion electrochemistry work station of black box minor, electro-chemical test is carried out in as deep as 3000 meters of seawater, realize corrosion potential/electric current, all kinds of measurement data such as constant potential/galvanostatic polarization and AC impedance are acquired and store according to the frequency of setting.The configuration of the present invention is simple is compact, and scalability is high, can carry out the electrochemical in-situ test under various metals or organic coating coating sample deep-marine-environment simultaneously；, independent current source simple with reclaimer operation is laid, it is high pressure resistant, small in size, it in conjunction with the deep sea installations of any other form or can be carried, long working life.
Description
Technical field
The invention belongs to metals in deep-marine-environment and organic coating coating material corrosion electrochemistry original position automatic test technology
Field is related to a kind of deep-sea multichannel corrosion electrochemistry in-situ test system and its test method.
Background technique
As scientific and technological progress and earth resource are increasingly depleted, the mankind, which are pursuing always, expands deep space, deep-sea and the activity of deep ground
Space.The development and application of exploitation exploration, the deep-sea engineering construction and deep sea equipment of deep-sea oil gas, mineral products and living resources,
Key content as China's Development of Marine economy.Nowadays, China's autonomous Design, integrated manned underwater vehicle " flood dragon " number be
Deep diving is to 7000 meters.No. 981 semi-submersible type deepwater drilling platforms of offshore oil, depth of implements have marched the South Sea up to 3050 meters, have opened
Beginning deep ocean work.However, deep sea equipment is faced with serious corrosion harmfulness, and is possible to due to the particularity of deep-marine-environment
As exploitation deep-sea resources, using deep-sea space and construction deep-sea engineering system technical bottleneck, thus influence China ocean warp
Ji shapes up with deep sea equipment.Therefore the etching problem for researching and solving equipment material in deep-marine-environment is very urgent,
As the research hotspot in current material corrosion subject.
Compared with land equipment and shallow sea equipment, maximum deep sea equipment is not both to be acted on by huge static pressure.?
Some researches show that deep sea static pressure power and deep-sea corrosion may make the mechanical property of material that deep fades occur.Organic coating is
To one of the most important means of offshore engineering structure protection in deep-marine-environment, deep sea pressure can accelerate the failure of organic coating, lead
Cause the earlier period damage of marine ship, oil platform, bathyscaph etc..Therefore, for corrosion of metal behavior in deep-marine-environment and have
The research of organic coating inefficacy mechanism, it has also become the problem of current various countries' corrosion scientific research personnel extremely pays close attention to.Current deep-sea material is rotten
Corrosion test research, mainly uses indoor simulation Acceleration study, and achieved many significant datas.However, real sea test more connects
The true service state of nearly material, data are more valuable.Due to the shortage of deep-sea electro-chemical test means, current real sea is surveyed
Examination mostly using weightless lacing film method, can not in real-time display or characterization deep-sea material corrosion kinetics process and aging shape
State can only judge extent of corrosion by sampling analysis after the end of the experiment.And to reflect the Dynamic Corrosion failure of material in real time
Behavior, it is necessary to carry out real extra large electrochemical in-situ research, it is horizontal that this will effectively promote deep-sea corrosion research.
Utility model content
Technical assignment of the invention be in view of the deficiencies of the prior art, seek development and design it is a kind of can 3000 meters of the depth of water with
The test device long-term in interior deep-sea marine environment, in situ for carrying out metal or organic coating coating material electrochemical data acquisition and
Its test method integrates power supply, electrochemical sensing and data and determines frequency acquisition/store function, can one-shot measurement at least four
The Electrochemistry Information of a above sample, it is corresponding anti-by corrosion potential/electric current, polarization curve and the measurement of ac impedance spectroscopy parsing
Heat/kinetic parameter is answered, in conjunction with the measurement data of marine environment, specifies deep-marine-environment material corrosion failure mechanism model.
The technical solution adopted by the present invention to solve the technical problems is: using oil reservoir logging high pressure sealing technology (>
30 MPa), the function element such as power supply, precision analog and digital circuit, memory and electrochemical sensor are sealed in titanium and are closed
In golden pressure hull, the deep-sea corrosion electrochemistry work station of black box minor is formed, electricity can be carried out in as deep as 3000 meters of seawater
Test chemical realizes all kinds of measurement data such as corrosion potential/electric current, constant potential/galvanostatic polarization and AC impedance according to setting
The fixed frequency is acquired and stores.Set of device can load more than one piece metal or organic coating coating sample, launch 100 ~
In the seawater of 3000 meters of depths, 1 ~ 6 month time can be laid under water according to test requirements document.
1, the present invention provides a kind of deep-sea multichannel corrosion electrochemistry in-situ test system, is designed using compact structure,
All chips are all made of high-density packages form, and main structure includes pressure hull and top cover, and pressure hull and top cover form
The closed test space, and inside it in space install multi-channel measurement electrode system, amplifier scaling circuit and filtering/
Compensation circuit, analog-digital converter, timer clock, power module, singlechip microcontroller, memory, digital-to-analogue conversion
Device and channel selecting relay, wherein
The power module is connected with singlechip microcontroller, and required operating voltage is provided for system；
The multi-channel measurement electrode system is set in pressure hull, and is stretched out by top cover comprising multiple parallel connections are even
The corrosion monitoring component connect；
The amplifier scaling circuit and filtering/compensation circuit are connected to the rear end of multi-channel measurement electrode system, mould
The front end of quasi- digital quantizer, is used for adaptively selected range, realizes the range switching during system electrochemical measurement；
The analog-digital converter and singlechip microcontroller interconnect, and for being acquired to signal, are passed to single-chip microcontroller
It calculated, handled and is stored in micro controller；
The timer clock is connected with singlechip microcontroller, provides correct time for system and carries out forced resetting, is
The relevant parameter and measurement result of system are stored in memory, and are communicated through communication interface and host computer；
The digital analog converter is connected to the output end of single-chip microcontroller micro controller, treats for generating a variety of pumping signals
Survey system is motivated, and according to the type of pumping signal, carries out electrochemical in-situ test；
The channel selecting relay is connected to the rear end of digital analog converter, before multi-channel measurement electrode system
End, for carrying out on-off in a manner of selecting one to multi-channel measurement electrode system.
Further, the corrosion monitoring component includes that resistance probe and three electrodes of the sudden and violent leakage in the corrosive environment of deep-sea are visited
Head, three electrode probes include working electrode, reference electrode and to electrode, and working electrode selects metal or organic coating coating to be measured
Material.
Further, three electrode probe and resistance probe sensing element use PEEK fire resistant special type Material injection
Molding, forms integrated corrosion monitoring component.
Further, the sealing ring between the corrosion monitoring component and top cover uses fluoroplastics sealing material, prevents liquid
It penetrates into inside pressure hull.
Further, the power module includes battery pack and electric pressure converter, and battery pack is system through electric pressure converter
Operating voltage is provided, or directly provides operating voltage by battery pack for system.
Further, the memory uses SD card data storage.
Further, the size of the pressure hull is designed as cylindrical shape according to the size of measuring system.
Further, the pressure hull material is selected as titanium alloy.
Further, using the close silk helixseal connection of rubber o-ring between the pressure hull and top cover.
Further, the singlechip microcontroller handles chip using STM32.
Further, the corrosion monitoring component count is at least four groups.
2, the present invention also provides a kind of deep-sea multichannel corrosion electrochemistry home position testing method, include the following steps:
1) utilize oil reservoir logging high pressure sealing technology, by multi-channel measurement electrode system, amplifier scaling circuit with
Filtering/compensation circuit, analog-digital converter, timer clock, power module, singlechip microcontroller, memory, digital simulation
Converter and channel selecting relay are sealed in the test space composed by pressure hull and top cover, and assembling is prepared into above-mentioned
A kind of deep-sea multichannel corrosion electrochemistry in-situ test system；
2) carry out deep-sea dispensing: the device that step 1) is assembled is fixed on deep-sea test device carries test for a long time,
Or real-time Electrochemical Detection is carried out in different depth separately through hawser suspension method, make multi-channel measurement electrode system therein
Sudden and violent leakage is in the corrosive environment of deep-sea；
3) required operating voltage is provided for system using self-contained power module, singlechip microcontroller controls number
Word analog converter generates pumping signal, selects the one in multi-channel measurement electrode system to carry out by channel selecting relay
Excitation, according to the type of pumping signal, is divided into following several operating modes for electrochemical in-situ test device:
A, when not output drive signal, current potential of the working electrode relative to reference electrode, as open circuit potential value are measured；
B, when exporting direct current wave excitation signal, then what is obtained is constant potential polarization result；
C, when exporting sine wave exciting signal, then what is obtained is ac impedance spectroscopy；
D, when exporting triangular wave pumping signal, then what is obtained is cyclic voltammetry curve；
Amplifier scaling circuit and filtering/compensation circuit ensure the high-precision and low phase misalignment of electrochemical measurement data
It adjusts, according to the characteristic of tested systems, adaptively selected current range obtains optimal measurement result；Timer clock is as system
The guarantee of reliability, periodically to system carry out forced resetting, device in place after, measuring system can be by preset time and frequency
Electrochemical measurement is automatically begun to, after being each measured, system is automatically into suspend mode, until next timing instant is opened after
Begin new measurement；After measurement result is converted by analog-digital converter, automatically save in memory；It, will after device recycling
It stores the data thought highly of to export in computer, completes test.
Further, the power module includes battery pack and integrated switching tube DC-DC converter, and battery pack is through prime collection
At switching tube DC-DC converter, operating voltage is provided for system, and design has reverse protection and overpressure protection.
Further, the dispensing depth for the device that step 1) is assembled is 100 ~ 3000 meters, can be in water according to test requirements document
Under lay 1 ~ 6 month time.
A kind of deep-sea multichannel corrosion electrochemistry in-situ test system of the invention and its test method, with prior art phase
It is than, generated beneficial effect,
Compared with prior art, the present invention its is simple and compact for structure；Scalability is high, can carry out simultaneously various metals or have
Electrochemical in-situ test under organic coating coating material deep-marine-environment；It is high pressure resistant, small in size, lay it is simple with reclaimer operation, can
In conjunction with deep sea installations in the form of with any other or carried；Low-power consumption, independent current source can be grown according to setpoint frequency
The data acquisition and storage in period works；By means of this invention, different materials deeply can be effectively studied in deep sea condition
Under corrosion mechanism, corrosion regularity and corrosion cause, for China deep-sea job facilities design, selection provide effectively according to
According to.
Detailed description of the invention
Fig. 1 is connection structure schematic illustration of the invention.
In figure, 1, multi-channel measurement electrode system, 2, amplifier scaling circuit and filtering/compensation circuit, 3, simulation number
Word converter, 4, timer clock, 5, integrated switch pipe DC-DC converter, 6,12 V Li-ion batteries piles, 7, pressure hull, 8,
Singlechip microcontroller, 9, SD card data storage, 10, digital analog converter, 11, channel selecting relay, 12, top cover.
Specific embodiment
A kind of 1 pair of deep-sea multichannel corrosion electrochemistry in-situ test system of the invention and its test side with reference to the accompanying drawing
Method is described in detail below.
Embodiment:
As shown in Fig. 1, a kind of deep-sea multichannel corrosion electrochemistry in-situ test system of the invention, main structure master
It to include pressure hull 7 and top cover 12, pressure hull 7 and top cover 12 form the closed test space, and inside it in space
Multi-channel measurement electrode system 1, amplifier scaling circuit and filtering/compensation circuit 2, analog-digital converter (ADC) are installed
3, timer clock 4, integrated switch pipe DC-DC converter 5,12 V Li-ion batteries piles 6, singlechip microcontroller (MCU) 8, SD
Card data storage 9, digital analog converter (DAC) 10 and channel selecting relay 11.
Wherein, 12 V Li-ion batteries piles 6 pass through prime integrated switch pipe DC-DC converter 5 and singlechip microcontroller 8
It is connected, provides 3.3 V operating voltages for whole system.Singlechip microcontroller 8 handles chip using STM32.Timer clock 4 with
Singlechip microcontroller 8 is connected, and as the guarantee of system reliability, provides correct time for system and carries out forced resetting.System
After the relevant parameter and measurement result of system are converted by analog-digital converter 3, using binary channels synchronous high-speed data acquisition side
Formula is automatically saved in SD card data storage 9.After device recycling, RS485 line is turned by USB and connects 7 inside number of pressure hull
According to communication interface and host computer, data are exported, complete whole process.There are four the above Measurement channel, digital simulations for device tool
Converter 10 is connected to the output end of single-chip microcontroller micro controller 8, for generating sine wave signal (corresponding AC impedance), triangular wave letter
Number corresponding CV measurement), straight wave signal (corresponding constant potential polarization) system to be measured is motivated, when not output drive signal
When, measure current potential of the WE relative to RE, as open circuit potential value OCP, while by 24 precision analog digital quantizers 3 and monolithic
Machine microcontroller 8 interconnects, and is acquired to signal, is calculated, handled and is stored in incoming single-chip microcontroller micro controller 8.
Apparatus of the present invention use wide input range DC-DC power source, and prime designs reverse protection and overpressure protection；Institute is functional
Element is powered using 3.3 V single supplies, and buck converter selects integrated switching tube DC-DC chip, has 200 mA output, 60 V
Wide input range, efficiency are up to 90%, can also keep stablizing output in OCL output capacitance-less；Circuit is managed in conjunction with precision voltage source
With low-power consumption analogue and digital circuit, power consumption is reduced, long term monitoring function may be implemented.
Timer clock 4 built in apparatus of the present invention, safeguards system reliability, in particular to timing force to system multiple
Position, device in place after, measuring system can automatically begin to electrochemical measurement by preset time and frequency, each be measured
Afterwards, system is automatically into suspend mode, until next timing instant starts new measurement after.Relay is selected by inner passage
Device 11 controls, and realizes time-controlled four-way cyclic corrosion electrochemical measurement.
Related multi-channel measurement electrode system 1 is set in pressure hull 7, and is stretched out by top cover 12 comprising four
The corrosion monitoring component of a more parallel connection, forms four or more Measurement channels.
After related amplifier scaling circuit and filtering/compensation circuit 2 are connected to multi-channel measurement electrode system 1
End, the front end of analog-digital converter 3, for ensure electrochemical measurement data high-precision and low phase detuning, according to tested
The characteristic of system, adaptively selected current range obtain optimal measurement result.Channel selecting relay 11 is connected to digital mould
The rear end of quasi- converter 10, the front end of multi-channel measurement electrode system 1, for selecting multi-channel measurement electrode system 1 side
Formula carries out on-off.
The pressure hull 7 of apparatus of the present invention uses pressure resistance to manufacture for the Titanium Alloy Design of 30 MPa, the size of pressure hull 7
It is designed as 125 mm of internal diameter φ according to the size of measuring system, the cylindrical shape of 5 mm of wall thickness is high using 1 " hickey of NPT
Means of press seals design ensures that device can 120 DEG C of 30 MPa, heatproof > of pressure resistance > (ocean floor heated fluid stream).On top cover 12 installation there are four with
On φ 25 mm, long 50mm cylindrical corrosion monitoring component comprising resistance probe of the sudden and violent leakage in the corrosive environment of deep-sea and
Three electrode probes.Resistance probe includes sensing element and sensing element, and connection type is existing common knowledge, no longer superfluous herein
It states.Three electrode probes include working electrode, reference electrode and to electrode, and working electrode selects metal or organic coating coating to be measured
Material, reference electrode Ag/AgCl are Pt to electrode.Three electrode probes and resistance probe sensing element etc. are all made of
PEEK fire resistant special type material injection molding.Sealing ring between corrosion monitoring component and top cover 12 uses fluoroplastics sealing material,
Prevent liquid from penetrating into inside pressure hull 7.
When implementation of the invention carries out deep-sea dispensing, it can be fixed on deep-sea test device and carry test for a long time, or is logical
The mode for crossing hawser suspention carries out quickly electrochemical monitoring in real time in different depth, easy to operate.The present embodiment design has four
12 V Li-ion batteries piles 6 of channel probe, scalability is high, can increase probe quantity according to actual needs, working principle is not sent out
Changing；Its precision voltage source management circuit and analogue and digital circuit are all made of low power dissipation design, and 1 ~ 6 month original may be implemented
Position electro-chemical test work.
The deep-sea multichannel corrosion electrochemistry home position testing method of the present embodiment, includes the following steps:
1) utilize oil reservoir logging high pressure sealing technology, by multi-channel measurement electrode system 1, amplifier scaling circuit with
Filtering/compensation circuit 2, analog-digital converter 3, timer clock 4, integrated switch pipe DC-DC converter 5,12 V lithium-ion electrics
Pond group 6, singlechip microcontroller 8, SD card data storage 9, digital analog converter 10 and channel selecting relay 11 seal
In the test space composed by pressure hull 7 and top cover 12, assembling is prepared into deep-sea multichannel corrosion electrochemistry in-situ test
Device；
2) carry out deep-sea dispensing: the device that step 1) is assembled is fixed on deep-sea test device carries test for a long time,
Or real-time Electrochemical Detection is carried out in different depth separately through hawser suspension method, make multi-channel measurement electrode system therein
In the corrosive environment of deep-sea, launching depth is 100 ~ 3000 meters for 1 sudden and violent leakage, can be laid under water 1 ~ 6 month according to test requirements document
Time；
3) 12 V Li-ion batteries piles 6 provide operating voltage through prime integrated switch pipe DC-DC converter 5 for system, and
Design has reverse protection and overpressure protection, and singlechip microcontroller 8 controls digital analog converter 10 and generates pumping signal, passes through
Channel selecting relay 11 selects the one in multi-channel measurement electrode system 1 to be motivated, will according to the type of pumping signal
Electrochemical in-situ test device is divided into following several operating modes:
A, when not output drive signal, current potential of the working electrode relative to reference electrode, as open circuit potential value are measured；
B, when exporting direct current wave excitation signal, then what is obtained is constant potential polarization result；
C, when exporting sine wave exciting signal, then what is obtained is ac impedance spectroscopy；
D, when exporting triangular wave pumping signal, then what is obtained is cyclic voltammetry curve；
Amplifier scaling circuit and filtering/compensation circuit 2 ensure the high-precision and low phase misalignment of electrochemical measurement data
It adjusts, according to the characteristic of tested systems, adaptively selected current range；Guarantee of the timer clock 4 as system reliability, timing are right
System carry out forced resetting, device in place after, measuring system can automatically begin to electrochemical measurement by preset time and frequency,
After being each measured, system is automatically into suspend mode, until next timing instant starts new measurement after；Measurement result
After being converted by analog-digital converter 2, automatically save in SD card data storage 9；After device recycling, SD card data are deposited
Data in reservoir 9 export in computer, complete test.
Its processing and fabricating of a kind of deep-sea multichannel corrosion electrochemistry in-situ test system of the invention is very simple and convenient, presses
Processing and fabricating shown in Figure of description.
Claims (9)
1. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system, which is characterized in that its main structure includes pressure hull
And top cover, pressure hull and top cover form the closed test space, and install multi-channel measurement electrode body in space inside it
System, amplifier scaling circuit and filtering/compensation circuit, analog-digital converter, timer clock, power module, single-chip microcontroller are micro-
Controller, memory, digital analog converter and channel selecting relay, wherein
The power module is connected with singlechip microcontroller, and required operating voltage is provided for system；
The multi-channel measurement electrode system is set in pressure hull, and stretched out by top cover comprising multiple to be connected in parallel
Corrosion monitoring component；
The amplifier scaling circuit and filtering/compensation circuit are connected to the rear end of multi-channel measurement electrode system, simulate number
The front end of word converter is used for adaptively selected range, realizes the range switching during system electrochemical measurement；
The analog-digital converter and singlechip microcontroller interconnect, and for being acquired to signal, are passed to single-chip microcontroller micro-control
It calculated, handled and is stored in device；
The timer clock is connected with singlechip microcontroller, provides correct time for system and carries out forced resetting, system
Relevant parameter and measurement result are stored in memory, and are communicated through communication interface and host computer；
The digital analog converter is connected to the output end of single-chip microcontroller micro controller, for generating a variety of pumping signals to body to be measured
System is motivated, and according to the type of pumping signal, carries out electrochemical in-situ test；
The channel selecting relay is connected to the rear end of digital analog converter, and the front end of multi-channel measurement electrode system is used
In carrying out on-off in a manner of selecting one to multi-channel measurement electrode system.
2. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1, which is characterized in that described
Corrosion monitoring component includes resistance probe and three electrode probes of the sudden and violent leakage in the corrosive environment of deep-sea, and three electrode probes include work
Electrode, reference electrode and to electrode, working electrode selects metal or organic coating coating material to be measured.
3. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1 or 2, which is characterized in that
Sealing ring between the corrosion monitoring component and top cover uses fluoroplastics sealing material.
4. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1 or 2, which is characterized in that
The power module includes battery pack and electric pressure converter, and battery pack provides operating voltage through electric pressure converter, for system, or
Directly operating voltage is provided for system by battery pack.
5. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1 or 2, which is characterized in that
The size of the pressure hull is designed as cylindrical shape according to the size of measuring system.
6. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1 or 2, which is characterized in that
Using the close silk helixseal connection of rubber o-ring between the pressure hull and top cover.
7. a kind of deep-sea multichannel corrosion electrochemistry in-situ test system according to claim 1 or 2, which is characterized in that
The singlechip microcontroller handles chip using STM32.
8. a kind of deep-sea multichannel corrosion electrochemistry home position testing method, which comprises the steps of:
1) utilize oil reservoir logging high pressure sealing technology, by multi-channel measurement electrode system, amplifier scaling circuit and filtering/
Compensation circuit, analog-digital converter, timer clock, power module, singlechip microcontroller, memory, digital-to-analogue conversion
Device and channel selecting relay are sealed in the test space composed by pressure hull and top cover, and assembling is prepared into claim 1
Or a kind of deep-sea multichannel corrosion electrochemistry in-situ test system described in 2 or 3；
2) carry out deep-sea dispensing: the device that step 1) is assembled is fixed on deep-sea test device and carries test for a long time, or single
Real-time Electrochemical Detection is solely carried out in different depth by hawser suspension method, leaks multi-channel measurement electrode system therein cruelly
In the corrosive environment of deep-sea；
3) required operating voltage is provided for system using self-contained power module, singlechip microcontroller controls digital mould
Quasi- converter generates pumping signal, selects the one in multi-channel measurement electrode system to be swashed by channel selecting relay
It encourages, according to the type of pumping signal, electrochemical in-situ test device is divided into following several operating modes:
A, when not output drive signal, current potential of the working electrode relative to reference electrode, as open circuit potential value are measured；
B, when exporting direct current wave excitation signal, then what is obtained is constant potential polarization result；
C, when exporting sine wave exciting signal, then what is obtained is ac impedance spectroscopy；
D, when exporting triangular wave pumping signal, then what is obtained is cyclic voltammetry curve；
Amplifier scaling circuit and filtering/compensation circuit ensure the high-precision and low phase detuning, root of electrochemical measurement data
According to the characteristic of tested systems, adaptively selected current range；Guarantee of the timer clock as system reliability, periodically to system into
Row forced resetting, device in place after, measuring system can be automatically begun to electrochemical measurement, each survey by preset time and frequency
After the completion of amount, system is automatically into suspend mode, until next timing instant starts new measurement after；Measurement result passes through mould
After quasi- digital quantizer conversion, automatically save in memory；After device recycling, the data in memory are exported into computer
In, complete test.
9. a kind of deep-sea multichannel corrosion electrochemistry home position testing method according to claim 8, which is characterized in that described
Power module includes battery pack and integrated switching tube DC-DC converter, battery pack through prime integrated switch pipe DC-DC converter,
Operating voltage is provided for system, and design has reverse protection and overpressure protection.
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