CN107462616A - Suitable for the sensor of nuclear power high ambient temperature water under high pressure environment electrochemistry noise measurement - Google Patents
Suitable for the sensor of nuclear power high ambient temperature water under high pressure environment electrochemistry noise measurement Download PDFInfo
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- CN107462616A CN107462616A CN201710571385.0A CN201710571385A CN107462616A CN 107462616 A CN107462616 A CN 107462616A CN 201710571385 A CN201710571385 A CN 201710571385A CN 107462616 A CN107462616 A CN 107462616A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The present invention relates to a kind of sensor suitable for the measurement of nuclear power high ambient temperature water under high pressure environment electrochemistry noise, including high-purity antimony electrode as reference electrode, the stainless steel and Stainless Steel Shell that have as the surface spraying to electrode ZrO2+Y2O3；The porcelain tube with diplopore is further fixed in stainless steel case body, two electrodes are separately fixed in porcelain tube, and front end is stretched out from porcelain tube front end, and the copper conductor that two electrode rear ends are drawn passes from the diplopore of porcelain tube rear end, and is sealed by ceramic powder sealant；The copper conductor drawn to rear end on electrode and reference electrode is penetrated in porcelain tube, so as to ensure the electric insulation of copper conductor and main body Stainless Steel Shell and thermal insulation.
Description
Technical field
The present invention relates to a kind of sensor suitable for the measurement of nuclear power high ambient temperature water under high pressure environment electrochemistry noise, belong to
Field of non destructive testing.
Background technology
Due to the electrochemical nature that metal material corrodes in nuclear power environment, electrochemical techniques are to characterize nuclear material corrosion
The effective means of damage.Electrochemistry noise (EN) is a kind of lossless glitch-free detection method in situ, and it can supervise detection online
The homogeneous corrosion and local corrosion of material, and the remote monitoring of material corrosion type and corrosion strength can be realized.With
Science and technology particularly electronic technology and Modern Mathematical Methods are (such as：Wavelet theory) fast development, nondestructively prison detection in situ
The electrochemical noise technique of material corrosion process is developed in recent years.Study both at home and abroad and mainly used three-electrode system
Electro-chemical test is carried out in high temperature and high pressure kettle, material is characterized by the time domains such as noise resistance, spectral noise resistance and frequency domain parameter
The corrosion behavior of material and media chemistry composition, the changing rule of experimental period, and then using in current potential noise and current noise spectrum
Temporal variations feature detection local corrosion (such as：Crack initiation and propagation) process.Experiment shows prolonged electrochemistry noise
Test is that the effective ways for monitoring stainless steel stress-corrosion cracking provide experimental basis for the on-line checking of nuclear material.But
Scene prison detection needs to develop corresponding sensor, and there is not been reported for research in this respect.Patent design of the present invention is a kind of
Suitable for the sensor of nuclear power high ambient temperature water under high pressure environment electrochemistry noise measurement, can be achieved to metallic material corrosion degree
Judge.
The content of the invention
It is an object of the invention to overcome vacancy of the prior art, there is provided one kind is applied to nuclear power high ambient temperature water under high pressure
The sensor of Environmental electrochemistry noise testing.In order to solve the above-mentioned technical problem, the present invention is to be achieved through the following technical solutions
's：
A kind of sensor suitable for the measurement of nuclear power high ambient temperature water under high pressure environment electrochemistry noise, including as reference electricity
High-purity antimony electrode of pole, to have as the surface spraying to electrode be 90-94%ZrO in mass ratio2：6-10%Y2O3Stainless steel
And Stainless Steel Shell, the porcelain tube with diplopore is further fixed in stainless steel case body, two electrodes are separately fixed in porcelain tube, preceding
End is stretched out from porcelain tube front end, and the copper conductor that two electrode rear ends are drawn passes from the diplopore of porcelain tube rear end, and close by ceramic powder
Envelope agent is sealed；The copper conductor drawn to rear end on electrode and reference electrode is penetrated in porcelain tube, so as to ensure copper conductor and master
The electric insulation of body Stainless Steel Shell and thermal insulation.
Preferably, 50 μm are not less than to electrode spray-on coating thickness.Stainless Steel Shell is 316L Stainless Steel Shells.
Brief description of the drawings
The sensor schematic for being applied to the measurement of nuclear power high ambient temperature water under high pressure environment electrochemistry noise of Fig. 1 inventions.
Description of reference numerals is as follows：1 reference electrode；2 pairs of electrodes；3 fluid sealants；4 oval diplopore porcelain tubes；5 316L are stainless
Steel tube body；6 electrode extraction wires
Fig. 2 be current potential after DC component is picked out under different test conditions, (left side one is classified as current potential and made an uproar current noise Time Domain Spectrum
Sound Time Domain Spectrum, the right side one are classified as current noise Time Domain Spectrum) (test condition a-b：105 DEG C, 0.6MPa；c-d：160 DEG C, 7MPa；
e-f：190 DEG C, 9MPa；g-h：220 DEG C, 10.5MPa；i-j：250 DEG C, 16MPa；k-l：293 DEG C, 19MPa).
Fig. 3 is the spectral noise resistance under the various test conditions being calculated.
Embodiment
The reference electrode that the present invention uses is diameter 3mm high-purity antimony electrode, its current potential in HTHP water environment
It is stable.To the ZrO that electrode is plasma spraying 92%2+ 8%Y2O3A diameter of 3mm of (mass ratio) 304NG stainless steels
Electrode.Spray ZrO2+ 8%Y2O3Purpose be in order to reduce the exposed area of 304NG stainless steels, reached reduction to work electricity
The purpose of pole polarization.The coating layer thickness of spraying is about 50 μm, and coating is stable in HTHP water environment, can meet that test will
Ask.The high-temperature high pressure water electrochemistry noise detection sensor detection operating temperature range of making is about 160 DEG C~310 DEG C, pressure
Scope is 6Mpa~15Mpa.Two electrodes load 316L stainless steel tubes, and (internal diameter 10mm, external diameter 12mm, length are
400mm), and from Cotronics companies of the U.S. Duropot809 series ceramic powder sealants developed are sealed, and are only exposed
Reference electrode and the front end to electrode.The copper conductor drawn to the other end on electrode and reference electrode penetrates oval diplopore porcelain tube
In, so as to ensure the electric insulation of copper conductor and main body stainless steel tube and thermal insulation, finally load in 316L stainless steel tubes.
Installation and application method are as follows：
Step 1：Making a diameter of 3mm high-purity antimony electrode, one end is polished bright with sand paper, and the other end is burn-on copper conductor,
It is standby；
Step 2：Using surface spraying one of the plasma spraying method in a diameter of 3mm 304NG stainless steel electrodes one end
Layer ZrO2+ 8%Y2O3Coating, the other end are burn-on copper cash, standby；
Step 3：By above-mentioned two electrode load oval diplopore porcelain tube carry out electric insulation with it is heat-insulated, it is stainless to be reloaded into 316L
Steel pipe；
Step 4：The Duropot809 series ceramic powder sealants developed from Cotronics companies of the U.S. are sealed；
Step 5：Sensor is placed in progress electrochemistry noise test in autoclave.
Step 6：The electrochemical characteristic parameter such as noise resistance and spectral noise resistance is calculated, (spectrum) noise resistance is smaller, shows
Corrosion rate is bigger.
Illustrated below by way of specific test case：
The electrochemical sensor developed is placed in autoclave, contact conductor draw kettle outside, working electrode be 304NG not
Become rusty steel.Reference electrode is connected with working electrode with electrochemical workstation, carries out the test of corrosion potential.Solution is used in experiment
Distilled water.
Fig. 2 is the electrochemistry noise test result under different temperatures and pressure.Under different temperatures pressure condition, current potential, electricity
For flow noise signal all integrated distributions near zero, the change of current potential noise signal amplitude is little, in the range of 3mV, A and B bars
Under part, the fluctuation of current potential noise signal is bigger, and this may be with the ruptures of 304NG stainless steel specimen surface passivating films and being passivated again
Close, tended towards stability with the elevated potential noise change of temperature, pressure, and fluctuation amplitude is held in the range of 1mV, is said
The state of bright now specimen surface film has been tended towards stability, it is notable that under the conditions of F (293 DEG C, 19MPa), current potential is made an uproar
The variation characteristic that acoustical signal and current noise signal rapid increase all occur and then slowly declined, because 304NG stainless steels try
Sample typically exhibits the form of homogeneous corrosion in HTHP water environment, so this noise variation characteristic is likely to control with activation
Corrosion processed is associated, and in this corrosion process, cathode reaction speed is determined by liberation of hydrogen process.Electric current is made an uproar under different test conditions
Acoustical signal amplitude changes also very little, is substantially at 1 μ A × cm-2In the range of.The method of applied statistics analysis can be simple and fast
The parsing noise data of speed, be classified as under different temperatures, pressure condition in table 1, current potential, current noise signal standard deviation and
The noise resistance being calculated, in table under different test conditions it can be seen from the variation tendency of noise resistance with temperature pressure
Certain downward trend is integrally presented in the increase noise resistance of power, but its change is little, maintains essentially in the model of an order of magnitude
In enclosing, noise resistance when minimum is also in 2000 Ω × cm2More than, it follows that working electrode sample under different test conditions
Corrosion stable, electrode are in the homogeneous corrosion state of activation control.
(A under the different temperatures of table 1, pressure condition：105 DEG C, 0.6MPa；B：160 DEG C, 7MPa；C：190 DEG C, 9MPa；D：
220 DEG C, 10.5MPa；E：250 DEG C, 16MPa；F：293 DEG C, 19MPa) electrochemistry noise detection related resolution parameter value
Electrochemical noise signal is transformed into by Time Domain Spectrum by frequency domain spectra by fast Fourier transform, obtained by correlation computations
Spectral noise resistance view under to different test conditions is as shown in Figure 3.R under each test condition0snBy taking near 0.001Hz
Five points average and obtain, as table 1 last row shown in.
Claims (3)
1. a kind of sensor suitable for the measurement of nuclear power high ambient temperature water under high pressure environment electrochemistry noise, including as reference electrode
High-purity antimony electrode, to have as the surface spraying to electrode be 90-94%ZrO in mass ratio2：6-10%Y2O3Stainless steel and
Stainless Steel Shell.The porcelain tube with diplopore is further fixed in stainless steel case body, two electrodes are separately fixed in porcelain tube, front end
Stretched out from porcelain tube front end, the copper conductor that two electrode rear ends are drawn passes from the diplopore of porcelain tube rear end, and is sealed by ceramic powder
Agent is sealed；The copper conductor drawn to rear end on electrode and reference electrode is penetrated in porcelain tube, so as to ensure copper conductor and main body
The electric insulation of Stainless Steel Shell and thermal insulation.
2. sensor according to claim 1, it is characterised in that 50 μm are not less than to electrode spray-on coating thickness.
3. sensor according to claim 1, it is characterised in that Stainless Steel Shell is 316L Stainless Steel Shells.
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| CN201710571385.0A CN107462616A (en) | 2017-07-13 | 2017-07-13 | Suitable for the sensor of nuclear power high ambient temperature water under high pressure environment electrochemistry noise measurement |
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| CN201710571385.0A CN107462616A (en) | 2017-07-13 | 2017-07-13 | Suitable for the sensor of nuclear power high ambient temperature water under high pressure environment electrochemistry noise measurement |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11428623B2 (en) * | 2019-12-20 | 2022-08-30 | West Virginia University Board of Governors on behalf of West Virginia University | High temperature corrosion sensor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4153521A (en) * | 1977-08-05 | 1979-05-08 | Litvak Rafael S | Method of automatic control and optimization of electrodeposition conditions |
| CN105424590A (en) * | 2015-12-07 | 2016-03-23 | 天津大学 | Sensor and detection method for atmosphere corrosion detection of steel member or test piece |
| CN106018520A (en) * | 2016-07-22 | 2016-10-12 | 天津大学 | Electrode system for electrochemical measurement in high-temperature high-pressure water environment and application of electrode system |
| CN205844249U (en) * | 2016-07-22 | 2016-12-28 | 天津大学 | A kind of electrode system of electrochemical measurement in High Temperature High Pressure water environment |
-
2017
- 2017-07-13 CN CN201710571385.0A patent/CN107462616A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4153521A (en) * | 1977-08-05 | 1979-05-08 | Litvak Rafael S | Method of automatic control and optimization of electrodeposition conditions |
| CN105424590A (en) * | 2015-12-07 | 2016-03-23 | 天津大学 | Sensor and detection method for atmosphere corrosion detection of steel member or test piece |
| CN106018520A (en) * | 2016-07-22 | 2016-10-12 | 天津大学 | Electrode system for electrochemical measurement in high-temperature high-pressure water environment and application of electrode system |
| CN205844249U (en) * | 2016-07-22 | 2016-12-28 | 天津大学 | A kind of electrode system of electrochemical measurement in High Temperature High Pressure water environment |
Non-Patent Citations (2)
| Title |
|---|
| 宋诗哲 等: "《电化学噪声技术检测核电环境材料的腐蚀损伤》", 《中国材料进展》 * |
| 石江波: "《压水堆核电站关键材料的在线腐蚀监检测》", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11428623B2 (en) * | 2019-12-20 | 2022-08-30 | West Virginia University Board of Governors on behalf of West Virginia University | High temperature corrosion sensor |
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Address after: 300350 District, Jinnan District, Tianjin Haihe Education Park, 135 beautiful road, Beiyang campus of Tianjin University Applicant after: Tianjin University Address before: 300072 Tianjin City, Nankai District Wei Jin Road No. 92 Applicant before: Tianjin University |
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Application publication date: 20171212 |