CN104614310B - A kind of high temperature pressure corrosion electro-chemical measuring apparatus and measuring method - Google Patents
A kind of high temperature pressure corrosion electro-chemical measuring apparatus and measuring method Download PDFInfo
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- CN104614310B CN104614310B CN201510044673.1A CN201510044673A CN104614310B CN 104614310 B CN104614310 B CN 104614310B CN 201510044673 A CN201510044673 A CN 201510044673A CN 104614310 B CN104614310 B CN 104614310B
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Abstract
A kind of high temperature pressure corrosion electro-chemical measuring apparatus and measuring method, the measurement apparatus include autoclave heating mantle, be inserted in the autoclave body in autoclave heating mantle, the autoclave end cap on autoclave body is fixed on by autoclave fastening bolt；The autoclave end cap is provided with air inlet, exhaust outlet, pressure gauge socket and thermometric blind pipe socket, is also provided with the screw of reference electrode, working electrode and auxiliary electrode insertion；The gas outlet stop valve for being provided with the air inlet stop valve for opening and closing air inlet, the blast pipe of exhaust outlet and opening and closing outlet is provided with the air inlet pipe of air inlet；The invention also discloses the measuring method of the device；The measurement apparatus is reliable and is easily achieved, and solves the problem of expensive high temperature pressure corrosion electrochemical measuring electrode, difficult making and difficult elevated-temperature seal；Apparatus of the present invention make simple, good airproof performance, can meet the measurement of corrosion electrochemistry in high temperature, hyperbaric environment.
Description
Technical field
The invention belongs to high temperature pressure corrosion electrochemical measuring technology field, and in particular to a kind of high temperature pressure corrosion electrification
Learn measurement apparatus and measuring method.
Background technology
It is dense due to corrosive impurity in the high-temperature high pressure water media environment of station boiler and nuclear steam generator
Contracting, the corrosion of heat exchange pipeline is commonplace.Electrochemical measuring technology evaluates the important of material corrosion resistance, corrosion behavior and mechanism
Means.But relative to normal temperature and pressure system, under high-temperature and high-pressure conditions there is larger difficulty in electrochemical measurement, mainly due to not
The sealing of measurement signal transfer wire and high temperature high pressure device is easily realized simultaneously.At present, domestic related research institutes, generally
The measuring electrode provided using CORTEST companies of the U.S. or Dong Shen companies of Japan carries out high temperature pressure corrosion electrochemical research, electricity
The price of pole is also costly.Metal Inst., Chinese Academy of Sciences has been obtained for the related skill of high-temperature and high pressure electrochemistry electrode fabrication
The patent of art, but manufacture craft is relative complex, and in the market has no related commercially produced product.Due to high temperature pressure corrosion electrochemistry
There is difficulty in the acquisition of measuring electrode, corrosion behavior, the study mechanism of material in HTHP water environment are influenceed to a certain extent.
The content of the invention
In order to solve the problem of above-mentioned prior art is present, it is an object of the invention to provide a kind of high temperature pressure corrosion electricity
Chemical measurement device and measuring method, the measurement apparatus is reliable and is easily achieved, and solves high temperature pressure corrosion electrochemical measurement
The problem of electrode is expensive, making is difficult and elevated-temperature seal is difficult；Apparatus of the present invention make simple, good airproof performance, can meet
The measurement of corrosion electrochemistry in high temperature, hyperbaric environment.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of high temperature pressure corrosion electro-chemical measuring apparatus, including autoclave heating mantle 1, are inserted in autoclave heating mantle 1
Autoclave body 2, the autoclave end cap 4 on autoclave body 2 is fixed on by autoclave fastening bolt 3；The autoclave end cap 4
Air inlet 5, exhaust outlet 10, the socket of pressure gauge 6 and the socket of thermometric blind pipe 11 are provided with, reference electrode 7, working electrode 8 is also provided with
The screw inserted with auxiliary electrode 9；The air inlet stop valve for opening and closing air inlet is provided with the air inlet pipe of the air inlet 5
The gas outlet stop valve K2 for opening and closing outlet is provided with K1, the blast pipe of exhaust outlet 10；The reference electrode 7 and auxiliary
The structure of electrode 9 is identical, including wire column 15, is socketed in the glass tube 13 outside the upper end of wire column 15, is welded on wire column 15
Electrode low head 14 that is outside and being welded on the lower end of glass tube 13, is welded on the electrode external thread sleeve 12 outside the upper end of glass tube 13,
The bottom of wire column 15 is welded with platinized platinum 16 by wire 18, and the material of wire 18 is identical with the material of platinized platinum 16, reference electricity
Pole 7 and auxiliary electrode 9 are connected by electrode external thread sleeve 12 with the screw on autoclave end cap 4；The structure of the working electrode 8 is removed
The bottom of wire column 15 is welded with test electrode slice 17, and the material and test electrode slice 17 of wire 18 by wire 18
Material is identical outer, and other structures are with reference electrode 7 and auxiliary electrode 9, working electrode 8 also electrode external thread sleeve 12 and autoclave end cap
Screw connection on 4.
The material of the electrode external thread sleeve 12, electrode low head 14 and wire column 15 is close with glass tube thermal coefficient of expansion
Kovar alloy, it is ensured that soldering can be carried out between glass tube 13 and electrode external thread sleeve 12, electrode low head 14, is realized
Sealing, meets high temperature and high pressure environment use requirement.
The measuring method of high temperature pressure corrosion electro-chemical measuring apparatus described above, first, survey is processed into by test material
Electrode slice 17 is tried, is connected by wire 18 with the wire column 15 of the lower end of working electrode 8；Then by reference electrode 7, working electrode
8th, the electrode external thread sleeve 12 of auxiliary electrode 9 is attached with the screw being reserved on autoclave end cap 4；Then test solution is fallen
Enter in autoclave body 2, the liquid level of test solution will be controlled under the tie point of wire column 15 and wire electrode 18, it is to avoid wire column
15 or wire column 15 contacted with the tie point of wire electrode 18 with test fluid；Autoclave fastening bolt (3) is then used by autoclave
End cap 4 is sealed with autoclave body 2；If desired for deoxygenation, air inlet valve K1 and gas outlet valve K2 is closed, passes through air inlet
5th, exhaust outlet 10 carries out deoxygenation operation to system；Then autoclave body 2 is heated, when medium temperature reaches in autoclave body 2
To after setting value, wire column 15 and the electrochemical workstation of reference electrode 7, working electrode 8, auxiliary electrode 9 are attached, entered
Row electro-chemical test.
The present invention is compared to the prior art compared with having the following advantages that：
1) manufacture craft of electrode is simple, and high pressure etching apparatus is installed, makes simple.
2) reliability of glass tube and kovar alloy is high, test system good seal performance, 400 DEG C of highest heatproof, and highest is resistance to
Press 20MPa.
3) electrode uses sleeve type structure, and the use of glass tube realizes the insulation of wire column and kettle.
Brief description of the drawings
Fig. 1 is measurement apparatus structural representation of the present invention.
Fig. 2 is the structural representation of reference electrode, working electrode and auxiliary electrode.
Embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
As shown in figure 1, a kind of high temperature pressure corrosion electro-chemical measuring apparatus of the invention, including autoclave heating mantle 1, it is inserted in
Autoclave body 2 in autoclave heating mantle 1, the autoclave end cap 4 on autoclave body 2 is fixed on by autoclave fastening bolt 3；
The autoclave end cap 4 is provided with air inlet 5, exhaust outlet 10, the socket of pressure gauge 6 and the socket of thermometric blind pipe 11, is also provided with reference
The screw that electrode 7, working electrode 8 and auxiliary electrode 9 are inserted；Be provided with the air inlet pipe of the air inlet 5 open and close into
The gas outlet stop valve K2 for opening and closing outlet is provided with the air inlet stop valve K1 of gas, the blast pipe of exhaust outlet 10.
As shown in Fig. 2 the reference electrode 7 is identical with the structure of auxiliary electrode 9, including wire column 15, it is socketed in wire
Glass tube 13 outside the upper end of post 15, is welded on the outside of wire column 15 and is welded on the electrode low head 14 of the lower end of glass tube 13,
The electrode external thread sleeve 12 outside the upper end of glass tube 13 is welded on, the bottom of wire column 15 is welded with platinized platinum 16 by wire 18, led
The material of filament 18 is identical with the material of platinized platinum 16, and reference electrode 7 and auxiliary electrode 9 pass through electrode external thread sleeve 12 and autoclave end
Screw connection on lid 4；The structure of the working electrode 8 by wire 18 is welded with test electrode except the bottom of wire column 15
Piece 17, and the material of wire 18 is identical with the material for testing electrode slice 17 outer, other structures are with reference electrode 7 and auxiliary electrode
9, also electrode external thread sleeve 12 is connected working electrode 8 with the screw on autoclave end cap 4.
It is used as the preferred embodiment of the present invention, the material of the electrode external thread sleeve 12, electrode low head 14 and wire column 15
Matter is the kovar alloy close with glass tube thermal coefficient of expansion, it is ensured that glass tube 13 and electrode external thread sleeve 12, electrode low head
Soldering can be carried out between 14, sealing is realized, high temperature and high pressure environment use requirement is met.
As shown in figure 1, the measuring method of high temperature pressure corrosion electro-chemical measuring apparatus of the present invention, first, by test material
Test electrode slice 17 is processed into, is connected by wire 18 with the wire column 15 of the lower end of working electrode 8；Then by reference electrode 7,
Working electrode 8, the electrode external thread sleeve 12 of auxiliary electrode 9 are attached with the screw being reserved on autoclave end cap 4；It will then survey
Examination solution is poured into autoclave body 2, and the liquid level of test solution will be controlled under the tie point of wire column 15 and wire electrode 18, kept away
Exempt from wire column 15 or wire column 15 is contacted with the tie point of wire electrode 18 with test fluid；Then using autoclave fastening bolt (3)
Autoclave end cap 4 is sealed with autoclave body 2；If desired for deoxygenation, air inlet valve K1 and gas outlet valve K2 is closed, is led to
Cross air inlet 5, exhaust outlet 10 and deoxygenation operation is carried out to system；Then autoclave body 2 is heated, as Jie in autoclave body 2
Matter temperature is reached after setting value, and wire column 15 and the electrochemical workstation of reference electrode 7, working electrode 8, auxiliary electrode 9 are entered
Row connection, carries out electro-chemical test, and method of testing is：Can using corrosion electrochemistry study in commonly use polarization curve test and
Electrochemical impedance is tested, and corrosion characteristics of the working electrode 8 in high-temperature high-pressure medium are studied.
Claims (2)
1. a kind of measuring method of high temperature pressure corrosion electro-chemical measuring apparatus, it is characterised in that：The measurement apparatus includes height
Kettle heating mantle (1) is pressed, the autoclave body (2) in autoclave heating mantle (1) is inserted in, is fixed on by autoclave fastening bolt (3)
Autoclave end cap (4) on autoclave body (2)；The autoclave end cap (4) is provided with air inlet (5), exhaust outlet (10), pressure gauge
(6) socket and thermometric blind pipe (11) socket, are also provided with reference electrode (7), working electrode (8) and auxiliary electrode (9) insertion
Screw；The air inlet stop valve (K1) for opening and closing air inlet, exhaust outlet (10) are provided with the air inlet pipe of the air inlet (5)
Blast pipe on be provided with open and close outlet gas outlet stop valve (K2)；The reference electrode (7) and auxiliary electrode (9)
Structure it is identical, including wire column (15) is socketed in the glass tube (13) outside wire column (15) upper end, is welded on wire column
(15) electrode low head (14) that is outside and being welded on glass tube (13) lower end, is welded on the electrode outside glass tube (13) upper end
External thread sleeve (12), wire column (15) bottom is welded with platinized platinum (16), the material and platinized platinum of wire (18) by wire (18)
(16) material is identical, and reference electrode (7) and auxiliary electrode (9) pass through on electrode external thread sleeve (12) and autoclave end cap (4)
Screw is connected；The structure of the working electrode (8) by wire (18) is welded with test electrode except wire column (15) bottom
Piece (17), and the material of wire (18) is identical with the material of test electrode slice (17) outer, the same reference electrode of other structures (7) and
Auxiliary electrode (9), working electrode (8) is connected also by electrode external thread sleeve (12) with the screw on autoclave end cap (4)；
The measuring method of the measurement apparatus is：First, test material is processed into test electrode slice (17), passes through wire
(18) wire column (15) with working electrode (8) lower end is connected；Then by reference electrode (7), working electrode (8), auxiliary electrode
(9) electrode external thread sleeve (12) is attached with the screw being reserved on autoclave end cap (4)；Test solution is then poured into height
Press in kettle (2), the liquid level of test solution will be controlled under wire column (15) and the tie point of wire (18), it is to avoid wire
Post (15) or wire column (15) are contacted with the tie point of wire (18) with test fluid；Then using autoclave fastening bolt (3)
Autoclave end cap (4) is sealed with autoclave body (2)；If desired for deoxygenation, air inlet stop valve (K1) and gas outlet are closed
Stop valve (K2), deoxygenation operation is carried out by air inlet (5), exhaust outlet (10) to system；Then autoclave body (2) is added
Heat, after autoclave body (2) interior medium temperature reaches setting value, by reference electrode (7), working electrode (8), auxiliary electrode (9)
Wire column (15) be attached with electrochemical workstation, carry out electro-chemical test.
2. measuring method according to claim 1, it is characterised in that：The electrode external thread sleeve (12), electrode low head
(14) and wire column (15) material be the kovar alloy close with glass tube thermal coefficient of expansion.
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| CN106468650A (en) * | 2015-08-21 | 2017-03-01 | 中国石油天然气股份有限公司 | Reaction kettle and corrosion test system |
| CN106644917B (en) * | 2016-08-22 | 2019-10-11 | 中国船舶重工集团公司第七二五研究所 | A kind of electrolytic cell device for simulated deep-sea environment electro-chemical test |
| CN108169117A (en) * | 2018-02-12 | 2018-06-15 | 华电电力科学研究院有限公司 | Electrochemical corrosion measurement device and its application method in a kind of four main tubes of boiler deoxygenation condition solution medium |
| CN108956446A (en) * | 2018-10-15 | 2018-12-07 | 浙江德威硬质合金制造有限公司 | The test method of hard alloy corrosion resistance |
| CN109269974A (en) * | 2018-11-20 | 2019-01-25 | 重庆市特种设备检测研究院 | A kind of test method of the online Electrochemical corrosion rate of boiler |
| CN109297897B (en) * | 2018-12-13 | 2023-08-18 | 福州大学 | Temperature and humidity controllable high-voltage electric field environment corrosion test device and method |
| CN109827898B (en) * | 2019-03-29 | 2021-09-17 | 河海大学 | Metal corrosion test device |
| CN110095405B (en) * | 2019-05-30 | 2024-03-26 | 华能山东石岛湾核电有限公司 | Sealing device for high-temperature high-pressure corrosion electrochemical working electrode and use method |
| CN114221047A (en) * | 2021-12-08 | 2022-03-22 | 北京工业大学 | High-voltage-resistant battery powder testing pool |
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| CN100419416C (en) * | 2005-03-21 | 2008-09-17 | 张荣华 | Zr/ZrO2 electrode and producing method thereof and integrated high temperature high-pressure chemical sensor composed by the same |
| CN1304834C (en) * | 2005-03-25 | 2007-03-14 | 北京科技大学 | Dynamic high-temperature and pressure electro-chemical measurement experimental device |
| CN101470093B (en) * | 2008-04-16 | 2012-07-04 | 中国科学院金属研究所 | Working electrode for implementing electro-chemical test of high-temperature high-pressure water solution system |
| CN101520402A (en) * | 2009-02-24 | 2009-09-02 | 上海大学 | Experimental facility for testing electrochemical signals of various materials in high-temperature high-pressure environment |
| CN101865816A (en) * | 2010-05-28 | 2010-10-20 | 北京科技大学 | Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing |
| CN101900664B (en) * | 2010-08-04 | 2012-09-19 | 南京工业大学 | Vapor-liquid two-phase flow accelerated corrosion test device |
| CN102944602B (en) * | 2012-11-05 | 2014-07-02 | 中国科学院金属研究所 | High-temperature high-pressure in-situ multichannel rapid scratch electrode system |
| CN203705392U (en) * | 2013-12-27 | 2014-07-09 | 西安建筑科技大学 | Electrochemical experiment device for high-temperature leaching of mineral |
| CN204439517U (en) * | 2015-01-28 | 2015-07-01 | 西安热工研究院有限公司 | A kind of high temperature pressure corrosion electro-chemical measuring apparatus |
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