CN102401781A - Reference electrode for reinforced concrete and manufacturing method of reference electrode - Google Patents
Reference electrode for reinforced concrete and manufacturing method of reference electrode Download PDFInfo
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- CN102401781A CN102401781A CN2011102966060A CN201110296606A CN102401781A CN 102401781 A CN102401781 A CN 102401781A CN 2011102966060 A CN2011102966060 A CN 2011102966060A CN 201110296606 A CN201110296606 A CN 201110296606A CN 102401781 A CN102401781 A CN 102401781A
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Abstract
The invention discloses a reference electrode for reinforced concrete, which is provided with a sleeve, wherein a gel electrolyte is filled in an inner cavity of the sleeve, an Ag/AgCl electrode provided with a copper cable in a connecting manner is inserted in the gel electrolyte, the sleeve is sealed by using an epoxy resin material at the first end of the sleeve, which is provided with the copper cable in a connecting manner, and the second end opposite to the first end is filled with microporous ceramic. The invention realizes linkage with the external electrolyte by adopting the microporous ceramic, and ensures ion transmission. The reference electrode provided by the invention has high electrode potential stability and long service life, has the advantages of small volume, high strength, simpleness in manufacture and the like, can be completely used in a concrete system, and realizes long-term electrochemical corrosion monitoring of reinforcing steel bars.
Description
Technical field
The present invention relates to reinforced concrete structures corrosion and guard technology field, long-acting, durable, the embedment type reference electrode for inspecting of particularly a kind of steel reinforced concrete erosion monitoring or detection usefulness.
Technical background
It is the main reason that concrete structure durability descends that chlorion is invaded the corrosion that causes reinforcing bar, and therefore the military service security of serious threat xoncrete structure, supervises detection to the steel bar corrosion situation in the xoncrete structure in real time.Rusting rate and the corrosion degree of understanding reinforcing bar are significant to military service security and remaining life that we estimate xoncrete structure.
Chlorion is invaded and is caused that the corrosion of reinforcing bar mainly is galvanic corrosion, and contrast electrode is the core ingredient that detection system is supervised in the galvanic corrosion of realization reinforcing bar in real time, for the electrochemical real-time prison detects reference potential is provided.Therefore, the electrode potential stability of contrast electrode is to obtain the basic assurance that reliable and stable steel bar corrosion electrification school superintendent detects data.In addition, the service life that xoncrete structure generally will be rectificated, concrete must have long serviceable life with contrast electrode.At present, the restriction concrete mainly is the loss of contrast electrode electrolytic solution and the pollution that electrolytic solution receives other ions in the concrete with contrast electrode serviceable life.If can effectively solve the serviceable life that the problem of this two aspect can effectively improve contrast electrode.
The electrode potential of Ag/AgCl contrast electrode receives the electrolyte flow influence of the pollution of other ions of becoming estranged in the concrete less and become and use one of contrast electrode the most widely in the concrete.But the Ag/AgCl contrast electrode adopts liquid electrolyte more at present.Adopt liquid electrolyte mainly to have following two problems: (1) has increased difficulty for the encapsulation of contrast electrode, is prone to cause the contrast electrode leakage to cause the corrosion of reinforcing bar; (2) adopt liquid electrolyte, ion is prone to transmission in liquid, can not effectively reduce electrolytical loss, influences the stability and the serviceable life of contrast electrode.The employing solid electrolyte is considered to solve the effective means of above-mentioned two problems, but because the high alkalinity of xoncrete structure and long serviceable life, so used solid electrolyte must have high alkali resistance and water-retaining property and long-term chemical stability.
Methylcellulose base organic material can be used as construction timber, has good alkali resistance and long-term chemical stability, and methylcellulose base organic material has good water conservation effect.Consider to adopt methylcellulose base gel electrolyte to replace liquid electrolyte, make the electrode potential stability of contrast electrode and increase substantially serviceable life.
Publication number is CN1949595A; Open day is on April 18th, 2007; Denomination of invention discloses a kind of contrast electrode for the Chinese invention patent application of " copper/copper/saturated copper sulphate gel reference electrode "; Its electrode has the double-decker that ceramic inside and outside shell constitutes, and is equipped with the spiral fashion copper wire in the ceramic inner casing and is full of copper/saturated copper sulphate, is filled with gel electrolyte between the two-layer ceramic housing.Its gel electrolyte is made up of nano silicon, the concentrated sulphuric acid, polyacrylamide.For this application, its used electrode material is Cu, and interior reference electrolyte is saturated CuSO
4Solution, and reference electrolyte in by nano silicon, the concentrated sulphuric acid, polyacrylamide gel electrolyte not being, its effect is to be filled in the pollution that prevents extraneous ion between the inside and outside ceramic case.
Summary of the invention
The present invention is directed to the prior art deficiency, adopt gel electrolyte directly to replace liquid electrolyte, effectively reduce the difficulty of electrode package on the one hand; On the other hand, can improve resistance in the contrast electrode, hinder electrolytical loss, improve contrast electrode stability and serviceable life.
In order to realize the foregoing invention purpose; The present invention has adopted following technical scheme: a kind of reinforced concrete is used contrast electrode; It is characterized in that: have a sleeve pipe, cannula cavity is filled with gel electrolyte, one be connected with copper cable the Ag/AgCl electrode be inserted in the said gel electrolyte; Said sleeve pipe seals with epoxide resin material at first end that is connected to copper cable, is filling with the micropore ceramics hole with the said first end second opposed end.
Second end that is filled with micropore ceramics of said sleeve pipe is fixed with epoxy resin and is sealed, its effect be to the micropore ceramics piece fix and prevent in the reference electrolyte run off through the gap between ceramic block and sleeve pipe.
Second end that is filled with micropore ceramics of said sleeve pipe is provided with external thread, and the protective sleeve that is spirally connected, and protective sleeve is detachable design, when contrast electrode uses, dismantles, and loads onto the loss that can protect micropore ceramics and prevent electrolyte moisture when not using.
Said sleeve pipe adopts polytetrafluoroethylmaterial material to process; Said protective sleeve adopts polytetrafluoroethylmaterial material to process.
Said gel electrolyte is a methylcellulose base gel electrolyte, and said methylcellulose Binder Materials can be a kind of in methylcellulose, hydroxyethyl carboxymethyl cellulose, carboxyethyl methylphosphinate cellulose or the hydroxypropyl methylcellulose.
Can be added with the macromolecule water-keeping material in the said gel electrolyte, with further reduction water loss.
The said copper cable that is connected with the Ag/AgCl electrode adopts the single core copper cable of 0.6/1.0KVA.
The external diameter of said sleeve pipe is Φ 20mm, and internal diameter is Φ 16mm, and long is 100mm.
Said micropore ceramics is that thickness is the zeyssatite micropore ceramics of 10mm, and the aperture is 0.2um, and the porosity is 80%, can satisfy the ion migration, and effectively controls ion migration and water loss speed, the stability and the serviceable life of improving contrast electrode.
A kind of reinforced concrete is characterized in that may further comprise the steps with the manufacturing approach of contrast electrode:
(1) preparation Ag/AgCl electrode;
(2) preparation gel electrolyte: the KCl solution of preparation 0.5mol/L; To join solution be heated to 70～100 ℃; Add the methylcellulose Binder Materials again in the solution of thermotropism; Add 1g methylcellulose Binder Materials by per 10～15mL solution and add, after slowly stirring, in air, be cooled to room temperature and can make gel electrolyte;
(3) the micropore ceramics piece is fixed on an end of cannula cavity; In the gel electrolyte sprue bushing that makes; After treating gelling electrolyte cooling gelling; The Ag/AgCl electrode that is welded with copper cable is inserted along the center line of teflon sleeve, again with epoxy resin to the openend of sleeve pipe with epoxy sealing, can make the Ag/AgCl contrast electrode.
The present invention adopts micropore ceramics to realize and extraneous electrolytical the link, guarantees the transmission of ion.Thereby influence the potential stability and the serviceable life of contrast electrode for the pollution of controlling electrolytical loss of contrast electrode and extraneous ion; The present invention has adopted gel electrolyte; Also select effective micropore ceramics parameter and the method that prolongs ion expanding path (contrast electrode physical dimension) to control the entering of electrolytical loss and extraneous ion in the contrast electrode in addition, guarantee that institute invent that the current potential of the contrast electrode of development is stablized and prolongation contrast electrode serviceable life.This contrast electrode not only has high electrode potential stability and long serviceable life, and has that volume is little, intensity is high and make advantages such as simple, can be used for concrete system fully, realizes that the long-term galvanic corrosion prison of reinforcing bar detects.
Description of drawings
Fig. 1 is an Ag/AgCl contrast electrode basic structure principle schematic of the present invention.
Fig. 2 is an Ag/AgCl contrast electrode electrode potential change curve in time.
Embodiment
Be illustrated in figure 1 as the structure of contrast electrode of the present invention, it comprises copper cable 1, epoxy sealing cover 2, teflon sleeve 3, methylcellulose base gel electrolyte 4, Ag/AgCl electrode 5, micropore ceramics piece 6, epoxy resin fit sealing spare 7 and teflon protective sleeve 8.Micropore ceramics piece 6 is fixed on teflon sleeve 3 to be with an externally threaded end and to fix and seal formation epoxy resin fit sealing spare 7 with epoxy resin; Methylcellulose base gel electrolyte 4 is injected in the teflon sleeve 3; After treating the 4 cooling gellings of gelling electrolyte; The center line of the Ag/AgCl electrode 5 that is welded with copper cable 1 along teflon sleeve 3 inserted; With epoxy resin the openend of teflon sleeve 3 is filled again, form epoxy sealing cover 2, just can be made into Ag/AgCl contrast electrode of the present invention.
The external diameter of the sleeve pipe that is adopted is Φ 20mm, and internal diameter is Φ 16mm, and long is 100mm.The micropore ceramics that is adopted is that thickness is the zeyssatite micropore ceramics of 10mm, and the aperture is 0.2um, and the porosity is 80%.
The preparation of embodiment 1:Ag/AgCl electrode
To be of a size of the bar-shaped pure Ag (99.99%) of Φ 3 * 80mm and the copper wire welding back of copper cable and weld sealed, to prevent the generation of bimetallic corrosion with epoxy resin.The Ag rod is put into the greasy dirt that acetone soln is removed the surface behind 600# sand paper uniform grinding, put into 5% salpeter solution 1min after water cleans to remove the oxide on surface, more silver-colored rod is put into alcohol and cleans with ultrasound wave.Silver-colored rod after cleaning is put into electrolytic cell, and the silver rod is as anode, and MMO titanium base mixed-metal oxides is as negative electrode, with 1mA/cm
2Current density anode polarization in the HCl of 0.1mol/L solution made the Ag/AgCl electrode in 1 hour, the KCl solution of the electrode for preparing being put into 0.1mol/L is for use.
Embodiment 2: the preparation of gel electrolyte
The methyl cellulose gel solution that adopts 0.5mol/LKCl is as electrolyte; Its preparation method is following: the KCl solution of preparation 0.5mol/L; To join solution be heated to more than 70 ℃, add methylcellulose (amount of adding adds the 1g methylcellulose by every 10mL solution) again in the solution of thermotropism.After stirring, in air, be cooled to room temperature and can make gel electrolyte.In addition,, improve contrast electrode stability, can in gel electrolyte, add the macromolecule water-keeping material for improving the water retention property of gel electrolyte.
Another preparation embodiment of the gel electrolyte of embodiment 3:Ag/AgCl contrast electrode
This example is roughly the same with the preparation process of embodiment 2; Difference is that the hydroxyethyl carboxymethyl cellulose gel solution of gel electrolyte employing 0.5mol/LKCl is as electrolyte; Its preparation method is following: the KCl solution of preparation 0.5mol/L; To join solution be heated to more than 80 ℃, add hydroxyethyl carboxymethyl cellulose (amount of adding adds the 1g hydroxyethyl carboxymethyl cellulose by every 10mL solution) again in the solution of thermotropism.After stirring, in air, be cooled to room temperature and can make gel electrolyte.
Another preparation embodiment of the gel electrolyte of embodiment 4:Ag/AgCl contrast electrode
This example is roughly the same with the preparation process of embodiment 2; Difference is that the HEMC gel solution of gel electrolyte employing 0.5mol/LKCl is as electrolyte; Its preparation method is following: the KCl solution of preparation 0.5mol/L; To join solution be heated to boiling, add HEMC (amount of adding adds the 1g HEMC by every 12mL solution) again in the solution of thermotropism.After stirring, in air, be cooled to room temperature and can make gel electrolyte.
Another preparation embodiment of the gel electrolyte of embodiment 5:Ag/AgCl contrast electrode
This example is roughly the same with the preparation process of embodiment 2; Difference is that the hydroxypropyl methylcellulose gel solution of gel electrolyte employing 0.5mol/LKCl is as electrolyte; Its preparation method is following: the KCl solution of preparation 0.5mol/L; To join solution be heated to more than 90 ℃, add hydroxypropyl methylcellulose (amount of adding adds the 1g hydroxypropyl methylcellulose by every 10mL solution) again in the solution of thermotropism.In air, be cooled to room temperature and can make gel electrolyte.
Embodiment 6: the research of contrast electrode potential stability
Adopt secondary deionized water to prepare saturated aqua calcis, place beaker to be positioned in the thermostat water bath the saturated aqua calcis for preparing, the temperature of water-bath is set to 25 ℃, and the contrast electrode for preparing is positioned in the beaker.The Ag/AgCl contrast electrode that adopts digital multimeter to measure to be developed is with respect to the electrode potential of saturated calomel electrode situation over time, and is as shown in Figure 2.Test result shows: in the 30 day time of test, potential fluctuation is no more than 7mV, and the visible contrast electrode of being developed has higher potential stability.
Claims (10)
1. a reinforced concrete is used contrast electrode; It is characterized in that: have a sleeve pipe; Cannula cavity is filled with gel electrolyte; One be connected with copper cable the Ag/AgCl electrode be inserted in the said gel electrolyte, said sleeve pipe seals with epoxide resin material at first end that is connected to copper cable, is filling with the micropore ceramics hole with the said first end second opposed end.
2. reinforced concrete according to claim 1 is used contrast electrode, it is characterized in that: second end that is filled with micropore ceramics of said sleeve pipe carries out sealing and fixing with epoxy resin.
3. reinforced concrete according to claim 2 is used contrast electrode, it is characterized in that: second end that is filled with micropore ceramics of said sleeve pipe is provided with external thread, and is bolted in a protective sleeve.
4. reinforced concrete according to claim 3 is used contrast electrode, it is characterized in that: said sleeve pipe adopts polytetrafluoroethylmaterial material to process; Said protective sleeve adopts polytetrafluoroethylmaterial material to process.
5. reinforced concrete according to claim 1 is used contrast electrode; It is characterized in that: said gel electrolyte is a methylcellulose base gel electrolyte, and said methylcellulose Binder Materials can be a kind of in methylcellulose, hydroxyethyl carboxymethyl cellulose, carboxyethyl methylphosphinate cellulose or the hydroxypropyl methylcellulose.
6. reinforced concrete according to claim 5 is used contrast electrode, it is characterized in that: be added with the macromolecule water-keeping material in the said gel electrolyte to reduce the electrolyte water loss.
7. reinforced concrete according to claim 1 is used contrast electrode, it is characterized in that: the said copper cable that is connected with the Ag/AgCl electrode adopts the single core copper cable of 0.6/1.0KVA.
8. reinforced concrete according to claim 1 is used contrast electrode, it is characterized in that: the external diameter of said sleeve pipe is Φ 20mm, and internal diameter is Φ 16mm, and long is 100mm.
9. reinforced concrete according to claim 1 is used contrast electrode, it is characterized in that: said micropore ceramics is that thickness is the zeyssatite micropore ceramics of 10mm, and the aperture is 0.2um, and the porosity is 80%.
10. a reinforced concrete is characterized in that may further comprise the steps with the manufacturing approach of contrast electrode:
(1) preparation Ag/AgCl electrode;
(2) preparation gel electrolyte: the KCl solution of preparation 0.5mol/L; To join solution be heated to 70～100 ℃; Add the methylcellulose based cementitious material again in the solution of thermotropism; Add 1g methylcellulose based cementitious material by per 10～15mL solution and add, after slowly stirring, in air, be cooled to room temperature and can make gel electrolyte;
(3) the micropore ceramics piece is fixed on an end of cannula cavity; In the gel electrolyte sprue bushing that makes; After treating gelling electrolyte cooling gelling; The Ag/AgCl electrode that is welded with copper cable is inserted along the center line of teflon sleeve, again with epoxy resin to the openend of sleeve pipe with epoxy sealing, can make the Ag/AgCl contrast electrode.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680387A (en) * | 2012-04-28 | 2012-09-19 | 中交四航工程研究院有限公司 | Real-time monitoring sensor for durability of concrete structures and fabricating method thereof |
| CN102944594A (en) * | 2012-06-04 | 2013-02-27 | 哈尔滨工程大学 | Long-life reference electrode suitable for deep-sea high-hydrostatic pressure environment |
| CN103076365A (en) * | 2013-01-08 | 2013-05-01 | 苏州热工研究院有限公司 | Pen-type potential-chloride ion sensor |
| CN103207221A (en) * | 2013-03-22 | 2013-07-17 | 中交四航工程研究院有限公司 | Sensor for monitoring depth distribution of concentration and pH (potential of hydrogen) values of chloride ions in concrete protective layer and method for manufacturing sensor |
| CN103822950A (en) * | 2014-03-11 | 2014-05-28 | 苏州热工研究院有限公司 | Embedded type composite reference electrode for corrosion monitoring/detecting of reinforced concrete |
| CN104914148A (en) * | 2015-06-11 | 2015-09-16 | 哈尔滨工程大学 | Long-service-life reference electrode applicable to high-temperature and high-voltage corrosive environment |
| CN104964919A (en) * | 2015-05-22 | 2015-10-07 | 河海大学 | PH value gel electrolyte buffer layer applied in solid Ag/AgCl reference electrode, and production method thereof |
| CN106124583A (en) * | 2016-08-18 | 2016-11-16 | 河南理工大学 | A kind of reference electrode protection structure of the rotary erosion dynamic electrochemical test system of abrasion |
| CN106885835A (en) * | 2017-04-01 | 2017-06-23 | 江苏科技大学 | A kind of steel reinforced concrete erosion monitoring built-in type reference electrode and manufacture method |
| CN106990147A (en) * | 2017-06-06 | 2017-07-28 | 大连华城电子有限公司 | A kind of combination PH electrode reference liquid permeability apparatus |
| CN108776162A (en) * | 2018-09-18 | 2018-11-09 | 广州悦荣欣科技有限公司 | Electrochemical reference electrode |
| CN109342519A (en) * | 2018-09-29 | 2019-02-15 | 中国科学院长春应用化学研究所 | A kind of measuring device and preparation method thereof avoiding pollution pH combination electrode |
| CN109473741A (en) * | 2018-10-18 | 2019-03-15 | 中南大学 | The reference electrode of individual packages suitable for lithium ion battery |
| CN110261295A (en) * | 2019-06-05 | 2019-09-20 | 中国船舶重工集团公司第七二五研究所 | A kind of seawaterline elbow local corrosion electrochemical testing device and method |
| CN112924504A (en) * | 2021-01-28 | 2021-06-08 | 江苏科技大学 | Sensor for in-situ measurement of chloride ion concentration in concrete |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680387A (en) * | 2012-04-28 | 2012-09-19 | 中交四航工程研究院有限公司 | Real-time monitoring sensor for durability of concrete structures and fabricating method thereof |
| CN102680387B (en) * | 2012-04-28 | 2014-08-20 | 中交四航工程研究院有限公司 | Real-time monitoring sensor for durability of concrete structures and fabricating method thereof |
| CN102944594B (en) * | 2012-06-04 | 2015-10-28 | 哈尔滨工程大学 | Be applicable to the long service life reference electrode under deep-sea high hydrostatic pressure environment |
| CN102944594A (en) * | 2012-06-04 | 2013-02-27 | 哈尔滨工程大学 | Long-life reference electrode suitable for deep-sea high-hydrostatic pressure environment |
| CN103076365A (en) * | 2013-01-08 | 2013-05-01 | 苏州热工研究院有限公司 | Pen-type potential-chloride ion sensor |
| CN103207221A (en) * | 2013-03-22 | 2013-07-17 | 中交四航工程研究院有限公司 | Sensor for monitoring depth distribution of concentration and pH (potential of hydrogen) values of chloride ions in concrete protective layer and method for manufacturing sensor |
| CN103822950A (en) * | 2014-03-11 | 2014-05-28 | 苏州热工研究院有限公司 | Embedded type composite reference electrode for corrosion monitoring/detecting of reinforced concrete |
| CN104964919A (en) * | 2015-05-22 | 2015-10-07 | 河海大学 | PH value gel electrolyte buffer layer applied in solid Ag/AgCl reference electrode, and production method thereof |
| CN104914148A (en) * | 2015-06-11 | 2015-09-16 | 哈尔滨工程大学 | Long-service-life reference electrode applicable to high-temperature and high-voltage corrosive environment |
| CN104914148B (en) * | 2015-06-11 | 2017-08-04 | 哈尔滨工程大学 | Suitable for the long service life reference electrode under high temperature pressure corrosion environment |
| CN106124583A (en) * | 2016-08-18 | 2016-11-16 | 河南理工大学 | A kind of reference electrode protection structure of the rotary erosion dynamic electrochemical test system of abrasion |
| CN106124583B (en) * | 2016-08-18 | 2018-10-09 | 河南理工大学 | A kind of reference electrode protection structure of rotary erosion abrasion dynamic electrochemical test system |
| CN106885835A (en) * | 2017-04-01 | 2017-06-23 | 江苏科技大学 | A kind of steel reinforced concrete erosion monitoring built-in type reference electrode and manufacture method |
| CN106990147A (en) * | 2017-06-06 | 2017-07-28 | 大连华城电子有限公司 | A kind of combination PH electrode reference liquid permeability apparatus |
| CN108776162A (en) * | 2018-09-18 | 2018-11-09 | 广州悦荣欣科技有限公司 | Electrochemical reference electrode |
| CN109342519A (en) * | 2018-09-29 | 2019-02-15 | 中国科学院长春应用化学研究所 | A kind of measuring device and preparation method thereof avoiding pollution pH combination electrode |
| CN109473741A (en) * | 2018-10-18 | 2019-03-15 | 中南大学 | The reference electrode of individual packages suitable for lithium ion battery |
| CN110261295A (en) * | 2019-06-05 | 2019-09-20 | 中国船舶重工集团公司第七二五研究所 | A kind of seawaterline elbow local corrosion electrochemical testing device and method |
| CN112924504A (en) * | 2021-01-28 | 2021-06-08 | 江苏科技大学 | Sensor for in-situ measurement of chloride ion concentration in concrete |
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Application publication date: 20120404 |