CN101825600A - Method for preparing high-temperature electrochemical working electrode - Google Patents
Method for preparing high-temperature electrochemical working electrode Download PDFInfo
- Publication number
- CN101825600A CN101825600A CN201010180710A CN201010180710A CN101825600A CN 101825600 A CN101825600 A CN 101825600A CN 201010180710 A CN201010180710 A CN 201010180710A CN 201010180710 A CN201010180710 A CN 201010180710A CN 101825600 A CN101825600 A CN 101825600A
- Authority
- CN
- China
- Prior art keywords
- temperature
- electrode
- corrosion
- pvc pipe
- working electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a method for preparing a high-temperature electrochemical working electrode, and belongs to the technical field of electrochemical corrosion measurement and material characterization. The method is characterized in that: a welded double electrode is fixed in a base; a PVC pipe at a proper size is connected with the base and is sealed by an aluminum foil; commonly used Portland cement is used as a packaging material; the ordinary PVC pipe is used for packaging an infusion grinding tool; and finally, the PVC pipe is softened and stripped at a high temperature to prepare the high-temperature working electrode with high corrosion resistance and high temperature resistance. The whole working electrode is divided into two work testing parts and is convenient to monitor electrochemical noise under a high-temperature corrosion condition. The method has the advantages of low cost, simple process and easy operation, and is favorable for accurately monitoring the material corrosion performance in real time in the corrosion process under the high-temperature corrosion condition. The method is suitable for all metal matrixes for electrochemical detection, such as stainless steel, carbon steel and the like, and can be used in law measurement, mechanism inspection and characterization of material performance in a corrosive environment.
Description
Technical field
The invention belongs to galvanic corrosion measurement and material and characterize technical field, relate to the preparation method of working electrode in the high-temperature electrochemistry system.Be particularly related to: utilize portland cement commonly used to be encapsulating material, utilize the common PVC pipe for the encapsulation of perfusion grinding tool prepared corrosion resistivity strong, can resistant to elevated temperatures hot operation electrode.And whole working electrode is divided into 2 operation detection parts, is the preparation method of being convenient to a kind of high-temperature electrochemical working electrode of electrochemical noise monitoring under the high temperature corrosion condition.
Background technology
Electrochemical research is measured and is comprised common activation polarization, cyclic voltammetric, AC impedance and the methods such as electrochemical noise of rising at present.Because electrochemical method can accurately be measured the transfer of electric charge in the electrochemical reaction process, is widely applied to different field such as corrosion monitoring, material sign at present.And three electrodes of its basic composition: contrast electrode, be the important prerequisite that realizes these detection methods to the preparation of electrode, working electrode.Along with the raising of testing environment temperature, the preparation method of hot operation electrode not only has irreplaceable status in electrochemical field, have more important practical value.
High-molecular organic material is mainly used in the encapsulation of working electrode, for example teflon, poly-trifluoro-ethylene, polyaryletherketone and epoxy resin etc.Epoxy resin often is used in the encapsulation of electrochemical working electrode owing to have good processibility and high cost performance.But because of its curing material is crisp, resistance to cracking energy, and poor heat resistance make its application be subjected to certain restriction.The main application of epoxy encapsulation of current ambient temperature and the electrochemical measurement below 100 ℃ preparation work electrode.Though teflon, poly-trifluoro-ethylene have good heat-resistant, can use for a long time under 250-260 ℃ of hot conditions; Have good chemical stability, electrical insulating property and corrosion resistance simultaneously; But it is difficult for melt fabrication, and processing difficulties very easily causes encapsulated electrode to be revealed, and causes electrode to be scrapped, and its hydrophobicity performance makes in measurement easily and adhere to bubble at electrode surface, influences electrochemical measurement.Therefore the preparation method at electro-chemical systems under 150-250 ℃ and working electrode is very few.People such as the Niu Li of Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences in 2004 utilize the epoxy resin of the micromolecule crosslinking chemical mixture solidified modification of different proportion, in the calibration cell of preheating, water, encapsulate the preparation work electrode and carry out 100-200 ℃ of hot setting, make the working electrode of preparation under 250 ℃ of operating modes of high temperature, to use.Utilize the epoxy resin toughened encapsulating material of method that adds the SiO2 nano particle simultaneously, effectively reduce the fragility of epoxy resin; The working electrode of preparation can encapsulate most of electrochemical working electrodes such as gold, platinum, vitreous carbon, graphite 150 ℃ of uses.
Summary of the invention
The object of the invention has provided the preparation method of working electrode under a kind of high-temperature electrochemistry system.Utilize portland cement commonly used to be encapsulating material, utilize common PVC pipe and firm banking to be assembled into the perfusion grinding tool, two identical columnar metal electrode preparation of encapsulation corrosion resistivity strong, can resistant to elevated temperatures high-temperature electrochemical working electrode.The present invention is the basis of realizing that high-temperature electrochemistry detects, and has solved corrosion process, a material corrosion performance difficult problem real-time, that accurately monitor under the high temperature corrosion condition.
Technical scheme of the present invention is: the bipolar electrode that utilizes firm banking to be connected with wire bonds to finish is at the pvc pipe internal fixation, and utilizes encapsulant that firm banking is partly carried out encapsulation process.The portland cement encapsulating compound that disposes, stirs is poured in the pvc pipe.And the electrode that can finishes heat-treated, make that the moisture in the encapsulating compound in time volatilizees.Pvc pipe is softened peel off, the galvanochemistry duplex that obtains high temperature is made electrode.Process mesosilicic acid salt cement disposes the thickness of will trying one's best, and utilizes the foil sealing base.Processing step of the present invention is as follows:
1. utilize spot welding to be connected with lead respectively two identical metal electrodes.
2. will weld good bipolar electrode as accompanying drawing (4) and utilize base to fix, and the pvc pipe of appropriate size will be connected with base, and utilize foil sealing, leak liquid not between assurance base and the pvc pipe.
3. the portland cement that will mix, prepares pours in the grinding tool of pvc pipe and base composition, the submergence lead.
4. entire electrode placed 30 ℃ of constant temperature system constant temperature 24 hours, with moisture evaporate to dryness in the encapsulant.
5. and be warming up to 180 ℃ and make the pvc pipes as grinding tool soften, peel off.
6. remove the high-temperature electrochemical working electrode that aluminium foil and base obtain having double[-unit.
Effect of the present invention and benefit are: the present invention utilizes cheap material, simple technology has prepared the hot operation electrode and operation is easily gone, encapsulation, the connectivity problem of high-temperature electrochemistry testing electrode have been solved, be to realize the hot operation electrode that high-temperature electrochemistry detects provides the basis, help corrosion process under the high temperature corrosion condition, material corrosion performance in real time, monitoring accurately.The existence of two workplaces simultaneously is more convenient for fully utilizing multiple electrochemical detection method and is measured sign.The present invention is applicable to stainless steel, carbon steel etc., and all can be used as the metallic matrix of Electrochemical Detection, can be applicable in the sign of rule measurement, mechanism investigation and material property under the corrosive atmosphere.
Description of drawings
Accompanying drawing 1 is a hot operation electrodes base left-half synoptic diagram among the present invention.
Accompanying drawing 2 is hot operation electrodes base right half part synoptic diagram among the present invention.
Accompanying drawing 3 is hot operation electrode solidified forming structure and assembling left-half synoptic diagram among the present invention.
Accompanying drawing 4 is hot operation electrode solidified forming structure and assembling right half part synoptic diagram among the present invention.
Among the figure: 1 firm banking, 2 working electrode bottom tubs, 3 working electrode metal columns, 4PVC control grinding tool, 5 wire-protecting sleeve pipes, 6 working electrode leads.
Embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1:
Select for use the stainless steel column of SUS304 of two φ 4mm * 20mm to utilize spot welding to be connected with the Eureka wire of φ 1mm.Select for use the high density warming plate of 20mm * 20mm * 15mm to do submount material, the working metal electrode column that 2 welding are good is fixed in the middle of the base.Select for use the long φ 20mm * 2mmPVC pipe of 30mm to be sleeved on the base, and pvc pipe is inserted in the base bottom from top of electrodes.The outside unnecessary base of pvc pipe is removed, utilize aluminium foil, avoid fill material to reveal base and base and pvc pipe junction parcel.Then the portland cement that mixes is filled in the grinding tool, and is placed in 30 ℃ of constant temperature systems and placed 24 hours.Afterwards system being warming up to 180 ℃ makes pvc pipe softening and peel off in electrode body.After aluminium foil and base removed, electrode surface is carried out mechanical grinding and polishing, obtain resistant to elevated temperatures stainless steel duplex and make electrode.
Embodiment 2:
Select for use the carbon steel post of two φ 4mm * 20mm to utilize spot welding to be connected with the copper conductor of φ 1mm.Select for use the high density warming plate of 20mm * 20mm * 15mm to do submount material, the working metal electrode column that 2 welding are good is fixed in base and φ 20mm * 2mmPVC pipe that 30mm is long is sleeved on the base from top of electrodes.Utilize aluminium foil with base and base and pvc pipe junction parcel, avoid fill material to reveal.Then the portland cement that mixes is filled in the grinding tool, and is placed in 30 ℃ of constant temperature systems and placed 24 hours.Afterwards system being warming up to 180 ℃ makes pvc pipe softening and peel off in electrode body.After aluminium foil and base removed, electrode surface is carried out mechanical grinding and polishing, obtain resistant to elevated temperatures carbon steel duplex and make electrode.
Claims (1)
1. the preparation method of a high-temperature electrochemical working electrode, it is characterized in that the bipolar electrode that welding is good is fixed in the base, the pvc pipe of appropriate size is connected with base, and use foil sealing, utilize portland cement commonly used to be encapsulating material, utilize the common PVC pipe to be the encapsulation of perfusion grinding tool, again entire electrode is placed 30 ℃ of constant temperature systems be warming up to after 24 hours 180 ℃ softening and peel off pvc pipe, prepared corrosion resistivity strong, can resistant to elevated temperatures hot operation electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010180710A CN101825600A (en) | 2010-05-19 | 2010-05-19 | Method for preparing high-temperature electrochemical working electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010180710A CN101825600A (en) | 2010-05-19 | 2010-05-19 | Method for preparing high-temperature electrochemical working electrode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101825600A true CN101825600A (en) | 2010-09-08 |
Family
ID=42689639
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010180710A Pending CN101825600A (en) | 2010-05-19 | 2010-05-19 | Method for preparing high-temperature electrochemical working electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101825600A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108362748A (en) * | 2018-01-10 | 2018-08-03 | 北京科技大学 | A kind of preparation and application of heat-resisting wire beam electrode |
| CN111257389A (en) * | 2020-03-16 | 2020-06-09 | 昆明理工大学 | High-voltage reference electrode, preparation method and application |
| CN113267548A (en) * | 2021-06-25 | 2021-08-17 | 清华大学 | Method for producing an electrode system for an electrochemical test system |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4256561A (en) * | 1978-05-10 | 1981-03-17 | Dr. Eduard Fresenius Chemisch-Pharmazeutische Industrie Kg, Apparatebau Kg | Electrochemical measuring electrode |
| EP0486057A2 (en) * | 1990-11-16 | 1992-05-20 | Oronzio De Nora S.A. | Permanent reference electrode for monitoring the electrochemical potential of metal structures in concrete and soil |
| US5571396A (en) * | 1993-07-12 | 1996-11-05 | Dade International Inc. | Fluid analysis system and sensing electrode, electrode assembly, and sensing module components |
| CN1601266A (en) * | 2004-10-08 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for fabricating electrochemical working-electrode |
| CN101144790A (en) * | 2007-09-14 | 2008-03-19 | 哈尔滨工业大学 | All-solid reference electrode for monitoring steel bar corrosion of concrete and its preparation method |
| CN101661016A (en) * | 2009-09-18 | 2010-03-03 | 东北大学 | Method for measuring hydrogen pressure in solid steel and device |
-
2010
- 2010-05-19 CN CN201010180710A patent/CN101825600A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4256561A (en) * | 1978-05-10 | 1981-03-17 | Dr. Eduard Fresenius Chemisch-Pharmazeutische Industrie Kg, Apparatebau Kg | Electrochemical measuring electrode |
| EP0486057A2 (en) * | 1990-11-16 | 1992-05-20 | Oronzio De Nora S.A. | Permanent reference electrode for monitoring the electrochemical potential of metal structures in concrete and soil |
| US5571396A (en) * | 1993-07-12 | 1996-11-05 | Dade International Inc. | Fluid analysis system and sensing electrode, electrode assembly, and sensing module components |
| CN1601266A (en) * | 2004-10-08 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for fabricating electrochemical working-electrode |
| CN101144790A (en) * | 2007-09-14 | 2008-03-19 | 哈尔滨工业大学 | All-solid reference electrode for monitoring steel bar corrosion of concrete and its preparation method |
| CN101661016A (en) * | 2009-09-18 | 2010-03-03 | 东北大学 | Method for measuring hydrogen pressure in solid steel and device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108362748A (en) * | 2018-01-10 | 2018-08-03 | 北京科技大学 | A kind of preparation and application of heat-resisting wire beam electrode |
| CN108362748B (en) * | 2018-01-10 | 2020-06-26 | 北京科技大学 | Preparation and application methods of heat-resistant tow electrode |
| CN111257389A (en) * | 2020-03-16 | 2020-06-09 | 昆明理工大学 | High-voltage reference electrode, preparation method and application |
| CN113267548A (en) * | 2021-06-25 | 2021-08-17 | 清华大学 | Method for producing an electrode system for an electrochemical test system |
| CN113267548B (en) * | 2021-06-25 | 2022-03-29 | 清华大学 | Method for producing an electrode system for an electrochemical test system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108093501B (en) | Graphene heating film and graphene heating film assembly suitable for power battery pack | |
| CN101968511B (en) | Small electrode experiment device for measuring resistivity of mineral and solid insulating material | |
| CN103424313B (en) | In-situ tensile and hydrogen content monitoring device, and method for monitoring content of hydrogen by using same | |
| CN104458560B (en) | A kind of wire beam electrode and its preparation and application | |
| CN108548775A (en) | Enamel coating electrode and preparation method, corrosion resistance test method | |
| CN102788828B (en) | IrOx electrode prepared through cyclic thermo oxidation method | |
| CN101825600A (en) | Method for preparing high-temperature electrochemical working electrode | |
| CN104777210B (en) | Three-electrode electro Chemical measuring system for high pressure hydrothermal system and preparation method thereof | |
| CN106066353A (en) | Flexible array reference electrode and apply the method that its on-spot study metal welding seam corrodes | |
| CN102368564A (en) | Gel-type polymer electrolyte and preparation method thereof | |
| CN110333275A (en) | Corrosion monitoring electrode and preparation and detection method in a kind of conducting concrete environment | |
| CN104749234B (en) | A kind of platinum electrode for HTHP hydrothermal system and preparation method thereof | |
| CN204439591U (en) | A kind of working electrode of electrochemical property test three-electrode system | |
| CN109342520B (en) | A kind of all-solid-state pH combination electrode device and preparation method thereof | |
| CN202854016U (en) | Clamp device for alternating-current (AC) resistivity test of non-metallic materials | |
| WO2024045518A1 (en) | Screening method for optimal zinc ion concentration of primary loop during thermal state function test of nuclear power plant | |
| CN107328833A (en) | The high temperature resistant wire beam electrode and preparation method characterized for combined material chip | |
| CN209296543U (en) | A kind of thermoelectric couple corrosion experimental device | |
| CN104614255B (en) | A kind of axially loaded stress corrosion testing device of high temperature | |
| CN108519420B (en) | A kind of dissolved oxygen electrode, preparation method, dissolved oxygen probe and dissolved oxygen instrument | |
| CN105990279A (en) | Preparation device and method of metal thermal interface material | |
| CN110014718A (en) | A method of gallium base thermal interface material applications are enhanced into interface heat transfer in aluminium substrate | |
| CN204903454U (en) | A oxygen chemical sensor that is used for high temperature water under high pressure hot body to be | |
| CN106706736A (en) | Method for improving stability of iridium/iridium oxide pH (potential of Hydrogen) electrode | |
| CN210269702U (en) | Electrochemical test electrolytic cell with controllable temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100908 |