CN109187327A - Metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change device - Google Patents
Metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change device Download PDFInfo
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- CN109187327A CN109187327A CN201811114423.0A CN201811114423A CN109187327A CN 109187327 A CN109187327 A CN 109187327A CN 201811114423 A CN201811114423 A CN 201811114423A CN 109187327 A CN109187327 A CN 109187327A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
Abstract
The present invention discloses a kind of metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change device.It is to have threaded I-shaped rodlike the first working electrode of test button (1) that is stretched including both ends；By the second working electrode (4) constituted in insertion glass tube (6) behind platinum filament (8) and filamentary silver (7) welding；In the electrolytic cell (9) of hollow cylindrical structure, the first working electrode is arranged in electrolytic cell axle center, and electrolytic cell top surface plugs reference electrode (2) and auxiliary electrode (3), plugs the second working electrode in the middle part of the side wall of electrolytic cell；Reference electrode lower end connects Luggin capillary (11).This monitoring device being capable of real-time in-situ monitoring metal/electrolyte solution interface microcell pH value dynamic change；It is good with stability, response is fast, accuracy is high, high repeatability and other advantages；Overall structure is easy production, low in cost, easy to operate, easy to use, has wide range of applications.
Description
Technical field
The present invention relates to a kind of monitoring device of pH value dynamic change, specifically a kind of metal stresses corrosion process median surfaces
Microcell pH value Monitoring on Dynamic Change device.
Background technique
The stress corrosion (Stss Corrosion Cracking, SCC) of metal is a kind of relatively conventional local corrosion,
It is also one of maximum Corrosion Types of harm.When stress corrosion occurs apparent homogeneous corrosion does not occur for metal, in its table
The corrosion product that face generates is also few, unobvious.Therefore, stress corrosion is often sent out in the case where no any sign suddenly
It is raw, it is a kind of catastrophic corrosion.Take suitable safeguard procedures that can guarantee to avoid the occurrence and development of stress corrosion on metal
Installation security avoids losing.And understand metal stresses corrosion mechanism and influence factor be the key that develop guard technology.
The method of traditional research metal stresses corrosion mechanism and influence factor mainly has stretching experiment, speed electrokinetic potential pole
Change the surface physics technology of scanning technique and ex situ.Stretching experiment, by its loading method, can be divided into constant load, permanent deformation and
Slow strain rate tension etc..The surface physics technology of ex situ mainly uses scanning electron microscope (SEM) and EDS (Energy
Dispersive Spectrometer) etc. observation fracture apperance and incision position corrosion product composition is analyzed.These states
The inside and outside conventional method generally used is merely able to obtain integrated stress-strain information of the metal within certain a period of time that be corroded
And Electrochemistry Information, there is certain limitation.It is therefore desirable to develop new idea and method research stress corrosion, it is desirably to obtain
Real-time in-situ multidate information in metal stresses corrosion process, and the mechanism and influence factor of further investigated stress corrosion accordingly.
Metal/electrolyte solution interface microcell pH value dynamic change can obtain more during research stress corrosion
Electrochemistry Information and interface multidate information during stress corrosion, and then can be with the mechanism and its shadow of further investigated stress corrosion
The factor of sound[1].For example, can be gone to speculate that the composition of electrode surface film and its variation, discussion are answered according to the dynamic change of microcell pH value
The occurrence and development process of power corrosion, is sentenced the influence factor for judging developing stage locating for stress corrosion, furtheing investigate stress corrosion
The effect etc. of disconnected safeguard procedures.
Be traditionally used for the various glass electrodes of pH value determination, metal-metallic oxide electrode, ion selective electrode and
(quinone) quinhydrone electrode etc., general volume is larger, it is impossible to be used in the dynamic change of real-time in-situ monitoring microcell pH value.The most common glass
When glass electrode is used for pH value determination there is also cracky, be frequently necessary to be demarcated, operating process is complicated the disadvantages of, use
It is very inconvenient.
In recent years, continuous someone developed novel for measuring electrodes/probes/sensor of microcell pH value etc..But
They largely all there is a problem that such or such, for example stability is poor, low-response, and accuracy is low, poor reproducibility, grasp
Make complexity, it is expensive etc..
Summary of the invention
In view of the above-mentioned problems of the prior art, the present invention is intended to provide a kind of metal stresses corrosion process median surface is micro-
The method of polyaniline electrochemistry is gathered platinum microelectrode surface, passes through potentiostat by area's pH value Monitoring on Dynamic Change device
Electrolytic cell is acquired monitoring data, realizes that real-time in-situ monitoring metal/electrolyte solution interface microcell pH value dynamic becomes
Change；The features such as stability for ensuring to monitor is strong, response is fast, accuracy is high, favorable reproducibility；And reach easy to operate, it is easy to use,
The purpose having wide range of applications.
To achieve the goals above, this metal stress corrosion process median surface microcell pH value Monitoring on Dynamic Change device, packet
The first working electrode is included, first working electrode is that both ends have the threaded I-shaped rodlike test button that is stretched；
Second working electrode, second working electrode by platinum filament with after filamentary silver welding be inserted into glass tube in constitute, as
Platinum microelectrode；
Double potentiostat system electrolytic cell, the double potentiostat system electrolytic cell are hollow cylindrical structure, the electrolysis
The first working electrode is arranged in the axle center in pond, and the top surface of the electrolytic cell plugs reference electrode and auxiliary electrode, the electrolysis simultaneously
Second working electrode vertical with first working electrode is inserted in the middle part of the side wall in pond；
The reference electrode is saturated calomel electrode, and the lower end of reference electrode connects Luggin capillary, Luggin capillary
Bottom end extends in the middle part of the active section of the first working electrode；
First working electrode, the second working electrode, reference electrode and auxiliary electrode pass through conducting wire and constant potential respectively
Instrument connection, the screw thread at the test button both ends that are stretched of first working electrode are connect with machine clamp is stretched.
Further, the auxiliary electrode is the platinized platinum of 20mm × 20mm.
Further, two rubber stoppers, threaded portion are inserted into the test button both ends that are stretched of first working electrode respectively
Divide and is completely exposed rubber stopper.
Further, the inoperative section at the test button both ends that are stretched of first working electrode passes through silicone rubber seal.
Further, the control of the distance between second working electrode and the first working electrode is at 50 μm.
Further, it is 2mm that the distance between the bottom end of the Luggin capillary and the first working electrode are constant.
Further, the length of the platinum filament is 1.5cm, diameter is 50 μm.
Further, the glass tube is the quartz glass capillary of internal diameter 0.2cm.
Further, it is bonded with rubber pad at the areole for being inserted into the second working electrode, the second work electricity after insertion
Pole is sufficiently bonded with rubber pad.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the present apparatus being capable of real-time in-situ monitoring metal/electrolyte solution interface microcell pH value dynamic change；
2, the present apparatus is good with stability, response is fast, accuracy is high, high repeatability and other advantages；
3, present apparatus overall structure is easy production, low in cost, easy to operate, easy to use, has wide range of applications.
Detailed description of the invention
Fig. 1 is to carry out gold in real-time in-situ monitor stress corrosion process using the present invention by scan-type electrochemical microscope
Category/electrolyte solution interface microcell pH value dynamic change experimental provision schematic diagram；
Fig. 2 is the platinum microelectrode schematic diagram through Polyaniline-modified that diameter is 50 μm；
Fig. 3 is the test button schematic diagram that is stretched in the present invention；
Fig. 4 is potentiostat system electrolyser construction schematic diagram in the present invention；
In figure: 1, the first working electrode, 2, reference electrode, 3, auxiliary electrode, the 4, second working electrode, 5, scan-type electrochemical
Microscope, 6, glass tube, 7, filamentary silver, 8, platinum filament, 9, electrolytic cell, 10, rubber stopper, 11, Luggin capillary.
Specific embodiment
Below with reference to examples and drawings, the present invention will be further described.
In the present invention, the dynamic of electrode/electrolyte solution interface microcell pH value during stress corrosion metal occurs
The experimental provision that variation carries out real-time in-situ monitoring is dual-electrode system, and two potentiostat combinations are measured.It can
It to be measured simultaneously using two common potentiostats, can also be measured by other potentiostat devices, the present invention
By scan-type electrochemical microscope (Scanning Electrochemical Microscopy, SECM) as permanent in embodiment
Potentiometer measures.
As shown in figures 1 and 3, this metal stress corrosion process median surface microcell pH value Monitoring on Dynamic Change device, including
First working electrode 1, first working electrode 1 are that both ends have the threaded I-shaped rodlike test button that is stretched, and are drawn
The middle part elongated portion for stretching test button is active section.
The test button that is stretched is generally rodlike or sheet, in the majority with I-shaped sample.The present invention is had using both ends
The I-shaped bar samples of screw thread, intermediate narrower portion are active section.When calculating stress and strain by drawing force, drawn described
It stretches and measures diameter respectively at the upper, middle and lower three of test button active section, be averaged as specimen finish.
Second working electrode 4, as shown in Fig. 2, second working electrode 4 is by being inserted into glass after platinum filament 8 and 7 welding of filamentary silver
It is constituted in pipe 6, the through hole for being pierced by platinum filament 8 to 6 tail portion of glass tube is sintered, and welding is for connecting potentiostat on filamentary silver 7
Copper conductor, the second working electrode 4, i.e. platinum microelectrode is made.Platinum filament 8 and filamentary silver 7 after welding pass through ultrapure water, ethyl alcohol and third
Ketone is successively cleaned by ultrasonic, and the platinum filament 8 after cleaning is placed on clean workbench with filamentary silver 7 and is dried by Infrared irradiation
It does spare；The probe portion of platinum microelectrode first passes through abrasive paper for metallograph and polishes, and for eliminating bubble, then passes through 0.05 μm of nanometer
Aluminium powder polishing, is then polished by flannelette, cleans, dry spare finally by ultrapure water.
Double potentiostat system electrolytic cell 9, as shown in Figure 1 and Figure 4, the double potentiostat system electrolytic cell 9 are hollow
The first working electrode 1 is arranged in cylindrical structure, the axle center of the electrolytic cell 9, and the top surface of the electrolytic cell 9 plugs reference electrode simultaneously
2 and auxiliary electrode 3, second working electrode vertical with first working electrode 1 is inserted in the middle part of the side wall of the electrolytic cell 9
4；Electrolytic cell 9 uses organic glass material, is bonded after being cut, being polished by chloroform, the top of cylindrical hollow electrolytic cell 9
The central symmetry of face and bottom surface offers the hole for being disposed vertically the first working electrode 1, and 9 top surface of electrolytic cell opens up useful simultaneously
It is offered in the middle part of the hole for placing reference electrode 2 and auxiliary electrode 3,9 side wall of electrolytic cell for placing after Polyaniline-modified
The hole of second working electrode 4.
It is cleaned, dry after the second working electrode 4, reference electrode 2 and auxiliary electrode 3 be placed in 0.5moldm- 3C6H5NH2·HCl+1.5mol·dm-3Electrochemical polymerization is carried out in HCl solution, and the second working electrode 4 is applied in polymerization process
The constant potential of 0.70V, polymerization time 600s.After the completion of polymerization, detecting probe surface will polymerize a strata aniline modified membrane.
As shown in Figure 1, the reference electrode 2 is saturated calomel electrode, the lower end of reference electrode 2 connects Luggin capillary
11, the bottom end of Luggin capillary 11 extends in the middle part of the active section of the first working electrode 1.
First working electrode 1, the second working electrode 4, reference electrode 2 and auxiliary electrode 3 are sequentially placed into electrolytic cell 9
Corresponding position, the screw thread at the test button both ends that are stretched of first working electrode 1 is connect with machine clamp is stretched, in electrolytic cell
Corrosion electrolyte is added in 9, then the first working electrode 1, the second working electrode 4, reference electrode 2 and auxiliary electrode 3 lead to respectively
Conducting wire is crossed to connect with the scan-type electrochemical microscope 5 as potentiostat.
Further, as shown in Figure 1, the auxiliary electrode 3 is the platinized platinum of 20mm × 20mm.
Further, as shown in figure 3, two rubbers are inserted at the test button both ends that are stretched of first working electrode 1 respectively
Rubber plug 10, threaded portion is completely exposed rubber stopper 10, convenient to connect with the fixture of stretching-machine.
Further, the inoperative section at the test button both ends that are stretched of first working electrode 1 passes through silicone rubber seal.
Further, the distance between second working electrode 4 and the first working electrode 1 are controlled by charge-coupled device
At 50 μm.
Further, the distance between the bottom end of the Luggin capillary 11 and the first working electrode 1 pass through charge-coupled device
Constant part is 2mm.
Further, the length of the platinum filament 8 is 1.5cm, diameter is 50 μm.
Further, the glass tube 6 is the quartz glass capillary of internal diameter 0.2cm, and thermal expansion coefficient should be with 8 phase of platinum filament
Closely, glass tube 6 is put into progress boiling cleaning in the concentrated sulfuric acid first before device is built, then passes through ultrapure water, will rush
Glass tube 6 after washing is placed on clean workbench and is dried for standby by Infrared irradiation.
Further, it is bonded with rubber pad at the areole for being inserted into the second working electrode 4, with liquid-leakage preventing, after insertion
Second working electrode 4 is sufficiently bonded with rubber pad.
The working principle of this monitoring device is as follows:
Tensile stress is applied to the test button that is stretched of the first working electrode 1, in the common of tensile stress and electrolyte solution
Under effect, cathodic polarization potential or anode polarization current potential E1 are applied to the first working electrode 1, stress corrosion occurs for metal,
During stress corrosion, cathodic polarization potential E2=-0.60V is applied to the second working electrode 4, at this time in the second working electrode 4
Upper generation H+The reaction being reduced,
H++ e → H (1),
2H→H2 (2)。
The current data collected by potentiostat is that the first working electrode 1 is generated at polarization potential E1 respectively
The reduction current that corrosion current and the second working electrode 4 are generated at -0.60V cathodic polarization potential E2, the reduction current pair
Answer H+It is reduced the electric current of generation, the dynamic change of the reduction current is microcell H+The dynamic change of concentration.Reduction current is exhausted
To bigger, the surveyed region H of value+Concentration is bigger.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change device, which is characterized in that
Including the first working electrode (1), first working electrode (1) is that both ends have the threaded I-shaped rodlike gold that is stretched
Belong to sample；
Second working electrode (4), second working electrode (4) is by being inserted into glass tube (6) behind platinum filament (8) and filamentary silver (7) welding
Middle composition, as platinum microelectrode；
Double potentiostat system electrolytic cell (9), the double potentiostat system electrolytic cell (9) are hollow cylindrical structure, the electricity
The first working electrode (1) is arranged in the axle center of Xie Chi (9), and the top surface of the electrolytic cell (9) plugs reference electrode (2) and auxiliary simultaneously
The side wall middle part of electrode (3), the electrolytic cell (9) is inserted with second working electrode vertical with the first working electrode (1)
(4)；
The reference electrode (2) is saturated calomel electrode, and the lower end of reference electrode (2) connects Luggin capillary (11), Lu Jinmao
The bottom end of tubule (11) extends in the middle part of the active section of the first working electrode (1)；
First working electrode (1), the second working electrode (4), reference electrode (2) and auxiliary electrode (3) pass through conducting wire respectively
It is connect with potentiostat, the screw thread at the test button both ends that are stretched of first working electrode (1) is connect with machine clamp is stretched.
2. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
The auxiliary electrode (3) is the platinized platinum of 20mm × 20mm.
3. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
Two rubber stoppers (10) are inserted at the test button both ends that are stretched of first working electrode (1) respectively, and threaded portion is complete
It is complete to expose rubber stopper (10).
4. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 3,
It is characterized in that,
The inoperative section at the test button both ends that are stretched of first working electrode (1) passes through silicone rubber seal.
5. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
The distance between second working electrode (4) and the first working electrode (1) control at 50 μm.
6. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
Constant the distance between the bottom end and the first working electrode (1) of the Luggin capillary (11) are 2mm.
7. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
The length of the platinum filament (8) is 1.5cm, diameter is 50 μm.
8. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
The glass tube (6) is the quartz glass capillary of internal diameter 0.2cm.
9. microcell pH value Monitoring on Dynamic Change device in a kind of metal stresses corrosion process median surface according to claim 1,
It is characterized in that,
It is bonded with rubber pad at areole for being inserted into the second working electrode (4), the second working electrode (4) and rubber after insertion
Rubber mat is sufficiently bonded.
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| CN110286036A (en) * | 2019-07-19 | 2019-09-27 | 佛山科学技术学院 | A kind of original position stretching and microcell electrochemistry synchronous testing device |
| CN110763874A (en) * | 2019-11-01 | 2020-02-07 | 江苏师范大学 | Method and device for researching metal stress corrosion dynamic process by monitoring pitting corrosion |
| CN111443124A (en) * | 2020-04-24 | 2020-07-24 | 常州大学 | Experimental device for stray current corrosion simulation and near-surface micro-area pH measurement |
| CN113567523A (en) * | 2020-04-29 | 2021-10-29 | 中国科学院海洋研究所 | Device and method for measuring pH value of electrode solution interface |
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