CN104297145A - Electrochemical test method for researching influence of aerosol on atmosphere corrosion of metal material - Google Patents
Electrochemical test method for researching influence of aerosol on atmosphere corrosion of metal material Download PDFInfo
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- CN104297145A CN104297145A CN201310299125.4A CN201310299125A CN104297145A CN 104297145 A CN104297145 A CN 104297145A CN 201310299125 A CN201310299125 A CN 201310299125A CN 104297145 A CN104297145 A CN 104297145A
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Abstract
The invention relates to an electrochemical test method of atmosphere corrosion of a metal material and particularly provides the electrochemical test method for researching influence of an aerosol on the atmosphere corrosion of the metal material. In the method, micro-distance electrode probes with an electrode distance being not more than 10[mu]m are employed. A medium generating the aerosol includes various single-components salt solutions and double-component mixed salt solutions. Each solution, in the form of the aerosol and through an aerosol generator, is individually deposited on a set of micro-distance galvanic couple electrodes and micro-distance double-electrode probes and is dried, wherein a depositing amount is based on the depositing amount in a real marine atmosphere environmental. The double-electrode probes, with the aerosol deposited thereon, are placed into environments having different relative humidity, and then galvanic couple currents and electrochemical impedances are measured after the system is stable. The invention provides a research method for atmosphere corrosion of metal in an electrochemical manner, which can obtain electrochemical information during a corrosion process conveniently and quickly and allows influences of atmosphere corrosion of properties of the aerosol on the metal to be known.
Description
Technical field
The present invention relates to the atmospheric corrosion Electrochemical Measurement Technology of metal material, be specially a kind of electrochemical test method studied gasoloid and atmospheric corrosion of metal materials is affected.
Technical background
In atmospheric corrosion to metal erosion behavioral implications the most serious surely belong to sea salt particle, especially to the easily passive metal such as aluminium, stainless steel, so the corrosion behavior of metal material attracts most attention under naval air environment always.But because typical naval air environment average relative humidity is higher, people's more attention is the impact of Cl-under high humility, have ignored some physicochemical properties of sea salt particle itself in air to the impact of metal erosion behavior.No matter sea salt particle or other atmosphere pollutions, mainly exist with aerosol form, its particle size range is from 10
-3μm-100 μm, deposit to metal surface by gravity settling or other modes with aerosol form and then affect its corrosion behavior.The particle diameter of marine aerosol generally distributes at about one micron to some tens of pm, and after moisture absorption, particle diameter can reach original 1 ~ 2 times.Because of its particle diameter and composition characteristic, gasoloid has the characteristic being much different from tank solution or bulky grain particle.As in gasoloid particle size range, gas (as the oxygen) diffusion in drop is very fast, there will not be obvious concentration gradient; In addition, its moisture absorption or crystallization behavior are also obviously different from bulky grain or tank solution, for marine aerosol, in its moisture absorption or crystallization process, can form high ion concentration, as Cl in drop
-, and then can corrosion of metal be accelerated, especially to Al and Alalloy or stainless steel.Moreover, because the special moisture absorption of gasoloid or crystallization behavior, obviously can extend the time that aerosol liquids state exists, then can increase the wetting time of metal surface, effective etching time of metal is lengthened.
But up to the present, the impact of aerocolloidal special physico-chemical character on corrosion does not also cause the special concern of corrosion circle scholar, only has minority scholar to be studied from particle diameter angle.One of its reason lacks gasoloid preparation and detection means, be corroded the restriction of behavioral study method, foregoing a few studies achievement mainly infers corrosion mechanism by observing erosion profile under scanning electron microscope, because the making of microelectrode is more difficult, electrochemical means rarely have people to attempt.Under second focus being current atmospheric corrosion circle is paid close attention to mainly concentrates on ocean and industrial atmospheric environment, these areas have higher relative humidity mostly, mask the impact that aerocolloidal character causes to a certain extent.
Summary of the invention
The object of the present invention is to provide a kind of electrochemical test method studied gasoloid and atmospheric corrosion of metal materials is affected.
Technical scheme of the present invention is:
A kind of electrochemical test method studied gasoloid and atmospheric corrosion of metal materials is affected, the method is deposited on by salt solusion on the workplace of macro electrodes probe in the form of an aerosol, on workplace, the salt particle of deposition is formed after drying, tested in the environmental cabinet of different relative humidity by the macro electrodes probe depositing aerosol salt particle, Galvanic Current and electrochemical impedance are measurement parameter; Described macro electrodes probe refers to the probe of interelectrode distance≤10 of adjacent metal μm; Described gasoloid be by aerosol generator by salt solusion with microfluidic aerosol drops and disperse discontinuous state be deposited on macro electrodes probe workplace on.
Described different relative humidity adopts different saturated salt solution to control, or adopts the mixed solution of different saturated salt solution and organic solution to control.
Described salt solusion is single component salt solusion, bi-component salt solusion or polycomponent salt solusion.
Each electrode of described macro electrodes probe can select same metal material parallel to place, or, select the parallel placement that two kinds of different metal materials are alternately arranged; Electrode metal material used and size carry out selection adjustment according to test condition.
Form salt particle after the crystallization of described microfluidic aerosol droplet drying and be of a size of 5 ~ 20 μm, occupying the majority of tens microns.
Advantage of the present invention and beneficial effect are:
(1) the invention provides a kind of electrochemical means to study the impact of gasoloid on atmospheric corrosion, some information in acquisition electrochemical process easier than conventional method in the past, and convenient and swift.
(2) have employed the macro electrodes probe of electrode separation≤10 μm in the present invention, its spacing is consistent with the aerocolloidal particle diameter of sea salt particle, the metal electrode (as shown in Figure 3) of insulation clearance both sides can be connected after salt particle moisture absorption, ensure effective measurement of electrochemical signals.
(3) aerosol generator is passed through, the salt particle particle diameter deposited can be made mainly to be distributed between 5 ~ 20 μm, consistent with ocean particle gasoloid, and in discontinuously arranged uniformly, the salt particle particle that the mineralization mode in the past that avoids causes problem that is comparatively large or that distribute in flakes.
(4) macro electrodes probe and being combined of aerosol generator, makes just can monitor obvious galvanic corrosion signal when a small amount of salt particle of deposition.This deposition closer to the deposition in the true atmospheric environment in open air, as naval air environment.
(5) have employed mixing salt solution in the present invention as aerocolloidal generation medium, closer to the situation in true environment.Gasoloid in physical environment is substantially all polycomponent.
(6) in the present invention in order to obtain a series of relative humidity conditions be more or less the same in less RH range, the mixed solution that have employed saturated salt solution and organic solution carries out relative humidity control, this relative humidity control mode is easy to operate, and more accurate, more stable.
Accompanying drawing explanation
Fig. 1 is the present invention's macro electrodes sonde configuration used schematic diagram.
Fig. 2 is the drawing in side sectional elevation of Fig. 1 macro electrodes sonde configuration.
Fig. 3 is pattern after probe spacing and aerosol deposition; In figure: (a) probe spacing; Pattern after (b) aerosol deposition.
Fig. 4 is Galvanic Current change curve (NaCl) under different relative humidity.
Fig. 5 is (the NaCl & NH of Galvanic Current curve under different relative humidity
4cl).
Fig. 6 is results of AC impedance (NaCl) under different relative humidity.
Fig. 7 is (the NaCl & NH of results of AC impedance under different relative humidity
4cl).
Embodiment
Below by way of drawings and Examples in detail the present invention is described in detail.
The present invention establishes a kind of electrochemical test method studied gasoloid and affect atmospheric corrosion of metal materials.
Be specially a kind of electrochemical test method studied gasoloid and atmospheric corrosion of metal materials is affected.The method is adopted as the macro electrodes probe of electrode separation≤10 μm, generating aerocolloidal medium is single component, bi-component or polycomponent salt solusion, with aerosol generator, often kind of solution is deposited on the workplace of macro electrodes probe in the form of an aerosol, and dry (deposition with the deposition under true naval air environment for benchmark), on workplace, form the salt particle (as shown in Figure 3) of deposition after drying; Afterwards the electrode probe depositing salt particle is put into different relative humidity conditions, after stable, measure Galvanic Current and electrochemical impedance respectively.
The electrode probe adopted in the present invention has plurality of specifications, and the salt solusion of employing also has multiple combination, and wherein a kind of macro electrodes sonde configuration design as depicted in figs. 1 and 2.
This macro electrodes probe comprises: several metal electrodes 1 of parallel placement, are anchored on the wire 2 on metal electrode, plays the epoxy resin 3 of insulating effect, probing shell 4 for package metals electrode and wire.Shell 4 for the protection of probe needs to have some strength (optional PVC material), and shape is upper and lower both ends open tubular structure, according to operating mode, can select pipe or other polygon pipes; Spacing between the adjacent metal electrode 1 of parallel placement is≤10 μm (in figure distances shown in A), and the upper surface of metal electrode 1 will be unified to be exposed to as workplace outside epoxy resin 3, and the lower surface of metal electrode 1 encapsulates in the inner by epoxy resin 3; One end of wire 2 will independently be connected in each metal electrode 1, the other end then picks out from the reverse direction of workplace or the side of shell, wire 2 must not be in the same plane with the workplace of metal electrode 1, fully insulate with epoxy resin between other wires that metal electrode and not being attached thereto connects, must not short circuit; Epoxy resin 3 used will ensure that mobility is enough good, guarantees to solidify between rear different metal electrode fully to insulate, and must not leave micropore and gap etc.; Also good insulation will be kept between probing shell 4 and metal electrode 1 and wire 2.
The quantity of metal electrode 1 and size can be selected according to actual test conditions, are not limited to two electrodes (but must be more than or equal to two) shown in figure, as required can parallel placement of multiple layers metal electrode film; Simultaneously under the prerequisite of handled easily, the size of its workplace also can be selected as required.In addition, the material of metal electrode 1 can experimentally need to select various metal material.According to the difference measuring electrochemical signals, same metal material parallel can be selected to place, also can select the parallel placement that two kinds of metal materials not of the same race are alternately arranged.As required, metal material can select the sheet material commonly used, and also can select metal forming.The connection of wire 2 should ensure same group of good contact between wire and sheet metal, keeps the abundant insulation between different group wire and sheet metal again, must not short circuit.Epoxy resin 3 used must have excellent mobility when encapsulating, and guarantees the abundant insulation of solidifying between rear different conductor and metal electrode, must not leave micropore and gap.Protecting sheathing 4 is under the prerequisite with some strength, and its material and shape can be selected according to actual condition, are not limited to the shape shown in Fig. 1.
The galvanic couple of microspur described in following examples electrode refers to as structure shown in Fig. 1 and Fig. 2, and pop one's head in as Cu-Al galvanic couple electrode, single-layer metal sheet sectional dimension is 3.0cm × 1.5mm, and two panels, is spaced apart between electrode slice and is less than or equal to 10 μm altogether.Described microspur bipolar electrode probe refers to structure shown in Fig. 1 and Fig. 2, and be Al bipolar electrode probe, for the measurement of EIS, Al electrode metal sheet sectional dimension is 3.0cm × 1.5mm, and material is commercial-purity aluminium, is wherein spaced apart between Al electrode and is less than or equal to 10 μm.
Following examples utilize WDB-5A type aerosol generator to prepare particulate.
Aerocolloidal generation medium selects saturated NaCl solution, or saturated NaCl solution and saturated NH
4the mixed solution of Cl.
Different relative humidity controls by adopting the mixed solution of different saturated salt solution and different saturated salt solution and organic solution.
The measurement of embodiment 1(Galvanic Current)
First the particulate of single component (NaCl solution) is deposited on Cu-Al galvanic couple electrode surface, after drying, under putting it into its critical moisture absorption relative humidity (76%) environment, measures the change of Galvanic Current.Select slightly lower than the environment of critical moisture absorption relative humidity (being about 72%), repeat said process.Then by blending constituent (saturated NaCl solution and saturated NH
4the mixed solution of Cl) particulate be deposited on Cu-Al galvanic couple electrode surface, after drying, under being placed on lower relative humidity conditions equally (72% and 65%), measure the change of Galvanic Current.Measurement result is shown in Fig. 4 and Fig. 5.
As seen from Figure 4, when the critical moisture absorption point of NaCl (76%RH), there is high value in Galvanic Current, and this facilitates the carrying out of corrosion process after NaCl moisture absorption is described.On the contrary, when slightly critical lower than NaCl moisture absorption point, current value is extremely low, consider the performance of experimental facilities itself, can think, at this moment current value and ground unrest, at an order of magnitude, illustrate that electrode surface does not occur to detect the corrosion behavior obtained, and also illustrate that obvious moisture absorption behavior does not occur the deposition salt of electrode surface.Fig. 5 then shows deposition salt-mixture (NaCl and NH
4cl) the Galvanic Current change of ACM electrode probe when 72%RH and 65%RH, similar when its rule and separately deposition NaCl, when 72%RH, corrosion current value is more obvious, then can't detect obvious electric current during 65%RH, illustrate that combination gas colloidal sol is there occurs obvious moisture absorption lower than during the respective critical moisture absorption point of its blending constituent.(note: NH
4the critical moisture absorption of Cl o'clock about 78%, higher than the critical moisture absorption point of NaCl.）
The measurement of embodiment 2(electrochemical impedance)
The particulate (NaCl) of single component is deposited on microspur bipolar electrode detecting head surface, after drying, under putting it into critical moisture absorption relative humidity conditions (with embodiment 1), measures the change of its EIS in different time.Select the environment (being about 72%) lower than critical moisture absorption relative humidity, repeat said process.Then (saturated NaCl solution and saturated NH will be mixed
4the mixed solution of Cl) particulate be deposited on microspur bipolar electrode surface, after drying, under being placed on lower relative humidity conditions (with embodiment 1), measure the change of EIS.Measurement result is shown in Fig. 6 and Fig. 7.
Deposition single component NaCl bipolar electrode probe its critical moisture absorption point (76%RH) and comparatively low relative humidity (72%RH) time impedance spectrum as shown in Figure 6.When lower than critical relative moisture, Nyquist figure shows as a great capacitive reactance arc of radius, and extend in time and substantially do not change.This illustrates that deposition salt does not have moisture absorption, and do not have conducting between bipolar electrode, electrode surface is dry state, and EIS spectrogram now shows the feature of electrode self.When critical relative moisture, electrode surface still shows as single capacitive reactance arc, but its radius has obvious reduction, describes the deposition salt moisture absorption of electrode surface.Deposition salt-mixture (NaCl and NH
4cl) the impedance spectrum situation of change of bipolar electrode probe when 72%RH and 65%RH is shown in Fig. 7.Similar when its result and single component mineralization.The change of impedance spectrum also illustrates that combination gas colloidal sol is there occurs obvious moisture absorption lower than during the respective critical moisture absorption point of its blending constituent.
By embodiment 1 and embodiment 2 known, adopt this kind of method all to obtain stable Electrochemistry Information, describe the rationality of scheme, also demonstrate the reliability of adopted electrode probe.And the implementation case demonstrates salt-mixture particle gasoloid and has lower critical moisture absorption relative humidity, and under same experimental situation, the wetting time that it causes metal material surface than single component gasoloid is longer, extends etching time.In addition, the moisture absorption under low relative humidity of combination gas colloidal sol can form the microlayer model of high ion concentration, is degrading corrosion environment further.The present invention can be used to research some physicochemical property aerocolloidal to the impact of atmospheric corrosion of metal materials behavior, can carry out Real-Time Monitoring further under natural atmosphere environment to atmospheric corrosion.
Claims (5)
1. the electrochemical test method studied gasoloid and atmospheric corrosion of metal materials is affected, it is characterized in that: the method is deposited on by salt solusion on the workplace of macro electrodes probe in the form of an aerosol, on workplace, the salt particle of deposition is formed after drying, tested in the environmental cabinet of different relative humidity by the macro electrodes probe depositing salt particle, Galvanic Current and electrochemical impedance are measurement parameter; Described macro electrodes probe refers to the probe of interelectrode distance≤10 of adjacent metal μm; Described gasoloid be by aerosol generator by salt solusion with microfluidic aerosol drops and disperse discontinuous state be deposited on macro electrodes probe workplace on.
2. the electrochemical test method that affects atmospheric corrosion of metal materials of research gasoloid according to claim 1, is characterized in that: described different relative humidity adopts different saturated salt solution to control; Or different relative humidity adopts the mixed solution of different saturated salt solution and organic solution to control.
3. the electrochemical test method that affects atmospheric corrosion of metal materials of research gasoloid according to claim 1, is characterized in that: described salt solusion is single component salt solusion, bi-component salt solusion or polycomponent salt solusion.
4. research gasoloid according to claim 1 electrochemical test method that atmospheric corrosion of metal materials is affected, it is characterized in that: each electrode of described macro electrodes probe can select same metal material parallel to place, or, select the parallel placement that two kinds of different metal materials are alternately arranged; Electrode metal material used and size carry out selection adjustment according to test condition.
5. the electrochemical test method that affects atmospheric corrosion of metal materials of research gasoloid according to claim 1, is characterized in that: form salt particle after the crystallization of described microfluidic aerosol droplet drying and be of a size of 5 ~ 20 μm, occupying the majority of tens microns.
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Cited By (6)
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| CN105004770A (en) * | 2015-07-02 | 2015-10-28 | 国家电网公司 | Electrochemical sensor used for atmosphere corrosive monitoring, and application method thereof |
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| CN106468651A (en) * | 2016-09-22 | 2017-03-01 | 国网山东省电力公司电力科学研究院 | A kind of atmospheric corrosiveness on-line monitoring system and its method |
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| CN108896475A (en) * | 2018-08-28 | 2018-11-27 | 北京科技大学 | A kind of salt fog that simulating multi-environment factor/ultraviolet coupling accelerated test method |
| CN109765172A (en) * | 2019-04-04 | 2019-05-17 | 中国船舶重工集团公司第七二五研究所 | A kind of metal and coating material sea atmosphere corrosion in-situ measurement device and method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004770A (en) * | 2015-07-02 | 2015-10-28 | 国家电网公司 | Electrochemical sensor used for atmosphere corrosive monitoring, and application method thereof |
| CN105466823A (en) * | 2016-01-14 | 2016-04-06 | 中国科学院金属研究所 | Test method for simulating deposition of aerosol on surface of sample |
| CN106468651A (en) * | 2016-09-22 | 2017-03-01 | 国网山东省电力公司电力科学研究院 | A kind of atmospheric corrosiveness on-line monitoring system and its method |
| CN108169297A (en) * | 2017-12-12 | 2018-06-15 | 广西电网有限责任公司电力科学研究院 | A kind of atmospheric corrosiveness monitoring sensor and preparation method thereof |
| CN108896475A (en) * | 2018-08-28 | 2018-11-27 | 北京科技大学 | A kind of salt fog that simulating multi-environment factor/ultraviolet coupling accelerated test method |
| CN108896475B (en) * | 2018-08-28 | 2024-07-05 | 北京科技大学 | Salt fog/ultraviolet coupling acceleration test method for simulating multiple environmental factors |
| CN109765172A (en) * | 2019-04-04 | 2019-05-17 | 中国船舶重工集团公司第七二五研究所 | A kind of metal and coating material sea atmosphere corrosion in-situ measurement device and method |
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