CN102323205A - Method for detecting hydrogen permeation current and hydrogen distribution at metal stress corrosion crack - Google Patents
Method for detecting hydrogen permeation current and hydrogen distribution at metal stress corrosion crack Download PDFInfo
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- CN102323205A CN102323205A CN201110132370A CN201110132370A CN102323205A CN 102323205 A CN102323205 A CN 102323205A CN 201110132370 A CN201110132370 A CN 201110132370A CN 201110132370 A CN201110132370 A CN 201110132370A CN 102323205 A CN102323205 A CN 102323205A
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Abstract
The invention relates to a metal corrosion research, in particular to a method for detecting a hydrogen permeation current and the hydrogen distribution at a metal stress corrosion crack, which comprises the following steps of: respectively drilling holes at positions on the side wall and at the bottom of a test sample, which are respectively at a distance of 0.2 to 0.5mm from the crack; using the drilled test sample as an anode tank; and then measuring the hydrogen permeation current and the hydrogen distribution at the crack by a Devanathan-Stachurski method. Due to the adoption of the method disclosed by the invention, the limitation that the conventional method cannot be suitable for a complex test sample with the crack and the like is overcome, not only the hydrogen permeation currents at the tip end and on the side wall of the metal stress corrosion crack can be detected, but also the basic can be provided for analysing a crack propagation mechanism.
Description
Technical field
The present invention relates to metal erosion research, is exactly the detection method that place, a kind of metal stresses corrosion cracking crack hydrogen infiltration electric current and hydrogen distribute specifically.
Background technology
Say that from the galvanochemistry angle metal erosion process is divided into anodic process and cathodic process.Anodic process is that metal loses the oxidized process of electronics, that is:
Fe-2e→Fe
2+
Cathodic process is that oxygenant obtains the process that electronics is reduced, and in most of corrosion environment, cathodic process is that oxygen or hydrogen or the two have the process that is reduced concurrently.In order to study the process that hydrogen is reduced in the metal erosion process, Devanathan-Stachurski has invented the electrochemical detection method of measuring the rate of diffusion of atomic hydrogen in the metal, is sheet but the Devanathan-Stachurski method requires test button.Metal stresses corrosion cracking crackle sidewall is considered to the cathodic area in the crackle, and the hydrogen that produces in the cathodic area diffuses to below the crackle sidewall, migrates to certain position of crack tip then, and the metal that causes crack tip ruptures with the mode of hydrogen embrittlement.
Summary of the invention
The object of the invention is to provide the detection method of place, a kind of metal stresses corrosion cracking crack hydrogen infiltration electric current and hydrogen distribution.
For realizing above-mentioned purpose, the present invention adopts technical scheme to be:
The detection method that a kind of metal stresses corrosion cracking crack place hydrogen infiltration electric current and hydrogen distribute: the hole of holing respectively apart from crackle 0.2-0.5mm place in the sidewall of sample and bottom; The back sample of will holing then utilizes the Devanathan-Stachurski method as the anode pond, promptly measures place, crack hydrogen infiltration electric current and hydrogen and distributes.
The described hole diameter is 8mm; Inwall plates palladium in the hole simultaneously.Said sample is a rectangular parallelepiped.
Advantage of the present invention is: adopt method of the present invention to overcome traditional measurement method and can not be applicable to the limitation that has complex samples such as crackle; Except can detecting metal stresses corrosion cracking crack tip and crackle sidewall hydrogen infiltration electric current, can also foundation be provided for analyzing crack propagation mechanism.Method of the present invention needs in advance metal to be holed, and operation is simple, can be applied to any test button with complicated shape.
Description of drawings
The variation diagram of the 1Cr18Ni9Ti stainless steel that Fig. 1 provides for the embodiment of the invention crack tip and crackle sidewall hydrogen infiltration current density under the drying and watering cycle sea conditions.
Fig. 2 contains FeCl for the 1Cr18Ni9Ti stainless steel that the embodiment of the invention provides in drying and watering cycle
3Acid seawater under the variation diagram of crack tip and crackle sidewall hydrogen infiltration current density.
The 1Cr18Ni9Ti stainless steel pre-flawed specimen boring synoptic diagram that Fig. 3 provides for the embodiment of the invention.
Embodiment
Embodiment 1
1. early-stage preparations; With the sidewall of rectangular parallelepiped 1Cr18Ni9Ti stainless steel sample and the bottom hole of holing respectively apart from crackle 0.2mm place; Make hole not penetrate sample; Then sample is placed in the exsiccator after overpickling, washing, acetone oil removing and dries naturally, and the welding upper conductor is as working electrode (referring to Fig. 3) on sample.
2. the plating palladium plates palladium in the hole of having bored, and plating palladium liquid is formulated by 0.8g/L palladium bichloride, 60g/LNaOH and redistilled water, and current density is 12mA/cm
2, 2 minutes time.
3. encapsulation electrolytic cell injects 0.2mol/LNaOH solution in plating the palladium sample aperture, draw the back sealing through two platinum filaments respectively, and wherein one as auxiliary electrode, and another root links to each other with the Hg/HgO contrast electrode.Respectively working electrode, contrast electrode, auxiliary electrode are received electrochemical workstation.
4. measure hydrogen infiltration electric current with the Devanathan-Stachurski method, before the experiment, experimental provision is placed constant temperature oven, (under the 150mV vs.Hg/HgO polarized potential) passivation in 0.2mol/LNaOH solution of plating palladium side is density stabilized until background current.On the stainless steel sample, apply certain pulling force; Drip seawater 0.5ml in cracks, the hydrogen that etchant solution and cracks metal generation electrochemical reaction produce is adsorbed in the crackle sidewall, because the hydrogen atom diameter is little; Can penetrate into metal inside; When the opposite side of hydrogen atom arrival crackle sidewall, when promptly being full of the hole of 0.2mol/LNaOH solution, because the oxidation of hole inwall plating palladium layer; Therefore hydrogen atom is oxidized to hydrogen ion, can detect hydrogen infiltration electric current and notes through electrochemical workstation.
5. hydrogen infiltration electric current is measured in drying and watering cycle, after cracks sea water solution drying, drips distilled water 0.5ml, repetitive process 4, (referring to Fig. 1).Later drying and watering cycle process all drips 0.5ml distilled water, carries out 5 drying and watering cycles.As can be seen from Figure 1, after dripping seawater, can both observe hydrogen infiltration electric current at crack tip and crackle sidewall in the sample cracks.Hydrogen infiltration electric current increases to a maximal value earlier, and the process that slowly reduces then is a drying and watering cycle process.In first three drying and watering cycle process; The detected hydrogen infiltration of crackle sidewall current density is all the time greater than the detected hydrogen infiltration in crack tip place current density; Since the 4th drying and watering cycle, crack tip place detected hydrogen infiltration current density begins to surpass the detected hydrogen infiltration of crackle side-walls current density.From development trend; The hydrogen infiltration electric current of crackle side-walls reaches maximal value when second drying and watering cycle; Though also extreme value can occur in the drying and watering cycle process afterwards; But all do not have to surpass the extreme value of second drying and watering cycle, be downward trend, explain that the hydrogen of crackle side-walls is mainly replenished by cracks metal and etchant solution reaction.And the hydrogen of crack tip infiltration electric current increases gradually; Even in the process of cracks etchant solution drying; Hydrogen infiltration electric current also increases; Explanation generates the hydrogen except etchant solution reacts at the crack tip place, and the hydrogen of other local generations of crackle also can move to the crack tip place, shows as the continuous increase of crack tip hydrogen infiltration electric current in the drawings.Under stress, the destruction of passivation film on stainless steel surface, will make between crackle front end and crackle two walls has bigger potential difference (PD), and hydrogen is moved to the crack tip place by the crackle sidewall gradually under the effect of potential difference (PD).Hydrogen is assembled at the crack tip place in a large number, and the crack tip metal is ruptured with the hydrogen embrittlement mode.
Embodiment 2
1. early-stage preparations; With the sidewall of rectangular parallelepiped 1Cr18Ni9Ti stainless steel sample and the bottom hole of holing respectively apart from crackle 0.2mm place; Make hole not penetrate sample, then sample is placed in the exsiccator after overpickling, washing, acetone oil removing and dries naturally, and the welding upper conductor is as working electrode on sample.
2. the plating palladium plates palladium in the hole of having bored, and plating palladium liquid is formulated by 0.8g/L palladium bichloride, 60g/LNaOH and redistilled water, and current density is 12mA/cm
2, 2 minutes time.
3. encapsulation electrolytic cell injects 0.2mol/LNaOH solution in plating palladium sample aperture, draw the back sealing through two platinum filaments respectively, and wherein one as auxiliary electrode, and another root links to each other with the Hg/HgO contrast electrode.Respectively working electrode, contrast electrode, auxiliary electrode are received electrochemical workstation.
4. measure hydrogen infiltration electric current with the Devanathan-Stachurski method, before the experiment, experimental provision is placed constant temperature oven, (under the 150mV vs.Hg/HgO polarized potential) passivation in 0.2mol/LNaOH solution of plating palladium side is density stabilized until background current.On the stainless steel sample, apply certain pulling force, (etchant solution comprises 0.1mol/LHCl, 0.06mol/LFeCl to drip etchant solution 0.5ml in cracks
3And seawater), the hydrogen that etchant solution and cracks metal generation evolving hydrogen reaction produce is adsorbed in the crackle sidewall, because the hydrogen atom diameter is little; Can penetrate into metal inside; When the opposite side of hydrogen atom arrival crackle sidewall, when promptly being full of the hole of 0.2mol/LNaOH solution, because the oxidation of hole inwall plating palladium layer; Therefore hydrogen atom is oxidized to hydrogen ion, can detect hydrogen infiltration electric current and notes through electrochemical workstation.
5. hydrogen infiltration electric current is measured in drying and watering cycle, after cracks etchant solution drying, drips distilled water 0.5ml, repetitive process 4.Later drying and watering cycle process all drips 0.5ml distilled water, carries out 5 drying and watering cycles (referring to Fig. 2).As can be seen from Figure 2, in first three drying and watering cycle process, the hydrogen of crack tip and crackle sidewall infiltration current density is more or less the same, and in same scope, changes.Since the 4th drying and watering cycle, the hydrogen of crack tip infiltration current density explains that apparently higher than the hydrogen infiltration current density of crackle sidewall the hydrogen of other local generations of crackle also can move to the crack tip place.And; Since the 4th drying and watering cycle, all the hydrogen infiltration electric current than first three drying and watering cycle is little at the detected hydrogen infiltration of crack tip electric current, still; More high than the detected hydrogen infiltration of crackle side-walls electric current, explain that a large amount of hydrogen moves to crack tip from the crackle sidewall.
Claims (3)
1. place, metal stresses corrosion cracking crack hydrogen permeates the detection method of electric current and hydrogen distribution; It is characterized in that: the hole of holing respectively apart from crackle 0.2-0.5mm place in the sidewall of sample and bottom; The back sample of will holing then utilizes the Devanathan-Stachurski method as the anode pond, promptly measures place, crack hydrogen infiltration electric current and hydrogen and distributes.
2. the detection method that distributes by place, the described metal stresses corrosion cracking of claim 1 crack hydrogen infiltration electric current and hydrogen, it is characterized in that: the described hole diameter is 8mm; Inwall plates palladium in the hole simultaneously.
3. the detection method that distributes by place, the described metal stresses corrosion cracking of claim 1 crack hydrogen infiltration electric current and hydrogen, it is characterized in that: said sample is a rectangular parallelepiped.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697924A (en) * | 2015-03-12 | 2015-06-10 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Device and method for determining hydrogen permeation current under ocean environment condition |
| CN104880400A (en) * | 2014-12-02 | 2015-09-02 | 浙江工业大学 | High pressure hydrogen penetration test device and method |
| CN105136596A (en) * | 2015-07-20 | 2015-12-09 | 西安科技大学 | Crack tip stress corrosion cracking situation test system and crack tip stress corrosion cracking situation test method having constant-displacement load |
| CN109187326A (en) * | 2018-09-25 | 2019-01-11 | 江苏师范大学 | Metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1983003007A1 (en) * | 1982-02-26 | 1983-09-01 | Arup, Hans | Method and device for determining hydrogen flux |
| CN2466637Y (en) * | 2001-03-09 | 2001-12-19 | 中国科学院海洋研究所 | Underwater deposit corrosion factor in-situ detecting device |
| CN101963569A (en) * | 2010-08-26 | 2011-02-02 | 长沙新中大环境科技有限公司 | Double-electrolyte digital sensor for detecting diffusion and permeation rate of atomic hydrogen in metal |
-
2011
- 2011-05-11 CN CN201110132370.7A patent/CN102323205B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1983003007A1 (en) * | 1982-02-26 | 1983-09-01 | Arup, Hans | Method and device for determining hydrogen flux |
| CN2466637Y (en) * | 2001-03-09 | 2001-12-19 | 中国科学院海洋研究所 | Underwater deposit corrosion factor in-situ detecting device |
| CN101963569A (en) * | 2010-08-26 | 2011-02-02 | 长沙新中大环境科技有限公司 | Double-electrolyte digital sensor for detecting diffusion and permeation rate of atomic hydrogen in metal |
Non-Patent Citations (1)
| Title |
|---|
| M. A. V. DEVANATHAN ET.: "A Technique for the Evaluation of Hydrogen Embrittlement Characteristics of Electroplating Baths", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104880400A (en) * | 2014-12-02 | 2015-09-02 | 浙江工业大学 | High pressure hydrogen penetration test device and method |
| CN104880400B (en) * | 2014-12-02 | 2017-06-27 | 浙江工业大学 | High Pressure Hydrogen pervasion test device and method of testing |
| CN104697924A (en) * | 2015-03-12 | 2015-06-10 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Device and method for determining hydrogen permeation current under ocean environment condition |
| CN105136596A (en) * | 2015-07-20 | 2015-12-09 | 西安科技大学 | Crack tip stress corrosion cracking situation test system and crack tip stress corrosion cracking situation test method having constant-displacement load |
| CN109187326A (en) * | 2018-09-25 | 2019-01-11 | 江苏师范大学 | Metal stresses corrosion process median surface microcell pH value Monitoring on Dynamic Change method |
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