CN102323205B - 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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- CN102323205B CN102323205B CN201110132370.7A CN201110132370A CN102323205B CN 102323205 B CN102323205 B CN 102323205B CN 201110132370 A CN201110132370 A CN 201110132370A CN 102323205 B CN102323205 B CN 102323205B
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- hydrogen
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- electric current
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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 of a kind of metal stresses corrosion cracking crack place hydrogen infiltration electric current and olefin hydrogen specifically.
Background technology
From galvanochemistry angle, Process of Metallic Corrosion 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 the process that oxygenant obtains electronics and is reduced, in most of corrosion environment, cathodic process be oxygen or hydrogen or the two have the process be reduced concurrently.In order to study the process that hydrogen in Process of Metallic Corrosion is reduced, Devanathan-Stachurski has invented the electrochemical detection method of the rate of diffusion measuring metal Atom hydrogen, but Devanathan-Stachurski method requires that test button is sheet.Metal stresses corrosion cracking crackle sidewall is considered to the cathodic area in crackle, and the hydrogen trap produced in cathodic area, to crackle sidewall, then migrates to certain position of crack tip, causes the metal of crack tip to rupture in the mode of hydrogen embrittlement.
Summary of the invention
The object of the invention is the detection method providing a kind of metal stresses corrosion cracking crack place hydrogen infiltration electric current and olefin hydrogen.
For achieving the above object, the present invention adopts technical scheme to be:
The detection method of a kind of metal stresses corrosion cracking crack place hydrogen infiltration electric current and olefin hydrogen: hole of holing respectively apart from crackle 0.2-0.5mm place in the sidewall of sample and bottom, sample after boring is then utilized Devanathan-Stachurski method as anode pool, namely measures crack place hydrogen infiltration electric current and olefin hydrogen.
Described hole diameter is 8mm; Simultaneously at hole inwall plating palladium.Described sample is rectangular parallelepiped.
Advantage of the present invention is: the limitation adopting method of the present invention to overcome traditional measurement method can not to be applicable to complex samples such as crackles, except can detecting metal stresses corrosion cracking crack tip and crackle sidewall hydrogen infiltration electric current, foundation can also be provided for analyzing crack propagation mechanism.Method of the present invention needs to hole to metal in advance, and operation is simple, can be applied to any test button with complicated shape.
Accompanying drawing explanation
The variation diagram of 1Cr18Ni9Ti stainless steel crack tip and crackle sidewall hydrogen infiltration current density under drying and watering cycle sea conditions that Fig. 1 provides for the embodiment of the present invention.
The 1Cr18Ni9Ti stainless steel that Fig. 2 provides for the embodiment of the present invention contains FeCl in drying and watering cycle
3acid seawater under crack tip and crackle sidewall hydrogen infiltration current density variation diagram.
The 1Cr18Ni9Ti stainless steel pre-flawed specimen boring schematic diagram that Fig. 3 provides for the embodiment of the present invention.
Embodiment
Embodiment 1
1. early-stage preparations, to be holed respectively apart from crackle 0.2mm place in the sidewall of rectangular parallelepiped 1Cr18Ni9Ti stainless steel sample and bottom hole, hole is made not penetrate sample, then sample is placed in exsiccator and naturally dries after overpickling, washing, acetone oil removing, sample welds upper conductor as working electrode (see Fig. 3).
2. plate palladium, in the hole of having bored, plate palladium, 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. encapsulate electrolytic cell, inject 0.2mol/LNaOH solution plating in palladium sample aperture, sealing after drawing respectively by two platinum filaments, wherein one as auxiliary electrode, and another root is connected with Hg/HgO contrast electrode.Respectively working electrode, contrast electrode, auxiliary electrode are received electrochemical workstation.
4. measure hydrogen infiltration electric current by Devanathan-Stachurski method, before experiment, experimental provision is placed in constant temperature oven, plating palladium side in 0.2mol/LNaOH solution (under 150mV vs.Hg/HgO polarized potential) passivation until background current is density stabilized.Stainless steel sample applies certain pulling force, seawater 0.5ml is dripped in cracks, the hydrogen that etchant solution and cracks metal generation electrochemical reaction produce is adsorbed in crackle sidewall, because hydrogen atom diameter is little, metal inside can be penetrated into, when hydrogen atom arrives the opposite side of crackle sidewall, when being namely full of the hole of 0.2mol/LNaOH solution, due to the oxidation of hole inwall plating palladium layers, hydrogen atom is oxidized to hydrogen ion, therefore, it is possible to hydrogen infiltration electric current detected by electrochemical workstation and record.
5. hydrogen infiltration electric current is measured in drying and watering cycle, when after the drying of cracks sea water solution, drips distilled water 0.5ml, repetitive process 4, (see 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 in sample cracks, hydrogen infiltration electric current can be observed at crack tip and crackle sidewall.Hydrogen infiltration electric current first increases to a maximal value, and the process then slowly reduced is a drying and watering cycle process.In first three drying and watering cycle process, the hydrogen infiltration current density that crackle sidewall detects is greater than the hydrogen infiltration current density that crack tip place detects all the time, from the 4th drying and watering cycle, the hydrogen infiltration current density that crack tip place detects begins to exceed the hydrogen infiltration current density that crackle side-walls detects.From development trend, the hydrogen infiltration electric current of crackle side-walls reaches maximal value when second drying and watering cycle, although also there will be extreme value in drying and watering cycle process afterwards, but all not more than the extreme value of second drying and watering cycle, in downward trend, illustrate that the hydrogen of crackle side-walls is mainly obtained by reacting supplementary by cracks metal and etchant solution.And the hydrogen infiltration electric current of crack tip increases gradually, even in the process of cracks etchant solution drying, hydrogen infiltration electric current is also increase, illustrate except etchant solution is except crack tip place reacts generation hydrogen, the hydrogen of the generation in other places of crackle also can move to crack tip place, shows as the continuous increase of crack tip hydrogen infiltration electric current in the drawings.Under effect of stress, the destruction of passivation film on stainless steel surface, will make there is larger potential difference (PD) between crackle front end and crackle two wall, hydrogen moves to crack tip gradually by crackle sidewall under the effect of potential difference (PD).Hydrogen is assembled in a large number at crack tip place, and crack tip metal can be made to rupture in hydrogen embrittlement mode.
Embodiment 2
1. early-stage preparations, to be holed respectively apart from crackle 0.2mm place in the sidewall of rectangular parallelepiped 1Cr18Ni9Ti stainless steel sample and bottom hole, make hole not penetrate sample, then sample is placed in exsiccator and naturally dries after overpickling, washing, acetone oil removing, sample welds upper conductor as working electrode.
2. plate palladium, in the hole of having bored, plate palladium, 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. encapsulate electrolytic cell, in plating palladium sample aperture, inject 0.2mol/LNaOH solution, sealing after drawing respectively by two platinum filaments, wherein one as auxiliary electrode, and another root is connected with Hg/HgO contrast electrode.Respectively working electrode, contrast electrode, auxiliary electrode are received electrochemical workstation.
4. measure hydrogen infiltration electric current by Devanathan-Stachurski method, before experiment, experimental provision is placed in constant temperature oven, plating palladium side in 0.2mol/LNaOH solution (under 150mV vs.Hg/HgO polarized potential) passivation until background current is density stabilized.Stainless steel sample applies certain pulling force, and (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 crackle sidewall, because hydrogen atom diameter is little, metal inside can be penetrated into, when hydrogen atom arrives the opposite side of crackle sidewall, when being namely full of the hole of 0.2mol/LNaOH solution, due to the oxidation of hole inwall plating palladium layers, hydrogen atom is oxidized to hydrogen ion, therefore, it is possible to hydrogen infiltration electric current detected by electrochemical workstation and record.
5. hydrogen infiltration electric current is measured in drying and watering cycle, when after the drying of cracks etchant solution, 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 (see Fig. 2).As can be seen from Figure 2, in first three drying and watering cycle process, the hydrogen infiltration current density of crack tip and crackle sidewall is more or less the same, and changes in same scope.From the 4th drying and watering cycle, the hydrogen infiltration current density of crack tip, apparently higher than the hydrogen infiltration current density of crackle sidewall, illustrates that the hydrogen of the generation in other places of crackle also can move to crack tip place.And, from the 4th drying and watering cycle, the hydrogen infiltration electric current detected at crack tip is all little than the hydrogen infiltration electric current of first three drying and watering cycle, but, the hydrogen infiltration electric current detected than crackle side-walls is high, illustrates that a large amount of hydrogen moves to crack tip from crackle sidewall.
Claims (2)
1. the detection method of metal stresses corrosion cracking crack place hydrogen infiltration electric current and olefin hydrogen, it is characterized in that: in hole of holing respectively apart from crackle 0.2-0.5mm place with the sidewall of precracked specimen and bottom, sample behind described boring hole is then utilized Devanathan-Stachurski method as anode pool, detect metal stresses corrosion cracking crack tip and crackle sidewall hydrogen infiltration electric current, namely measure crack place hydrogen infiltration electric current and olefin hydrogen;
Described hole diameter is 4-8mm; In described hole, plate palladium, plating palladium liquid is formulated by 0.8g/L palladium bichloride, 60g/L NaOH and redistilled water, and current density is 12mA/cm
2, the time is 2 minutes.
2. permeate the detection method of electric current and olefin hydrogen by metal stresses corrosion cracking crack according to claim 1 place hydrogen, it is characterized in that: described sample is rectangular parallelepiped.
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| CN201110132370.7A CN102323205B (en) | 2011-05-11 | 2011-05-11 | Method for detecting hydrogen permeation current and hydrogen distribution at metal stress corrosion crack |
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| CN102323205B true CN102323205B (en) | 2015-03-18 |
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| 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 |
| CN105136596B (en) * | 2015-07-20 | 2017-11-17 | 西安科技大学 | Sharp stress corrosion cracking state verification system and method is split with permanent 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| JPS59500063A (en) * | 1982-02-02 | 1984-01-12 | エルハオス，フリ−ドリツヒ ヴイルエルム | Preheating furnace for long materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| A Technique for the Evaluation of Hydrogen Embrittlement Characteristics of Electroplating Baths;M. A. V. Devanathan et.;《Journal of The Electrochemical Society》;19631231;第110卷(第8期);第886-890页 * |
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