CN102560328A - Experiment method for carrying out hydrogen permeation on metal sample through electrochemical process - Google Patents
Experiment method for carrying out hydrogen permeation on metal sample through electrochemical process Download PDFInfo
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- CN102560328A CN102560328A CN 201010575189 CN201010575189A CN102560328A CN 102560328 A CN102560328 A CN 102560328A CN 201010575189 CN201010575189 CN 201010575189 CN 201010575189 A CN201010575189 A CN 201010575189A CN 102560328 A CN102560328 A CN 102560328A
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Abstract
The invention relates to an experiment method for carrying out electrolytic hydrogen permeation on a metal sample through an electrochemical process. A PS-12 type constant potential/constant current instrument is connected with an electrolytic tank to carry out electrochemical hydrogen permeation, the sample is put on the cathode of the electrolytic tank, a platinum sheet is an anode, an electrolyte is 1NH2SO4+0.25gNaASO2, and the hydrogen charging effect is relevant to the temperature, the hydrogen charging current density, the hydrogen charging time and the material of the sample in the hydrogen charging process. According to the invention, the best hydrogen charging current is 50mA, the hydrogen charging time is 150h, and the hydrogen charging temperature is room temperature. After the hydrogen charging, the sample is cleaned, and is put in a diffusible hydrogen analyzer to detect the diffusible hydrogen concentration, and other samples must be preserved in liquid nitrogen to reduce the overflow of hydrogen in the sample. By adopting the method of the invention, the highest diffusive hydrogen concentration of the metal sample can reach 6.3ppm.
Description
Technical field
What the present invention relates to is a kind of metal to be carried out the method that electrochemistry is oozed hydrogen, particularly the electrochemistry of heavy casting and forging metallic substance is oozed hydrogen, belongs to metallic substance, electrochemical field.
Background technology
In recent years, the heavy casting and forging manufacture level of China improves fast, and domestic heavy manufacturing concern has had world-class processing units and manufacturing capacity.Big Steel Castings is forged key components and parts and often is in working ordeies such as high temperature, high pressure, and quality directly has influence on the integral level and the serviceability of outfit.White point is the important factor in order of heavy casting and forging performance, and existence that it is generally acknowledged hydrogen and stress in the steel is to impel forging to form the major cause of white point, and when the hydrogen in the steel reached a certain content, the plasticity of steel significantly reduced, and impelled hydrogen embrittlement fully to show.When hydrogen richness surpasses 2cm
3During/100g (ppm), the plasticity of heavy casting and forging just almost completely disappears.The forge piece that general smelting, casting ingot method are produced, hydrogen richness is considerably beyond this limit.In the forge piece process of cooling, some is dissolved by the austenite that the line of segragation does not change to change hydrogen partly earlier, has increased the hydrogen richness of line of segragation.The austenite of line of segragation decomposes with the temperature reduction, and the Wasserstoffatoms that separate out this moment becomes hydrogen molecule, produces crunch; When this pressure can not be relaxed by the plasticity of steel, just make the steel part fragility and sclerosis occur, add the internal stress that forge piece when cooling produces if when being enough to make material damage; Position in this forge piece inside-line of segragation enriched hydrogen just produces tiny crack; And development is grown up thus, and after poor hydrogen zone was arrived in crack growth, stress was relaxed by the plasticity of steel; Crackle just stops to grow up, and forms white point.Confirm that the critical hydrogen richness of generation white point and the process method that expansion hydrogen to forge piece does not produce white point are significant to improving the forge piece performance.
Summary of the invention
The object of the invention is to provide a kind of method of utilizing electrochemical method that test button is oozed hydrogen, obtains the critical hydrogen richness that produces the heavy casting and forging white point through analyzing, and then optimizes thermal treatment and expand hydrogen technology, overcomes the hydrogen embrittlement defective of present heavy casting and forging.
Technical scheme of the present invention is:
Copper conductor on PS-12 type constant potential/galvanostat and the electrolyzer is linked to each other, test button is placed the negative electrode of electrolyzer, platinized platinum is an anode, utilizes the cathode effect of electrolytic process to make hydrogen get into metal inside.Testing used electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, ooze and ooze hydrogen effect and temperature, hydrogenation electric current density in the hydrogen process, ooze the hydrogen time and the sample material is relevant.Best hydrogenation electric current of the present invention is 50mA, and oozing the hydrogen time is 150h, and oozing the hydrogen temperature is room temperature.After oozing hydrogen, sample is cleaned the hydrogen concentration that places the diffusible hydrogen analyser to measure sample, for the hydrogen that reduces in the sample overflows, sample must place liquid nitrogen to preserve before the test hydrogen concentration.
Embodiment
Content in conjunction with the inventive method provides following three embodiment:
Embodiment 1:
Hydrogen is oozed in the electrolysis of YB70 (Cr5) steel
Be of a size of 30 * 15 * 5 YB70 steel sample through the 1000# sand papering with cutting, be placed on the negative electrode of electrolyzer with acetone and washed with de-ionized water, platinized platinum is an anode, and electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, connecting the potentiometer power supply, hydrogenation electric current is set is 40mA, and oozing the hydrogen time is 100h, and experiment is at room temperature carried out, and after oozing hydrogen and finishing sample is cleaned to place the diffusible hydrogen analyser to test hydrogen richness, and the hydrogen concentration that obtains in the sample is 5.4ppm.
Embodiment 2:
Hydrogen is oozed in the electrolysis of 34CrNi3Mo steel
To be of a size of 30 * 15 * 5 34CrNi3Mo steel sample through the 1000# sand papering and with after acetone and the washed with de-ionized water, and place electric tank cathode, platinized platinum is an anode, and electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, connect potentiometer, it is 50mA that hydrogenation electric current is set, and fills hydrogen time 150h, oozes the hydrogen experiment under the room temperature, after oozing hydrogen and finishing sample is cleaned to place the diffusible hydrogen analyser to test hydrogen richness, the hydrogen concentration that obtains sample is 6.3ppm.
Embodiment 3:
Hydrogen is oozed in the electrolysis of 30Cr2Ni4MoV steel
The 34Cr2Ni4MoV steel is cut into is of a size of 30 * 15 * 5 sample, sample places electric tank cathode with sample then through the 1000# sand papering and with acetone and washed with de-ionized water, and platinized platinum is an anode, and electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, connect potentiometer, it is 30mA that hydrogenation electric current is set, and fills hydrogen time 200h, oozes hydrogen under the room temperature, after oozing hydrogen and finishing sample is cleaned to place the diffusible hydrogen analyser to test hydrogen richness, the hydrogen concentration that obtains sample through test is 5.8 ppm.
Claims (3)
1. a test button electrochemistry is oozed the experimental technique of hydrogen, utilizes PS-12 type constant potential/galvanostat to connect electrolyzer and carries out electrochemistry and ooze hydrogen, and sample is placed the negative electrode of electrolyzer, and platinized platinum is an anode, and electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, fill fill in the hydrogen process hydrogen effect with temperature, fill the hydrogen current density, fill the hydrogen time and the sample material is relevant; It is 50mA that the best of the present invention is filled the hydrogen electric current, and filling the hydrogen time is 150h, and filling the hydrogen temperature is room temperature; After filling hydrogen, the clean diffusible hydrogen analyser that places of sample is surveyed the expansion hydrogen concentration, for the hydrogen that reduces in the sample overflows, other samples must place liquid nitrogen to preserve.
2. test button as claimed in claim 1 oozes hydrogen methods, it is characterized in that, adopts electrochemical method that metal is oozed hydrogen.
Test button as claimed in claim 1 ooze hydrogen methods, it is characterized in that electrolytic solution is 1NH
2SO
4+ 0.25gNaASO
2, it is 50mA that the best is filled the hydrogen electric current, and filling the hydrogen time is 150h, and filling the hydrogen temperature is room temperature.
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CN 201010575189 CN102560328A (en) | 2010-12-07 | 2010-12-07 | Experiment method for carrying out hydrogen permeation on metal sample through electrochemical process |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106226167A (en) * | 2016-08-10 | 2016-12-14 | 江苏大学 | A kind of measurement becomes the assay device of test button anti-hydrogen embrittlement performance under the conditions of prestressing force |
CN108893690A (en) * | 2018-06-13 | 2018-11-27 | 昆明理工大学 | A kind of silver-magnesium-nickel alloys refined crystalline strengthening method |
CN109975479A (en) * | 2017-12-28 | 2019-07-05 | 中核建中核燃料元件有限公司 | A kind of Gaseous hydrogenation device for the measurement of zirconium alloy pipe hydride orientation factor |
CN110530690A (en) * | 2019-07-24 | 2019-12-03 | 西安交通大学 | A kind of electrochemical cathode hydrogen filling method of metal and alloy sample |
CN110863170A (en) * | 2019-10-29 | 2020-03-06 | 中国船舶重工集团公司第七二五研究所 | α/nearly α titanium alloy hydrogen filling test method |
CN112630273A (en) * | 2020-12-30 | 2021-04-09 | 核工业西南物理研究院 | Electrochemical hydrogen permeation electrolytic cell in multi-atmosphere environment and application method thereof |
-
2010
- 2010-12-07 CN CN 201010575189 patent/CN102560328A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106226167A (en) * | 2016-08-10 | 2016-12-14 | 江苏大学 | A kind of measurement becomes the assay device of test button anti-hydrogen embrittlement performance under the conditions of prestressing force |
CN106226167B (en) * | 2016-08-10 | 2020-01-24 | 江苏大学 | Test device for measuring hydrogen brittleness resistance of metal sample under variable prestress condition |
CN109975479A (en) * | 2017-12-28 | 2019-07-05 | 中核建中核燃料元件有限公司 | A kind of Gaseous hydrogenation device for the measurement of zirconium alloy pipe hydride orientation factor |
CN108893690A (en) * | 2018-06-13 | 2018-11-27 | 昆明理工大学 | A kind of silver-magnesium-nickel alloys refined crystalline strengthening method |
CN110530690A (en) * | 2019-07-24 | 2019-12-03 | 西安交通大学 | A kind of electrochemical cathode hydrogen filling method of metal and alloy sample |
CN110863170A (en) * | 2019-10-29 | 2020-03-06 | 中国船舶重工集团公司第七二五研究所 | α/nearly α titanium alloy hydrogen filling test method |
CN112630273A (en) * | 2020-12-30 | 2021-04-09 | 核工业西南物理研究院 | Electrochemical hydrogen permeation electrolytic cell in multi-atmosphere environment and application method thereof |
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C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20120711 |