CN104034762A - Multichannel hydrogen measuring device and method used for hydrogen permeation behavior of metallic material - Google Patents
Multichannel hydrogen measuring device and method used for hydrogen permeation behavior of metallic material Download PDFInfo
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- CN104034762A CN104034762A CN201410225714.2A CN201410225714A CN104034762A CN 104034762 A CN104034762 A CN 104034762A CN 201410225714 A CN201410225714 A CN 201410225714A CN 104034762 A CN104034762 A CN 104034762A
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Abstract
The invention discloses a multichannel hydrogen measuring device and a multichannel hydrogen measuring method used for hydrogen permeation behavior of a metallic material. The device comprises a sample, a reference electrode, an auxiliary electrode, a cathode tank, anode tanks and a multichannel potentiostat, wherein the cathode tank is in a barrel-shaped structure of which the top is open; the anode tanks are in cylinder-shaped structures of which the tops and bottoms are open, the cathode tank, the sample and the anode tanks are sequentially and vertically arranged from the bottom to top, wherein the reference electrode and the auxiliary electrode are vertically arranged in the cathode tank and are connected with corresponding channels of the potentiostat respectively through wires passing through a seal reference electrode fixing hole and a seal auxiliary electrode fixing hole formed in one side of the cathode tank; the anode tanks are uniformly distributed in the upper plane of the sample; the auxiliary electrodes and the reference electrodes are arranged in the anode tanks, wires of the auxiliary electrodes and the reference electrodes are respectively connected with corresponding channels of the potentiostat; the sample is connected with corresponding channel of the potentiostat through a wire. By adopting the multichannel hydrogen measuring device, as multichannel electrolysis tank technology is adopted, hydrogen permeation behaviors of multiple parts of the metallic material can be simultaneously measured, and the multichannel hydrogen measuring device is simple to operate, low in cost and high in precision.
Description
Technical field
The invention belongs to field of measuring technique, relate to a kind of hyperchannel hydrogen-measuring apparatus and method for metal material hydrogen permeation behavior.The present invention, by setting up the hydrogen infiltration electric current of the multiple local locations of hyperchannel Devnathan-Stachurski (D-S) electrolytic cell measuring metallic materials, reaches the object of research material local organization difference to hydrogen infiltration current affects in conjunction with metallographic method simultaneously.
Background technology
Can there is evolving hydrogen reaction in metal material, the metal inside that hydrogen atom is diffused into crack tip becomes fragile this region in corrosion process, brittle fracture occurs under effect of stress and then affect the structural safety of metal material.The single channel D-S double-electrolyzer device and method that has all followed Devnathan-Stachurski employing for this present situation most researcher comes measuring metallic materials chemical composition and the impact of thermal treatment on hydrogen permeation behavior, owing to cannot obtaining the hydrogen infiltration electric current of the multiple local locations of material in this device one-shot measurement process, and then cause for histological difference very few on the research of metal material hydrogen permeation behavior impact.
The present invention is improved on forefathers' basis, measures the hydrogen infiltration electric current of the multiple local locations of material in equivalent environment by setting up hyperchannel D-S electrolytic cell, thereby and reaches the object of research material histological difference on hydrogen permeation behavior impact in conjunction with metallographic method.
Summary of the invention
The object of the invention is the defect existing for prior art, provide a kind of for studying hyperchannel hydrogen-measuring apparatus and the method for metal material hydrogen permeation behavior.The present invention be by set up hyperchannel Devnathan-Stachurski (D-S) electrolytic cell with reach once can the multiple local locations of measuring metallic materials hydrogen infiltration electric current, reach the object of research material local organization difference to hydrogen infiltration current affects in conjunction with metallographic method simultaneously.
In order to achieve the above object, the present invention realizes the technical scheme that object adopts and is:
A kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior, comprise sample 1, contrast electrode 2, auxiliary electrode 3, cathode pool 5, anode pool 6 and hyperchannel potentiostat 9, the barrel shaped structure that wherein said cathode pool 5 is upper shed, the tubular construction that described anode pool 6 is upper and lower opening, and from bottom to top successively by cathode pool 5, sample 1 and several anode pools 6 are vertically settled, wherein said contrast electrode 2 and auxiliary electrode 3 are arranged in described cathode pool 5 up and down, and be connected with the respective channel of described potentiostat 9 by penetrating the sealing contrast electrode fixed orifice 7 that described cathode pool 5 one sides arrange and sealing wire in auxiliary electrode fixed orifice 8 respectively, several described anode pools 6 are distributed in the upper plane of described sample 1, and each anode pool 6 is provided with auxiliary electrode and contrast electrode and its wire and is connected with the respective channel of described potentiostat 9 respectively, described sample 1 is connected with the respective channel of described potentiostat 9 by wire.
Cathode pool 5 described above is also provided with inlet 4.
The quantity of anode pool 6 described above is 4.
Cathode pool 5 described above and the material of anode pool 6 are teflon.
Between cathode pool 5, sample 1 and anode pool 6 described above, be fix and seal with silicon rubber by chloroform.
In order to achieve the above object, the present invention realizes another technical scheme that object adopts and is:
The method of testing of a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior of the present invention, is characterized in that comprising following concrete steps:
1) sample to be tested 1 is made into the thin slice that 0.5mm is thick, sample 1 both side surface is polished to 1000# sand paper step by step with abrasive paper for metallograph, mechanical buffing, then adopt galvanostatic method that sample 1 one side is carried out to plating nickel on surface, sample 1 after nickel plating is used anhydrous alcohol wiping after adopting Ultrasonic Cleaning clean in acetone, cold wind dries up, stand-by;
2) by step 1) in sample 1 nickel plating one for preparing face up and be placed between 5 and 4 anode pools 6 of cathode pool, adopt chloroform with silicon rubber, 4 anode pools 6 to be fixedly connected with and to be sealed with sample 1 respectively with cathode pool 5;
3) preparation fill hydrogen solution and expand hydrogen solution, described in fill the mixed liquor that hydrogen solution is the thiocarbamide of 0.2mol/L NaOH and 0.22g/L, expansion hydrogen solution be 0.1mol/L NaOH solution.
4) by step 3) in prepare fill hydrogen solution and expand hydrogen solution inject respectively 5 and 4 anode pools 6 of cathode pool;
5) on sample 1, applying 200mV current potential, to ensure permeate the hydrogen atom of coming from cathode pool 5 oxidized and then to make the hydrogen concentration of sample 1 anode surface be zero at once, and sample 1 nickel plating current density is simultaneously reduced to 0.2 μ A/cm
2shi Xuanyong 1.5mA/cm
2electric current carries out cathodic polarization, is recorded and is shown that sample 1 each local location releases hydrogen electric current in hydrogen solution and be worth over time filling by hyperchannel potentiostat 9.
What nickel plating described above adopted is the mixing nickel-plating liquid of nickel sulfate solution, nickel chloride solution and BAS, the NiSO that described nickel sulfate solution is 250g/L
4.6H
2o, the NiCl that nickel chloride solution is 45g/L
2.6H
2o, the H that BAS is 40g/L
3bO
3.The current density that described nickel plating adopts is 10mA/cm
2, the time is 60s.
Of the present inventionly for the hyperchannel hydrogen-measuring apparatus of metal material hydrogen permeation behavior and the advantage of method and good effect be:
1. the present invention has changed the behavior that in the past adopts the infiltration of single channel D-S electrolytic cell method research metal material hydrogen, and employing hyperchannel D-S electrolytic cell technology, the hydrogen permeation behavior of the multiple local locations of measuring metallic materials simultaneously, and then be convenient to the impact of research material local organization difference on hydrogen permeation behavior.
2. the present invention is simple to operate flexibly, can experimental demand change flexibly passage number;
3. the installation cost that research method of the present invention adopts is lower, and degree of accuracy is high.
Brief description of the drawings
Fig. 1 is the structural representation of a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior of the present invention;
In figure, 1. sample; 2. contrast electrode; 3. auxiliary electrode; 4. inlet; 5. cathode pool; 6. anode pool; 7. sealing contrast electrode fixed orifice; 8. sealing auxiliary electrode fixed orifice; 9. hyperchannel potentiostat
Embodiment
Below in conjunction with accompanying drawing, a kind of hyperchannel hydrogen-measuring apparatus and method for metal material hydrogen permeation behavior of the present invention is described in further detail.
A kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior of the present invention, comprise sample 1, contrast electrode 2, auxiliary electrode 3, cathode pool 5, anode pool 6 and hyperchannel potentiostat 9, the barrel shaped structure that wherein said cathode pool 5 is upper shed, the tubular construction that described anode pool 6 is upper and lower opening, and from bottom to top successively by cathode pool 5, sample 1 and several anode pools 6 are vertically settled, wherein said contrast electrode 2 and auxiliary electrode 3 are arranged in described cathode pool 5 up and down, and be connected with the respective channel of described potentiostat 9 by penetrating the sealing contrast electrode fixed orifice 7 that described cathode pool 5 one sides arrange and sealing wire in auxiliary electrode fixed orifice 8 respectively, several described anode pools 6 are distributed in the upper plane of described sample 1, and each anode pool 6 is provided with contrast electrode and auxiliary electrode and its wire and is connected with the respective channel of described potentiostat 9 respectively, described sample 1 is connected with the respective channel of described potentiostat 9 by wire, between described cathode pool 5, sample 1 and anode pool 6, be fix and seal with silicon rubber by chloroform, inlet 4 in described device is convenient to inject and fill hydrogen solution in cathode pool 5.
The method of testing of a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior of the present invention, comprises the steps:
First sample to be tested is made into the disk film sample that 0.5mm is thick, sample both side surface is polished to 1000# sand paper step by step with abrasive paper for metallograph, mechanical buffing, then adopt galvanostatic method that sample one side is carried out to plating nickel on surface, nickel-plating liquid used is the mixed liquor of nickel sulfate solution, nickel chloride solution and BAS, the NiSO that described nickel sulfate solution is 250g/L
4.6H
2o, the NiCl that nickel chloride solution is 45g/L
2.6H
2o, the H that BAS is 40g/L
3bO
3, nickel plating current density is: 10mA/cm
2, the time is: 60s, and the sample after nickel plating is used anhydrous alcohol wiping after adopting Ultrasonic Cleaning clean in acetone, and cold wind dries up, stand-by.
Then the sample nickel plating one preparing is faced up and is placed between 5 and 4 anode pools 6 of cathode pool, adopt chloroform with silicon rubber, 4 anode pools 6 to be fixedly connected with and to be sealed with sample 1 respectively with cathode pool 5;
Then preparation fill hydrogen solution and expand hydrogen solution, described in fill the mixed liquor that hydrogen solution is the thiocarbamide of 0.2mol/L NaOH and 0.22g/L, expansion hydrogen solution be 0.1mol/L NaOH solution, inject respectively 5 and 4 anode pools 6 of cathode pool;
Last on sample 1, apply 200mV current potential to ensure permeate the hydrogen atom of coming from cathode pool 5 oxidized and then to make sample anode side hydrogen concentration be zero at once, the current density of sample 1 nickel plating one side is reduced to 0.2 μ A/cm2 below and reaches while stablizing and selects 1.5mA/cm2 electric current to carry out cathodic polarization by the time; Record and show that sample 1 each local location releases hydrogen electric current in hydrogen solution and be worth over time filling by hyperchannel potentiostat 9.
Claims (8)
1. the hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior, comprise sample (1), contrast electrode (2), auxiliary electrode (3), cathode pool (5), anode pool (6) and hyperchannel potentiostat (9), it is characterized in that: the barrel shaped structure that described cathode pool (5) is upper shed, the tubular construction that described anode pool (6) is upper and lower opening, and from bottom to top successively by cathode pool (5), sample (1) and several anode pools (6) are vertically settled, wherein said contrast electrode (2) and auxiliary electrode (3) are arranged in described cathode pool (5) up and down, and be connected with the respective channel of described potentiostat (9) by penetrating the sealing contrast electrode fixed orifice (7) that described cathode pool (5) one sides arrange and sealing wire in auxiliary electrode fixed orifice (8) respectively, described several anode pools (6) are distributed in the upper plane of described sample (1), be provided with its wire of auxiliary electrode and contrast electrode and be connected with the respective channel of described potentiostat (9) respectively in each anode pool (6), described sample (1) is connected with the respective channel of described potentiostat (9) by wire.
2. a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 1, is characterized in that: described cathode pool (5) is also provided with inlet (4).
3. a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 1, is characterized in that: the quantity of described anode pool (6) is 4.
4. a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 1, is characterized in that: described cathode pool (5) and the material of anode pool (6) are teflon.
5. a kind of hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 1, is characterized in that: between described cathode pool (5), sample (1) and anode pool (6), be fixed and sealed with silicon rubber by chloroform.
6. a method of testing for the hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 1, is characterized in that comprising following concrete steps:
1) sample to be tested is made into the thin slice that 0.5mm is thick, sample both side surface is polished to 1000# sand paper step by step with abrasive paper for metallograph, mechanical buffing, then adopt galvanostatic method that sample one side is carried out to plating nickel on surface, sample after nickel plating is used anhydrous alcohol wiping after adopting Ultrasonic Cleaning clean in acetone, cold wind dries up, stand-by;
2) by step 1) in sample (1) nickel plating one for preparing face up and be placed between cathode pool (5) and 4 anode pools (6), adopt chloroform with silicon rubber, 4 anode pools (6) to be fixedly connected with and to be sealed with sample (1) respectively with cathode pool (5);
3) preparation fill hydrogen solution and expand hydrogen solution, described in fill the mixed liquor that hydrogen solution is the thiocarbamide of 0.2mol/L NaOH and 0.22g/L, expansion hydrogen solution be 0.1mol/L NaOH solution.
4) by step 3) prepare fill hydrogen solution and expand hydrogen solution inject respectively cathode pool (5) and 4 anode pools (6);
5) on sample (1), applying 200mV current potential, to ensure permeate the hydrogen atom of coming from cathode pool (5) oxidized and then to make the hydrogen concentration of sample (1) anode surface be zero at once, and sample (1) nickel plating current density is simultaneously reduced to 0.2 μ A/cm
2shi Xuanyong 1.5mA/cm
2electric current carries out cathodic polarization, is recorded and is shown that each local location of sample (1) releases hydrogen electric current in hydrogen solution and be worth over time filling by hyperchannel potentiostat (9).
7. the method for testing of the hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior according to claim 6, it is characterized in that: what described nickel plating adopted is the mixing nickel-plating liquid of nickel sulfate solution, nickel chloride solution and BAS, the NiSO that described nickel sulfate solution is 250g/L
4.6H
2o, the NiCl that nickel chloride solution is 45g/L
2.6H
2o, the H that BAS is 40g/L
3bO
3.
8. according to the method for testing of the hyperchannel hydrogen-measuring apparatus for metal material hydrogen permeation behavior described in claim 6 or 7, it is characterized in that: the current density that described nickel plating adopts is 10mA/cm
2, the time is 60s.
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Cited By (7)
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| CN104515732A (en) * | 2014-12-19 | 2015-04-15 | 北京科技大学 | Hydrogen permeability testing device for metal material under high liquid pressure |
| 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 |
| CN107796739A (en) * | 2017-10-17 | 2018-03-13 | 中石化炼化工程（集团）股份有限公司 | The devices and methods therefor that metallic hydrogen penetrating quality is tested under wet gas environments |
| CN110095523A (en) * | 2018-01-29 | 2019-08-06 | 宝山钢铁股份有限公司 | A method of the prediction quick-fried occurrence probability size of enamelware squama |
| CN110369391A (en) * | 2019-07-13 | 2019-10-25 | 深圳市大柏光电子科技有限公司 | A kind of technique for cleaning LED package carrier harmful element |
| CN113049484A (en) * | 2019-12-27 | 2021-06-29 | 中国科学院海洋研究所 | Device and method for measuring hydrogen permeability of metal material |
| CN113791028A (en) * | 2021-09-13 | 2021-12-14 | 国网山东省电力公司电力科学研究院 | Detection device and method for directly detecting soil corrosion rate of metal material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104515732A (en) * | 2014-12-19 | 2015-04-15 | 北京科技大学 | Hydrogen permeability testing device for metal material under high liquid pressure |
| CN104515732B (en) * | 2014-12-19 | 2017-01-04 | 北京科技大学 | A kind of test metal material device of hydrogen penetrating quality under liquid high pressure |
| 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 |
| CN107796739A (en) * | 2017-10-17 | 2018-03-13 | 中石化炼化工程（集团）股份有限公司 | The devices and methods therefor that metallic hydrogen penetrating quality is tested under wet gas environments |
| CN107796739B (en) * | 2017-10-17 | 2020-06-12 | 中石化炼化工程（集团）股份有限公司 | Device and method for testing metal hydrogen permeability in moisture environment |
| CN110095523A (en) * | 2018-01-29 | 2019-08-06 | 宝山钢铁股份有限公司 | A method of the prediction quick-fried occurrence probability size of enamelware squama |
| CN110095523B (en) * | 2018-01-29 | 2021-05-14 | 宝山钢铁股份有限公司 | Method for predicting scale explosion occurrence probability of enamel product |
| CN110369391A (en) * | 2019-07-13 | 2019-10-25 | 深圳市大柏光电子科技有限公司 | A kind of technique for cleaning LED package carrier harmful element |
| CN113049484A (en) * | 2019-12-27 | 2021-06-29 | 中国科学院海洋研究所 | Device and method for measuring hydrogen permeability of metal material |
| CN113791028A (en) * | 2021-09-13 | 2021-12-14 | 国网山东省电力公司电力科学研究院 | Detection device and method for directly detecting soil corrosion rate of metal material |
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