CN104977333A - Hydrogen-filling additive for measuring hydrogen diffusion coefficient in steel and measuring method - Google Patents
Hydrogen-filling additive for measuring hydrogen diffusion coefficient in steel and measuring method Download PDFInfo
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- CN104977333A CN104977333A CN201410142544.1A CN201410142544A CN104977333A CN 104977333 A CN104977333 A CN 104977333A CN 201410142544 A CN201410142544 A CN 201410142544A CN 104977333 A CN104977333 A CN 104977333A
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Abstract
The invention discloses a hydrogen-filling additive for measuring hydrogen diffusion coefficient in steel and a measuring method, wherein the hydrogen-filling additive is nitrilotriacetic acid being 0.8-2.8 mmol/L in concentration. The measuring method includes following steps: (1) connecting a working electrode end of a potentiostat, connecting a reference electrode end to an anode electrolytic cell saturated calomel electrode, connecting an auxiliary electrode to an anode electrolytic cell platinum electrode, connecting a negative pole of a constant current source to a steel sample and connecting a positive pole of the constant current source to a cathode electrolytic cell platinum electrode; (2) adding a NaOH solution to the anode electrolytic cell, applying a constant-potential polarization potential, and filling the cathode electrolytic cell with a H2SO4 solution added with the hydrogen-filling additive when the polarization current density is less than 1 [mu]A/cm<2>; (3) according to the Fick's law, finding a time t of a point corresponding to a value of I<t>/I<max>=0.63 in a curve, calculating the value of t minus t<0> which is the time starting the constant current source to obtain a retardation time value t<L>; and (4) substituting the t<L> into a formula to calculate the effective diffusion coefficient of hydrogen in the steel sample. The invention avoids a defect of a highly toxic chemical reagent being used as a hydrogen-filling additive, thereby greatly reducing damage on human body and environment.
Description
Technical field
The invention belongs to metal material inspection field, particularly a kind ofly fill hydrogen adjuvant and method of testing thereof for hydrogen diffusion coefficient in tested steel.
Background technology
Along with the development in the fields such as automobile, oil, ocean, aviation, nuclear industry and hydrogen energy source, the requirement for the plow-steel performance used under facing hydrogen environment is more and more higher.Such as fastening parts of automobiles steel, vehicle door anti-collision joist superelevation are by force with steel, storage hydrogen pressure container, Oil and Natural Gas Transportation Pipeline, liquefied gas storage, Steels For Offshore Oil Platform and Aero-Space special alloy etc., material is not only needed to have high strength, more to have good resistant to hydrogen and cause fracture property, to guarantee the safety and reliability of materials'use.
Hydrogen spreads in the material, will crack initiation after regional area enrichment exceedes critical concentration, and under external force, crackle is constantly expanded and caused rupturing (hydrogen embrittlement), thus causes sudden pernicious malicious event.Therefore the dispersal behavior of Study of Hydrogen in steel is the important content of research hydrogen-induced fracture.In general, all there is crystal defects such as resembling dislocation, crystal boundary, snotter interface, carbide interface in metal and alloy, they can catch hydrogen, are commonly referred to hydrogen trap, and the existence of hydrogen trap can reduce Hydrogen diffusion coefficient to some extent.Electrochemical double-electrolyzer method is utilized to be a kind ofly have method that is simple, efficient, feature flexibly to test the hydrogen diffusion coefficient of the dispersal behavior of hydrogen in steel and material thereof.Utilizing the method to carry out in test process, needing to add to stop hydrogen atom to recombine chemical reagent into hydrogen molecule, to strengthen the absorption of hydrogen filling in the electrolytic solution of hydrogen side.
At present, generally As is used
2o
3, Na
3asO
4, Na
2s etc. have hypertoxicity or highly toxic material, and the hydrogen adjuvant (poisonous agent) that fills used introduced in " galvanochemistry fills the hydrogen induced cracking behavior of X70 pipe line steel and weld seam thereof under hydrogen condition " literary composition as people such as Zhang Yingrui is As
2o
3, it is 3.34 × l0 that its hydrogen permeability test records the effective diffusion cofficient of hydrogen in X70 steel under room temperature
-9cm
2/ s.The liberation of hydrogen electrolytic solution used that the people such as Zhao Liang introduce in " hydrogen is low temperature diffusion coefficient in steel " literary composition is 0.2mol/LNaOH+1%Na
2s, at 6mA/cm
2current density under constant-current electrolysis fill hydrogen, list the arrhenius equation between temperature.The hydrogen adjuvant that fills used is here Na
2s.And the people such as Chen Tao deliver " Fe to hydrogen at disordered state and ordered state Ni
3the impact of spreading in Fe alloy " on cathode surface, be combined into hydrogen molecule agents useful for same be 50mg/LNa for the prevention hydrogen atom introduced in article
3asO
4, namely containing 50mg/L Na
3asO
40.5mol/L H
2sO
4the stoichiometry comparison hydrogen atom of Fe when negative electrode oozes hydrogen is studied at disordered state and ordered state Ni in electrolytic solution
3the impact of spreading in Fe alloy.In sum, be necessary developing green low toxicity or nontoxic fill hydrogen adjuvant.
Summary of the invention
What the invention provides hydrogen diffusion coefficient in a kind of tested steel fills hydrogen adjuvant and method of testing, is intended to avoid prior art and uses severe toxicity and high malicious chemicals as the drawback of filling hydrogen adjuvant, reduce the harm to human body and environment.
For this reason, the solution that the present invention takes is:
In tested steel hydrogen diffusion coefficient fill a hydrogen adjuvant, it is characterized in that, described in fill hydrogen adjuvant adopt concentration be that acidity prepared by 0.8 ~ 2.8mmol/L nitrilotriacetic acid fills hydrogen electrolytic solution.
Described nitrilotriacetic acid concentration of filling hydrogen adjuvant is 1.8mmol/L.
A method of testing for hydrogen diffusion coefficient in steel, utilizes galvanochemistry double-electrolyzer method to test hydrogen diffusion behaviour in steel, it is characterized in that:
1, measure steel sample thickness L value, degreasing, activation are carried out to steel sample, then carries out single-side nickel-plating.
2, be installed in double-electrolyzer by steel sample, its nickel plating is facing to side, anode electrolysis pond.
3, be connected with steel sample by the working electrode end of potentiostat, contrast electrode end is connected with the saturated calomel electrode of side, anode electrolysis pond, and auxiliary electrode is connected with the platinum electrode of side, anode electrolysis pond.
4, the negative pole of constant current supply is connected steel sample, positive pole connects the platinum electrode of side, catholyte pond.
5, under room temperature, in anode electrolysis pond, add the NaOH solution of 0.2mol/L, utilize computer for controlling to apply 0.001 ~ 0.2V constant potential polarization current potential afterwards, now on steel sample surface, following reaction occurs:
OH
-+[H]-e→H
2O
Along with [H] in steel sample be diffused into gradually surface and oxidized, anodic oxidation aftercurrent tends towards stability gradually.
6,1 μ A/cm is less than in polarized current density
2time, will the 0.5mol/L H filling hydrogen adjuvant be added with
2sO
4solution injects catholyte pond, with 1 ~ 10mA/cm
2current density open constant current supply, and record time is now t
0; There is following reaction in the steel sample surface now filled in hydrogen electrolytic cell:
H
++e→[H]
[H]+[H]→H
2↑
[H]+M→M-H
When filling after hydrogen adjuvant is adsorbed in electrode surface, the overpotential of hydrogen on steel sample being raised, serves cathodic polarization effect, hinder [H] and be combined into H
2go adsorption process, thus promote hydrogen atom to steel sample internal divergence; Because hydrogen exists certain concentration difference in steel sample, hydrogen atom continuous anode electrolytic cell side is moved, when hydrogen atom arrives anode-side surface, under the catalysis and potentiostat anode polarization effect of nickel, hydrogen atom is oxidized, forms electric current in the loop, and prolongation in time, oxidation current increases gradually, finally reaches the equilibrium state of high point.
7, utilize Fick law, find the time t of the corresponding point of It/Imax=0.63 in curve, cut and remove that steel sample is original exists hydrogen time t used
0, obtain t retardation time filling hydrogen process
l, It is time-varying hydrogen atom infiltration electric current, hydrogen atom maximum infiltration electric current when Imax is stable state, by sample thickness L and retardation time t
lsubstitute into formula
calculate the effective diffusion cofficient D of hydrogen in steel
eff.
Beneficial effect of the present invention is:
The acidity adopting 0.8 ~ 2.8mmol/L nitrilotriacetic acid to prepare due to the present invention fills hydrogen electrolytic solution as filling hydrogen adjuvant, avoiding prior art uses severe toxicity or high malicious chemicals as the drawback of filling hydrogen adjuvant, in accurate test tapping while hydrogen diffusion coefficient, the harm to human body and environment can be significantly reduced.
Accompanying drawing explanation
Fig. 1 is hydrogen diffusion behaviour device schematic diagram in galvanochemistry double-electrolyzer method tested steel;
Fig. 2 is oxidation current curve over time in hydrogen trap test.
In figure: 1 is steel sample to be measured, and 2 is catholyte pond, and 3 is anode electrolysis pond, 4 is constant current supply, and 5 is potentiostat, and 6 is computer for controlling, 7 is potentiostat working electrode end, 8 is potentiostat contrast electrode end, and 9 is saturated calomel electrode (SCE), and 10 is that potentiostat auxiliary electrical is extreme, 11 is anode electrolysis pond platinum electrode, 12 is constant current supply negative pole, and 13 is constant current supply positive pole, and 14 is catholyte pond platinum electrode.
Embodiment
Embodiment:
Get SCD1 steel sample, its chemical composition (mass%) is: C0.0012, Si0.009, Mn0.2, P0.0068, S0.006, and (Ti+Ni+Cr+Cu) is 0.07, Fe surplus; Surfaceness is Ra1.072 μm, Rz6.122 μm, RPc81.6 peak value/cm.Steel sample 1 thickness L=1.0mm to be measured.
Single-side nickel-plating is carried out by after steel sample 1 to be measured degreasing, activation.Afterwards the nickel plating of steel sample 1 to be measured is installed in double-electrolyzer facing to side, anode electrolysis pond 3.Be connected with steel sample 1 to be measured by the working electrode end 7 of potentiostat 5, potentiostat contrast electrode end 8 is connected with the saturated calomel electrode 9 of side, anode electrolysis pond 3, and potentiostat auxiliary electrical extreme 10 is connected with the anode electrolysis pond platinum electrode 11 in anode electrolysis pond 3; Constant current supply negative pole 12 is connected to steel sample 1 to be measured, and the constant current supply positive pole 13 of constant current supply 4 is connected on the catholyte pond platinum electrode 14 in catholyte pond 2.Potentiostat 5 is connected with computer for controlling 6.(see figure 1)
Under room temperature (25 DEG C ± 0.5 DEG C) condition, in anode electrolysis pond 3, add 0.2mol/L NaOH solution, after-applied 0.05V constant potential polarization current potential (vs.SCE).1 μ A/cm is less than when anodic oxidation aftercurrent tends towards stability
2time, will the 0.5mol/L H filling hydrogen adjuvant be added with
2sO
4solution injects catholyte pond 2, with 1mA/cm
2current density open constant current supply 4, and record time is now t
0.
Owing to fill in hydrogen electrolytic solution containing filling hydrogen adjuvant, facilitate the diffusion of hydrogen atom to steel sample inside.When hydrogen atom diffuses to anode-side surface, under the catalysis and potentiostat anode polarization effect of nickel, hydrogen atom is oxidized, forms electric current in the loop.Prolongation in time, oxidation current increases gradually, finally reaches the equilibrium state of high point.
Utilize Fick law, find I in curve (see figure 2)
t/ I
maxthe time t of=0.63 corresponding point, deducts and starts dehydrogenation time t used
0, obtain t retardation time filling hydrogen process
l, substitute into formula
calculate the effective diffusion cofficient of hydrogen in steel, carry out the diffusion property of quantitatively characterizing hydrogen in steel sample with this.
Table 1 fills for prior art is added with 1% sodium sulphide the hydrogen trap related data that hydrogen adjuvant records steel sample; Table 2 fills for the embodiment of the present invention 1 ~ 6 is added with variable concentrations nitrilotriacetic acid the hydrogen trap related data that hydrogen adjuvant records steel sample.
Table 1 is added with 1% sodium sulphide and fills the hydrogen trap related data that hydrogen adjuvant records steel sample
Table 2 variable concentrations nitrilotriacetic acid of the present invention fills the hydrogen trap related data that hydrogen adjuvant records steel sample
From the numerical value of effective diffusion cofficient in table 2, in embodiment 1 ~ 6, the nitrilotriacetic acid of 0.2 ~ 2.8mmol/L concentration all can record the diffusion property of hydrogen in steel, and in embodiment 1 ~ 5 in the effective diffusion cofficient numerical value of hydrogen and table 1 existing sodium sulphide used fill hydrogen numerical value that adjuvant is surveyed and do not exceed ± 1 × 10
-6cm
2.s
-1, to illustrate the nitrilotriacetic acid of 0.8 ~ 2.8mmol/L concentration range as filling hydrogen adjuvant it is feasible.In view of using the effective diffusion cofficient numerical value of hydrogen measured by > 1.8mmol/L nitrilotriacetic acid to be tending towards constant, therefore can lock and using nitrilotriacetic acid as filling the optium concentration of hydrogen adjuvant for 1.8mmol/L.
Claims (3)
1. in tested steel hydrogen diffusion coefficient fill a hydrogen adjuvant, it is characterized in that, described in fill hydrogen adjuvant adopt concentration be that acidity prepared by 0.8 ~ 2.8mmol/L nitrilotriacetic acid fills hydrogen electrolytic solution.
2. in tested steel according to claim 1 hydrogen diffusion coefficient fill hydrogen adjuvant, it is characterized in that, described in fill hydrogen adjuvant nitrilotriacetic acid concentration be 1.8mmol/L.
3. the method for testing of filling hydrogen adjuvant of hydrogen diffusion coefficient in tested steel as claimed in claim 1, utilizes galvanochemistry double-electrolyzer method to test hydrogen diffusion behaviour in steel, it is characterized in that:
(1), measure steel sample thickness L value, degreasing, activation are carried out to steel sample, then carries out single-side nickel-plating;
(2), be installed in double-electrolyzer by steel sample, its nickel plating is facing to side, anode electrolysis pond;
(3), by the working electrode end of potentiostat be connected with steel sample, contrast electrode end is connected with the saturated calomel electrode of side, anode electrolysis pond, and auxiliary electrode is connected with the platinum electrode of side, anode electrolysis pond;
(4), by the negative pole of constant current supply connect steel sample, positive pole connects the platinum electrode of side, catholyte pond;
(5), under room temperature, in anode electrolysis pond, add the NaOH solution of 0.2mol/L, utilize computer for controlling to apply 0.001 ~ 0.2V constant potential polarization current potential afterwards, now on steel sample surface, following reaction occurs:
OH
-+[H]-e→H
2O
Along with [H] in steel sample be diffused into gradually surface and oxidized, anodic oxidation aftercurrent tends towards stability gradually;
(6), 1 μ A/cm is less than in polarized current density
2time, will the 0.5mol/L H filling hydrogen adjuvant be added with
2sO
4solution injects catholyte pond, with 1 ~ 10mA/cm
2current density open constant current supply, and record time is now t
0; There is following reaction in the steel sample surface now filled in hydrogen electrolytic cell:
H
++e→[H]
[H]+[H]→H
2↑
[H]+M→M-H
When filling after hydrogen adjuvant is adsorbed in electrode surface, the overpotential of hydrogen on steel sample being raised, serves cathodic polarization effect, hinder [H] and be combined into H
2go adsorption process, thus promote hydrogen atom to steel sample internal divergence; Because hydrogen exists certain concentration difference in steel sample, hydrogen atom continuous anode electrolytic cell side is moved, when hydrogen atom arrives anode-side surface, under the catalysis and potentiostat anode polarization effect of nickel, hydrogen atom is oxidized, forms electric current in the loop, and prolongation in time, oxidation current increases gradually, finally reaches the equilibrium state of high point;
(7), utilize Fick law, find the time t of the corresponding point of It/Imax=0.63 in curve, cut and remove that steel sample is original exists hydrogen time t used
0, obtain t retardation time filling hydrogen process
l, It is time-varying hydrogen atom infiltration electric current, hydrogen atom maximum infiltration electric current when Imax is stable state, by sample thickness L and retardation time t
lsubstitute into formula
calculate the effective diffusion cofficient D of hydrogen in steel
eff.
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Cited By (11)
| 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 |
| CN106248571A (en) * | 2016-10-10 | 2016-12-21 | 武汉钢铁股份有限公司 | Hydrogen diffusion coefficient evaluates the method for pipe line steel resistance against hydrogen cracking corrosive nature |
| CN106872337A (en) * | 2017-04-21 | 2017-06-20 | 北京科技大学 | The experimental provision and application method of hydrogen infiltration under a kind of constant stress stress state |
| CN107796752A (en) * | 2016-09-06 | 2018-03-13 | 鞍钢股份有限公司 | A kind of method for measuring steel hydrogen induced cracking (HIC) performance in hydrogen sulfide corrosion environment |
| CN108204938A (en) * | 2016-12-20 | 2018-06-26 | 核工业西南物理研究院 | Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating |
| CN108982301A (en) * | 2018-07-05 | 2018-12-11 | 河海大学 | A kind of measurement device and measuring method of hydrated calcium silicate gel chloride diffusion coefficient |
| CN109557152A (en) * | 2017-09-27 | 2019-04-02 | 鞍钢股份有限公司 | A kind of method of residual hydrogen reserves in Fast Evaluation steel |
| 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 |
| CN112129671A (en) * | 2020-09-24 | 2020-12-25 | 东北大学 | Device and method for measuring hydrogen diffusion coefficient of solid steel at high temperature |
| CN112481664A (en) * | 2020-11-10 | 2021-03-12 | 上海应用技术大学 | Non-toxic electrolyte for detecting fish scaling resistance of enamel steel and preparation method thereof |
| CN113186547A (en) * | 2021-04-19 | 2021-07-30 | 武汉科技大学 | Method and device for efficiently preparing high-purity high-pressure hydrogen by utilizing scrap steel |
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Cited By (16)
| 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 |
| CN107796752A (en) * | 2016-09-06 | 2018-03-13 | 鞍钢股份有限公司 | A kind of method for measuring steel hydrogen induced cracking (HIC) performance in hydrogen sulfide corrosion environment |
| CN106248571A (en) * | 2016-10-10 | 2016-12-21 | 武汉钢铁股份有限公司 | Hydrogen diffusion coefficient evaluates the method for pipe line steel resistance against hydrogen cracking corrosive nature |
| CN108204938B (en) * | 2016-12-20 | 2020-08-21 | 核工业西南物理研究院 | Hydrogen diffusion permeability measuring device in tritium-resistant coating |
| CN108204938A (en) * | 2016-12-20 | 2018-06-26 | 核工业西南物理研究院 | Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating |
| CN106872337A (en) * | 2017-04-21 | 2017-06-20 | 北京科技大学 | The experimental provision and application method of hydrogen infiltration under a kind of constant stress stress state |
| CN106872337B (en) * | 2017-04-21 | 2023-08-25 | 北京科技大学 | Experimental device for hydrogen permeation under constant stress loading state and application method |
| CN109557152A (en) * | 2017-09-27 | 2019-04-02 | 鞍钢股份有限公司 | A kind of method of residual hydrogen reserves in Fast Evaluation steel |
| 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 |
| CN108982301A (en) * | 2018-07-05 | 2018-12-11 | 河海大学 | A kind of measurement device and measuring method of hydrated calcium silicate gel chloride diffusion coefficient |
| CN108982301B (en) * | 2018-07-05 | 2020-09-29 | 河海大学 | Device and method for measuring diffusion coefficient of chloride ions in calcium silicate hydrate gel |
| CN112129671A (en) * | 2020-09-24 | 2020-12-25 | 东北大学 | Device and method for measuring hydrogen diffusion coefficient of solid steel at high temperature |
| CN112129671B (en) * | 2020-09-24 | 2021-11-30 | 东北大学 | Method for measuring hydrogen diffusion coefficient of solid steel at high temperature |
| CN112481664A (en) * | 2020-11-10 | 2021-03-12 | 上海应用技术大学 | Non-toxic electrolyte for detecting fish scaling resistance of enamel steel and preparation method thereof |
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Application publication date: 20151014 |