CN101819131B - Electrochemical test solution for evaluating corrosion resistance of cold-rolled sheet phosphate coating - Google Patents
Electrochemical test solution for evaluating corrosion resistance of cold-rolled sheet phosphate coating Download PDFInfo
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- CN101819131B CN101819131B CN200910010509A CN200910010509A CN101819131B CN 101819131 B CN101819131 B CN 101819131B CN 200910010509 A CN200910010509 A CN 200910010509A CN 200910010509 A CN200910010509 A CN 200910010509A CN 101819131 B CN101819131 B CN 101819131B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 24
- 230000007797 corrosion Effects 0.000 title claims abstract description 23
- 238000000840 electrochemical analysis Methods 0.000 title claims abstract description 18
- 239000012085 test solution Substances 0.000 title claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 14
- 239000010452 phosphate Substances 0.000 title claims abstract description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 13
- 239000011248 coating agent Substances 0.000 title claims description 5
- 238000000576 coating method Methods 0.000 title claims description 5
- 239000000243 solution Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 6
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 6
- 235000019800 disodium phosphate Nutrition 0.000 claims description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 6
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000003044 adaptive effect Effects 0.000 abstract description 3
- 230000003628 erosive effect Effects 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 239000011780 sodium chloride Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 3
- 238000012951 Remeasurement Methods 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 241000283984 Rodentia Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical compound [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- -1 phosphate anion Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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Abstract
The invention discloses an electrochemical test solution for evaluating corrosion resistance of a cold-rolled sheet phosphate film, which is characterized in that a solute is a phosphate composition, a solvent is distilled water, the concentration of the solution is 0.1-1% by mass percent, the pH value is 6-8, the adaptive temperature range is 0-60 ℃, and the electrochemical test solution has the advantages and effects that: the solution is neutral and has little erosion to the immersed materials; (2) the solution has stable acidity, and can reduce the influence of other factors on the pH value of the solution; (3) the solution is stable, the components are unchanged at 10-60 ℃, and the pH value is changed to be less than or equal to 0.01; (4) the method can quickly obtain stable electrochemical conditions, has obvious difference on electrochemical parameters expressed by the phosphorized material and the non-phosphorized material, and can truly and quickly evaluate the corrosion resistance of the phosphorized film.
Description
Technical field
The invention belongs to a kind of test chemical solution, specifically is a kind of electrochemical test solution that is used for metallurgy industry evaluating corrosion resistance of cold-rolled sheet phosphate coating ability usefulness.
Background technology
Phosphatization is as important surface preparation technology, obtained developing widely and using at aspects such as anti-corrosion, application, lubricated, finishes.The purposes of phosphating coat depends on the performance of phosphating coat, so the performance of objective evaluation phosphating coat just seems particularly important.Corrosion resisting property is an important usability of phosphating coat, and existing at present a series of conventional test method of testing comprises film remeasurement, copper sulphate pitting test, salt water test and electro-chemical test etc.The film remeasurement is comparatively accurate, but its result can not be directly corresponding to the corrosion stability of phosphating coat, than coarse-grain phosphating coat even compact more, and have better corrosion resisting property like thin brilliant phosphating coat; The corrosion stability of phosphating coat can both be more directly estimated in copper sulphate pitting test and salt water test, but can only provide result qualitatively, and introduces bigger personal error easily; Electro-chemical test comprises corrosion potential method, polarization method, electrochemical impedance method etc.; It is a kind of digital test technology of correct and objective evaluation phosphating coat performance; It can measure corrosion potential, current value or the resistance value of electrode in electrolyte solution that contains phosphating coat; Through these data can be regarded as dissolution velocity and the porosity of phosphating coat of metal, the corrosion resisting property of quantitative evaluation phosphating coat.
In the electro-chemical test process of phosphating coat corrosion resisting property, test solution may make phosphating coat change of properties, increase or reduce phosphating coat porosity, or change the interfacial structure etc. of matrix/phosphating coat.So, accurately estimate the corrosion resisting property of phosphating coat, should note the selection of electrochemical test solution.People such as Kiss find that the trbasic zinc phosphate rete all will dissolve fast in acid, alkaline, as to contain complexing agent solution; People such as Stiegditz discover, at NaCl and Na
2SO
4Etc. the infiltration that contains chlorion or sulfate ion in the neutrality, or the dissolving of phosphate anion all will make the character of phosphating coat change under the rete; People such as Wang discover that the porosity of phosphating coat increases with the enhancing of cathodic polarization in 0.01mol/LNaoH solution, and at 0.5mol/L Na
2SO
4Solution mesoporosity rate reduces and increases that (during pH=7.0, porosity is 2.8% with pH's; During pH=4.7, porosity is 36.5%); People such as Fils utilize at room temperature that the pH value is 8.5, concentration is 0.005mol/LNa
2HPO
4Solution is as the electro-chemical test personnel of phosphating coat, but this solution is alkalescence, and can only at room temperature make an experiment.
In sum; One of key factor of phosphating coat corrosion resisting property Electrochemical Measurement Technology is correct a kind of test solution that phosphating coat is not had erosion of selecting; This solution makes immersion phosphating coat wherein that marked change not take place; Promptly this solution can obtain stable electrochemical conditions apace, and to the phosphatization material and not the electrochemical parameter that showed of phosphatization material evident difference is arranged, also do not meet the electrochemical test solution of above-mentioned condition at present.
Summary of the invention
The object of the present invention is to provide a kind of novel electrochemical test solution.This solution has solved in the electro-chemical test process, owing to electrochemical test solution has the problem that Electrochemical results that erosion action makes the phosphating coat corrosion resisting property produces error to phosphating coat.
This novel electrochemical test solution, its solute are phosphate composition, and solvent is a distilled water, and solution concentration is 0.1～1% by mass percentage, and its pH value is 6～8, and the adaptive temperature scope is 0～60 ℃.
Described phosphate comprises potassium dihydrogen phosphate and sodium hydrogen phosphate composition, or both matched combined in the dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate.
When adopting potassium dihydrogen phosphate and sodium hydrogen phosphate combination solution, its two kinds of salt are 1: 1 proportioning of example in molar ratio.Said distillation electrical conductivity of water≤5 μ s/cm.
Advantage of the present invention and effect be,
(1) this solution is neutral, and is little to the material corrosion property that immerses.
(2) this solution has stable acidity, can reduce the influence of other factors to the pH value of solution value.
(3) this is solution-stabilized, and composition no change, pH value change≤0.01 between 10～60 ℃.
(4) can obtain stable electrochemical conditions fast, and to the phosphatization material and not the electrochemical parameter that showed of phosphatization material evident difference is arranged, can estimate the corrosion resisting property of phosphating coat truly, fast.
Description of drawings
Fig. 1 is the open circuit potential comparison diagram of cold-reduced sheet in different solutions after the phosphatization;
Fig. 2 is the electrochemical impedance Nyquist figure of the forward and backward cold-reduced sheet of phosphatization in the 3.5%NaCl solution;
Fig. 3 is the electrochemical impedance Nyquist figure of the forward and backward cold-reduced sheet of phosphatization among the present invention.
Embodiment
The present invention is applicable to that evaluating corrosion resistance of cold-rolled sheet phosphate coating can; Its characteristics are that its solute is a phosphate composition, and solution concentration is 0.1%～1% by mass percentage, and solvent adopts distilled water; Its pH value is 6～8, and this test chemical adaptive temperature scope is 10～60 ℃.Said distillation electrical conductivity of water≤5 μ s/cm.
Described phosphate; Comprise both matched combined in sour hydrogen dipotassium, potassium dihydrogen phosphate, sodium hydrogen phosphate, the sodium dihydrogen phosphate; When both examples during 1: 1 proportioning in molar ratio; This solution has stable acidity, can reduce the influence of other factors to the pH value of solution value, avoided since the variation of solution acidity to the phosphating coat Effect on Performance.Its effect is remarkable when potassium dihydrogen phosphate and sodium hydrogen phosphate combination.
Through contrast, specify effect of the present invention below to the electrochemical behavior of the forward and backward cold-reduced sheet of phosphatization in a specific embodiment of the present invention and the most frequently used 3.5%NaCl solution.
Step 1, with the KH of 0.025mol
2PO
4Na with 0.025mol
2HPO
4Be dissolved in the 200ml distilled water, at last with its constant volume 1000ml.The mass percent concentration of this solution is 0.7%, and between 10～60 ℃, its pH value is 6.86.
Step 2, place 3.5%NaCl solution and solution of the present invention to carry out the test of open circuit potential respectively the cold-reduced sheet after the phosphatization, sweep velocity is 0.166mv/s, when current potential at the changing value of 120s in the time during less than 5mV, termination test.
Step 3, the cold-reduced sheet that phosphatization is forward and backward place 3.5%NaCl solution and solution of the present invention to carry out the test of impedance Nyquist spectrogram respectively; Sweep velocity is 0.166mv/s; The used sine voltage signal amplitude of impedance spectrogram test be 10mV as pumping signal, range of scanned frequencies is 1 * 10
5Hz～1 * 10
-1Hz.
Step 4, judge the rodent size of electrochemical test solution according to the stable time of cold-reduced sheet open circuit potential after the phosphatization.
As shown in Figure 1, in 3.5%NaCl solution, the changing value of the open circuit potential in 120s of the cold-reduced sheet after the phosphatization is about 580s less than the time that 5mV occurs; In solution of the present invention; The changing value of the open circuit potential in 120s of the cold-reduced sheet after the phosphatization is about 180s less than the time that 5mV occurs; Cold-reduced sheet after this explanation phosphatization can obtain stable electrochemical potential apace in solution of the present invention; Solution of the present invention makes the character of immersion phosphating coat wherein that marked change not take place, and can reflect the corrosion resisting property of phosphating coat really.
Step 5, judge the corrosion resisting property of phosphating coat at the radius of electrochemical test solution middle impedance Nyquist spectrogram according to the forward and backward cold-reduced sheet of phosphatization.
As shown in Figure 2, in 3.5%NaCl solution, the impedance Nyquist spectrogram radius difference of the forward and backward cold-reduced sheet of phosphatization is less, and maximum Zim value approximately differs about 40 Ω.
As shown in Figure 3, in solution of the present invention, the impedance Nyquist spectrogram radius significant difference of the forward and backward cold-reduced sheet of phosphatization, maximum Zim value approximately differs about 3000 Ω.
Can find out from above-mentioned contrast, solution of the present invention to the phosphatization material and not the electrochemical parameter that showed of phosphatization material evident difference is arranged, help estimating accurately the corrosion resisting property of phosphating coat.
Experiment shows, in the test process the present invention solution-stabilized between 10～60 ℃, the composition no change, the pH value changes≤0.01.
Table 1 is several specific embodiment of the present invention.
Table 1 test figure
Claims (1)
1. one kind is used for the electrochemical test solution that evaluating corrosion resistance of cold-rolled sheet phosphate coating is used; It is characterized in that; Its solute adopts phosphate composition, and solvent is a distilled water, and solution concentration is 0.1%～1% by mass percentage; Described phosphate composition is by both matched combined in dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium hydrogen phosphate, the sodium dihydrogen phosphate, and its pH value of the routine in molar ratio 1:1 proportioning of its two kinds of salt is 6～8.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910010509A CN101819131B (en) | 2009-02-27 | 2009-02-27 | Electrochemical test solution for evaluating corrosion resistance of cold-rolled sheet phosphate coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910010509A CN101819131B (en) | 2009-02-27 | 2009-02-27 | Electrochemical test solution for evaluating corrosion resistance of cold-rolled sheet phosphate coating |
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| Publication Number | Publication Date |
|---|---|
| CN101819131A CN101819131A (en) | 2010-09-01 |
| CN101819131B true CN101819131B (en) | 2012-09-26 |
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| CN108203822B (en) * | 2016-12-16 | 2020-04-14 | 宝钢湛江钢铁有限公司 | Solution and method for evaluating corrosion resistance of water-based anti-rust layer on surface of steel plate |
| CN110361313B (en) * | 2019-07-11 | 2022-04-05 | 上海应用技术大学 | Electrochemical test method for quantitatively evaluating porosity of phosphating film |
| CN116068038A (en) * | 2021-11-04 | 2023-05-05 | 复旦大学 | Method for evaluating ion screening capability of GO/ANF/GO composite membrane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6264823B1 (en) * | 1998-09-18 | 2001-07-24 | Hoffman Industries International, Ltd. | Non-caustic cleaning of conductive and non-conductive bodies |
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2009
- 2009-02-27 CN CN200910010509A patent/CN101819131B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6264823B1 (en) * | 1998-09-18 | 2001-07-24 | Hoffman Industries International, Ltd. | Non-caustic cleaning of conductive and non-conductive bodies |
Non-Patent Citations (4)
| Title |
|---|
| JP特开2005-290441A 2005.10.20 |
| JP特开2008-45185A 2008.02.28 |
| 李玉荣等.中山舰船体钢耐蚀性能检测与分析.《材料保护》.2003,第36卷(第10期),第44-47页. * |
| 韩恩山等.常温钢铁磷化处理的研究.《腐蚀科学与防护技术》.2006,第18卷(第5期),第341-344页. * |
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