CN102269729A - Method for detecting quality of phosphating film - Google Patents
Method for detecting quality of phosphating film Download PDFInfo
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- CN102269729A CN102269729A CN2010102016468A CN201010201646A CN102269729A CN 102269729 A CN102269729 A CN 102269729A CN 2010102016468 A CN2010102016468 A CN 2010102016468A CN 201010201646 A CN201010201646 A CN 201010201646A CN 102269729 A CN102269729 A CN 102269729A
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- inflection point
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- phosphating film
- phosphating
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- 238000000034 method Methods 0.000 title abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 37
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000012085 test solution Substances 0.000 claims abstract description 3
- 229940075397 calomel Drugs 0.000 claims abstract 2
- 239000003792 electrolyte Substances 0.000 claims abstract 2
- 238000001514 detection method Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 5
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000000840 electrochemical analysis Methods 0.000 abstract description 4
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 abstract 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 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
- 238000007405 data analysis Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for detecting quality of a phosphating film, which comprises the step of processing a sample plate subjected to phosphating into a sample plate with the surface area not less than 1cm2The test piece adopts a three-electrode electrochemical test system, wherein a working electrode is a test piece to be tested, a reference electrode is a calomel electrode, an auxiliary electrode is a platinum wire mesh, the electrolyte solute concentration is 0.45-0.55% of monopotassium phosphate test solution by mass percent, the test of the curve of the relation between the open-circuit potential and the time is carried out under the room temperature condition, and when the curve has an inflection point, the time of the inflection point is recorded. When the time t of the inflection point is less than or equal to 300s, the quality of the phosphating film is poor; when the inflection point occurrence time is more than 300s and less than or equal to 700s, the quality of the phosphating film is general; when the inflection point occurrence time is more than 700s and less than or equal to 1000s, the quality of the phosphating film is good; when the time t of the inflection point is more than 1000s, the quality of the phosphating film is good.
Description
Technical field
The invention provides a kind of detection method of phosphorization film quality, a kind of specifically electrochemical test method that detects the phosphating coat crystalline state.
Background technology
Phosphatization is as important surface preparation technology, obtained developing widely and using at aspects such as anti-corrosion, application, lubricated, finishes.The crystalline state of phosphating coat comprises the crystal size of phosphating coat crystal grain, the homogeneity of phosphating coat and the compactness of phosphating coat, the combined action meeting of these three aspects directly reflects the quality of phosphating coat, can directly influence its in anti-corrosion, application, lubricate, the effect of aspect application such as finish, therefore, the phosphating coat crystalline state is detected seem particularly important.At present, the method for detection phosphating coat has: the heavy method of film, copper sulphate pitting test, salt water test, electrochemical impedance method and SEM observation etc.The heavy method of film mainly is to measure the size of phosphating coat weight, and this method can not detect the crystalline state of phosphating coat; The copper sulphate pitting test can only detect the compactness of phosphating coat, can not the crystalline state of phosphating coat comprehensively be detected; Salt water test is to detect the corrosion proof main method of phosphating coat, because test condition is relatively harsher, and the test period is long, introduces bigger personal error easily simultaneously; The electrochemical impedance method be can be correctly and a kind of digital test technology of objective detection phosphorization film quality, but this method data analysis be too numerous and diverse, simultaneously because electrolytic solution commonly used is 3.5%NaCl solution, and Cl in this solution
-Aggressivity stronger, and the corrosion stability of phosphating coat is relatively poor, when phosphating coat is immersed in the electrolytic solution, may make phosphating coat change of properties, increase or reduce the porosity of phosphating coat, perhaps change the interfacial structure of matrix/phosphating coat etc., the result of influence test; SEM observe be detect at present phosphorization film quality the most intuitively, the most compellent method, but this method needs special instrument and equipment, complicated operation needs the operating personnel of specialty, therefore can not use widely.
In sum, the method that detects phosphating coat at present exists following shortcoming:
1, detection is not comprehensive: can not the crystalline state of phosphating coat comprehensively be detected, can only detect at the local characteristics of phosphating coat crystalline state;
2, detection accuracy is poor: the test condition harshness, and test period is long, and personal error is bigger;
3, data analysis is numerous and diverse;
4, complicated operation needs special testing equipment;
5, the electrolytic solution aggressivity is strong, easily causes the test error of phosphorization film quality.
Summary of the invention
At the existing existing problem of method that detects phosphorization film quality, the object of the present invention is to provide a kind of detection method that detects comprehensive, accurate, easy phosphorization film quality.
To achieve the above object of the invention, solution of the present invention is: utilize continuous current/potentiostat, and test open circuit potential and the time relation curve of phosphating coat in phosphate solution, the time that flex point occurs according to this curve is detected the quality of phosphating coat.
Open circuit potential is meant that metal is immersed in the electrolytic solution, the electrode potential of metal when not having extrinsic current to pass through, and it often changes with the grade variation of condition of the one-tenth of the kind of electrode, electrolytic solution.It is because when the phosphatization plate immerses in the electrolytic solution that flex point appears in the open circuit potential of different phosphatization plates and time relation curve, at first test the open circuit potential and the time relation curve of phosphating coat, because phosphating coat is very thin, the corrosion stability of phosphating coat is relatively poor simultaneously, so phosphating coat will be exposed substrate metal by " puncture " soak certain hour in electrolytic solution after, owing to the difference of phosphating coat and substrate metal composition has caused open circuit potential and time relation curve flex point to occur, the time that this flex point occurs represents phosphating coat by the time of " puncture ", the length of this time is being represented the quality of phosphorization film quality, phosphorization film quality is good more, and the time that flex point occurs can be long more.The quality of isonomic phosphorization film quality depends primarily on size, density and the homogeneity of this phosphating coat crystal grain, and the zone that the fine and close no phosphatization of crystallite dimension tiny (usually less than 4 μ m), crystal grain does not go up and the phosphorization film quality of homogeneous grain size are good.
Concrete grammar is: will be processed into surface area through the model of phosphatization and be not less than 1cm
2Test piece, adopt the three-electrode electro Chemical test macro, wherein working electrode (promptly studying electrode) is that test piece to be measured, contrast electrode are that mercurous chloride electrode (SCE), auxiliary electrode are platinum gauze, the electrolytic solution solute concentration is 0.45%～0.55% potassium dihydrogen phosphate test solution according to mass percent, carry out the test of open circuit potential and time relation curve at ambient temperature, after flex point appearred in curve, the time of flex point appearred in record, detected the quality of phosphating coat according to the time that flex point occurs.
During the time t that occurs when flex point≤300s, phosphorization film quality is poor; When flex point time of occurrence 300s＜t≤700s, phosphorization film quality is general; When flex point time of occurrence 700s＜t≤1000s, phosphorization film quality is good; During the time t that flex point occurs＞1000s, phosphorization film quality is fine.
The present invention has following beneficial effect:
(1) this method is not subjected to interference from human factor, and testing liquid is little to the destruction of phosphating coat, can reflect the difference of different phosphorization film qualities with the numerical value that quantizes, and testing result is accurate.
(2) various characteristics of this method synthesis phosphating coat crystalline state reflects the quality of phosphating coat, can comprehensively reflect the quality of phosphating coat.
(3) this method test time is about 1000s, and test period is short.
(4) this method time of flex point occurring with the open circuit potential curve is detected the quality of phosphating coat, and test result analysis is simple.
(5) this method uses equipment simple, easy to operate.
Description of drawings
The open circuit potential curve map of Fig. 1 a plate;
The SEM of Fig. 2 a plate observes figure;
The open circuit potential curve map of Fig. 3 b plate;
The SEM of Fig. 4 b plate observes figure;
The open circuit potential curve map of Fig. 5 c plate;
The SEM of Fig. 6 c plate observes figure.
The open circuit potential curve map of Fig. 7 d plate;
The SEM of Fig. 8 d plate observes figure.
Embodiment
Below detect by phosphorization film quality 4 kinds of different phosphating coats, most preferred embodiment of the present invention is described.
Step 1, get a, b, four kinds of models of c, d with different phosphating coats.
Step 2, the test piece of above-mentioned model being processed into 100mm * 100mm.
Step 3, utilize M273 type continuous current/potentiostat, adopt the three-electrode electro Chemical test macro, in mass percent is in 0.5% potassium dihydrogen phosphate, respectively the test of open circuit potential curve is carried out in a, b, four kinds of test pieces with different phosphating coats of c, d, when flex point appears in the open circuit potential curve, end of test (EOT), the time that the record flex point occurs, the test polarization curve is seen Fig. 1, Fig. 3, Fig. 5, Fig. 7.
Step 4, the time that occurs according to flex point on the polarization curve that records in the step 3, the phosphorization film quality that pair has different phosphating coat test pieces according to table 1 detects, and the results are shown in Table 2.Table 1 detects table for phosphorization film quality, and table 2 is the testing result of the phosphorization film quality of a, b, c, four kinds of different phosphating coats of d.
Table 1 phosphorization film quality detects table
| The phosphorization film quality grade | Fine | Good | Generally | Difference |
| The time t that flex point occurs, s | ＞1000 | 700＜t≤1000 | 300＜t≤700 | ≤300 |
The assay of table 2a, b, c, four kinds of phosphorization film qualities of d
| Model | Flex point time of occurrence t, s | The assay of phosphorization film quality |
| a | 240 | Difference, phosphating coat crystal grain is thick, and is inhomogeneous, and zone, many places phosphatization does not go up |
| b | 630 | Generally, phosphating coat is thicker, and evenly, the regional area phosphatization does not go up |
| c | 780 | Good, phosphating coat crystal grain is more tiny, even, fine and close |
| d | 1050 | Fine, phosphating coat crystal grain is tiny, even, fine and close |
Above-mentioned 4 kinds of different phosphating coats are carried out SEM observe, observations is seen Fig. 2, Fig. 4, Fig. 6, Fig. 8.After the assay of table 2 contrasted with the observations of Fig. 2, Fig. 4, Fig. 6 and Fig. 8 respectively, can find: the present invention detects the result of phosphorization film quality and there is this good consistance in result that SEM observes.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010201646.8A CN102269729B (en) | 2010-06-07 | 2010-06-07 | Method for detecting quality of phosphating film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010201646.8A CN102269729B (en) | 2010-06-07 | 2010-06-07 | Method for detecting quality of phosphating film |
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| CN102269729A true CN102269729A (en) | 2011-12-07 |
| CN102269729B CN102269729B (en) | 2014-11-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376072A (en) * | 2021-05-14 | 2021-09-10 | 唐山钢铁集团有限责任公司 | Method for measuring porosity of phosphating film of steel plate |
| CN120725517A (en) * | 2025-06-19 | 2025-09-30 | 江苏威诺检测技术有限公司 | A data visualization display system and method based on data analysis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0569826A1 (en) * | 1992-05-12 | 1993-11-18 | Hughes Aircraft Company | Method and system for monitoring quality of phosphate coating |
| CN1854727A (en) * | 2005-04-29 | 2006-11-01 | 宝山钢铁股份有限公司 | Borate salt solution for cold-rolling plate bonderizing prediction |
-
2010
- 2010-06-07 CN CN201010201646.8A patent/CN102269729B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0569826A1 (en) * | 1992-05-12 | 1993-11-18 | Hughes Aircraft Company | Method and system for monitoring quality of phosphate coating |
| CN1854727A (en) * | 2005-04-29 | 2006-11-01 | 宝山钢铁股份有限公司 | Borate salt solution for cold-rolling plate bonderizing prediction |
Non-Patent Citations (4)
| Title |
|---|
| A. LOSCH等: "A new electrochemical method for the determination of the free surface of phosphate layers", 《APPLIED SURFACE SCIENCE》, vol. 52, 31 December 1991 (1991-12-31) * |
| G.LENDVAY-GYORIK: "A simple testing method for quality control of phosphate coatings based on impedance measurements", 《JOURNAL OF APPLIED ELECTROCHEMISTRY》, vol. 32, 31 December 2002 (2002-12-31) * |
| M.KHALEGHI等: "Characteristics of manganese phosphate coatings for wear-resistance applications", 《WEAR》, vol. 55, 31 December 1979 (1979-12-31) * |
| 林碧兰 等: "磷化膜电化学测试技术的研究进展", 《腐蚀科学与防护技术》, 30 November 2006 (2006-11-30) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376072A (en) * | 2021-05-14 | 2021-09-10 | 唐山钢铁集团有限责任公司 | Method for measuring porosity of phosphating film of steel plate |
| CN113376072B (en) * | 2021-05-14 | 2022-10-18 | 唐山钢铁集团有限责任公司 | Method for measuring porosity of phosphating film of steel plate |
| CN120725517A (en) * | 2025-06-19 | 2025-09-30 | 江苏威诺检测技术有限公司 | A data visualization display system and method based on data analysis |
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