CN103499319A - Method for measuring thickness of inner rust layer of weather resistant steel - Google Patents
Method for measuring thickness of inner rust layer of weather resistant steel Download PDFInfo
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- CN103499319A CN103499319A CN201310404602.9A CN201310404602A CN103499319A CN 103499319 A CN103499319 A CN 103499319A CN 201310404602 A CN201310404602 A CN 201310404602A CN 103499319 A CN103499319 A CN 103499319A
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Abstract
The invention provides a method for measuring the thickness of an inner rust layer of weather resistant steel. A scanning electron microscope is utilized to test, energy disperse spectroscopy scanning electron beams are utilized to scan along the selected linear track of the cross section of the rust layer, wherein a scanning line is perpendicular to the dividing line of the rust layer and a base material, the scanning electron beams are perpendicular to the cross section of the base material and the cross section of the rust layer; the thickness of the rust layer in metal is determined according to the change of the strength of the counting rate of a Fe element and a Cr element, the gathering beginning position of the Cr element is used as the starting point, samples conduct line scanning on the rust layer regions from outside to inside, the zoom low point of the Fe element is the dividing point of the base material and the rust layer, namely the terminal point of the inner rust layer, and the distance between the starting point and the terminal point is the thickness of the inner rust layer. According to the method, interference by human factors is small, accuracy of measuring the thickness of the inner rust layer of the weather resistant steel can be remarkably improved, and the problem that the measuring result is inaccurate in the prior art is effectively solved.
Description
Technical field
The invention belongs to the detection technique field, particularly a kind of for measuring the method for the interior rusty scale thickness of weathering steel (weather resisting steel).
Background technology
Weathering steel surface in corrosion environment can generate protective rust, and weather-resistance is preferably arranged, and it is applied widely.Surface Rust of Weathering Steel can be divided into interior rusty scale and outer rusty scale, and interior rusty scale mainly is comprised of alpha-feooh.Contain the Cr element in the weathering steel rusty scale, the existence of Cr in rusty scale can be accelerated the alpha-feooh transformation of γ-FeOOH to thermodynamics stable state, and alpha-feooh, with needle-like or the growth of rectangle sheet, causes interior rusty scale to present with the fine and close state of sheet.Cr has partly replaced the position of Fe in the alpha-feooh simultaneously, has formed the oxyhydroxide of bianry alloy element, and this oxyhydroxide has cation selective, stops Cl
-, SO
3 2-to the matrix surface infiltration, thereby make rusty scale there is protective effect.Outer rusty scale mainly is comprised of γ-FeOOH, and γ-FeOOH occurs with the combinate form of the plane of rupture of class floweriness, causes outer rusty scale loose, and surface exists many holes and crackle, a little less than protective effect.The inside and outside rusty scale of weathering steel is differentiated to the protective capability of matrix.For the Mechanism of Protection of more deep research weathering steel rusty scale, to the thickness measure of inside and outside rusty scale, be very necessary.
At present, the method for distinguishing inside and outside rusty scale is mainly Mechanical Method and microscopic method.Mechanical Method is the outer rusty scale of phased separation and interior rusty scale from outside to inside, and collection respectively, after grinding, use X-ray diffraction to analyze respectively structure and the composition of inside and outside rusty scale.But the method can not be measured inside and outside rusty scale thickness.Microscopic method is to utilize metaloscope or scanning electron microscope to observe structure and the pattern near the corrosion scales of matrix, with the content of thermodynamics stable state material in the spectral analysis corrosion product, carry out the compactness of indirect reaction rusty scale etc. by nitrogen absorption investigation corrosion product grain size.Distinguish inside and outside rusty scale according to the density of rusty scale, color etc., thereby according to the thickness of the tape measure rusty scale of image.Although the method can be distinguished the protectiveness of inside and outside rusty scale qualitatively, the result of its quantitatively characterizing rusty scale thickness is affected by human factors greatly, and therefore the thickness of measured rusty scale is also inaccurate.
In sum, existing measuring method also can't be measured the thickness of rusty scale in weathering steel exactly, awaits carrying out in this regard related work.
Summary of the invention
The present invention aims to provide a kind of simple, can reduce interference from human factor, thereby measures exactly the method for rusty scale thickness in weathering steel.
For this reason, the solution that the present invention takes is:
The measuring method of rusty scale thickness in a kind of weathering steel, its concrete grammar is:
At first, adopt scanning electron microscope to be tested weathering steel rusty scale zone, scanning electron microscope test vacuum tightness is 7 * 10
-3～10
-6pa, operating distance is 10mm; Utilize energy spectrometer to carry out line sweep to the rusty scale zone, the selected straight path of xsect that scanning beam is rusty scale along sample surfaces is that sweep trace is scanned, sweep trace is perpendicular to the boundary of rusty scale and base material, and scanning beam is perpendicular to the xsect of base material and rusty scale; Determine the thickness of rusty scale in metal by the variation of Fe element and Cr element count rate intensity, the Cr element of take starts enrichment place as starting point, the sample ecto-entad carries out line sweep to the rusty scale zone, the low spot that the Fe element skyrockets is matrix and rusty scale separation, be interior rusty scale terminal, the distance between starting point and terminal is interior rusty scale thickness.
The power spectrum signal drift amount of described energy spectrometer is not more than 0.1mm, and the accelerating potential of scanning beam is 20kV.
Beneficial effect of the present invention is:
The inventive method is simple; convenient operation; be subject to interference from human factor few; can significantly improve the accuracy of rusty scale thickness measure in weathering steel; solved the inaccurate problem of test result that prior art exists, for furtheing investigate and utilizing the Mechanism of Protection of weathering steel rusty scale that the data basis is provided.
The accompanying drawing explanation
Fig. 1 is embodiment 1 rusty scale Fe element and Cr elemental line scan energy spectrogram;
Fig. 2 is embodiment 1 rusty scale zone cross-sectional morphology figure;
Fig. 3 is embodiment 2 rusty scale Fe elements and Cr elemental line scan energy spectrogram;
Fig. 4 is embodiment 2 rusty scale zone cross-sectional morphologies.
Embodiment
Below, by embodiment, the present invention will be further described.
Instrument in embodiment:
Scanning electron microscope: the QUANTA400HV type scanning electron microscope (SEM) that FEI Co. produces;
Energy spectrometer: the PHOENIX type X-gamma ray spectrometer (EDS) that U.S. EDAX company produces.
Embodiment 1:
1. the pre-treatment of sample: the weathering steel sample that carries out exposure test at Anshan Atmospheric Corrosion Test Sites is carried out to sample cutting vertically, with conductive mosaic material edge sample, make sample.Xsect polishes through 240#, 500#, 800#, 1000# waterproof abrasive paper successively, then uses the antiscuffing paste polishing, and cleans up the rear non-felt polishing of using with anhydrous alcohol, obtains the plane of an energy horizontal positioned.
2. the test of testing sample:
The professional sample stage that the sample prepared is equipped with together with scanning electron microscope is fixed in the specimen pallet of scanning electron microscope, vacuumizes, and reaches the vacuum tightness 7 * 10 of test request
-3after Pa, tested.
Regulate the specimen pallet of scanning electron microscope, make the xsect of observed sample vertical with the scanning electron microscope beam direction, and parallel with the view screen vertical direction of scanning electron microscope.
The scanning electron microscope operating distance is 10mm, move horizontally sample tray, find and the xsect of confirmatory sample on the boundary of matrix and rusty scale, from boundary, utilize energy spectrometer ecto-entad under the accelerating potential 20.00kV of scanning beam condition to carry out line sweep to the rusty scale zone, image data, utilize the Origin software data processing, obtains energy spectrogram as shown in Figure 1.Wherein Cr element count rate intensity data amplifies 10 times of processing.As Fig. 1, spectrogram can be divided into to edge material, rusty scale and matrix three parts.The thickness of interior rusty scale is determined in the variation of the Fe element in rusty scale and Cr element count rate intensity per sample.It is starting point that the Cr element starts enrichment, and the low spot that the Fe element skyrockets is terminal, and the distance between starting point and terminal is interior rusty scale thickness.According to this kind of method, in embodiment 1 sample, rusty scale thickness is 7.24mm.
In the metal that application the present invention records, the rusty scale thickness results is accurate.
Utilize sem observation rusty scale zone xsect, as high-visible as Fig. 2, interior rusty scale is close proximity on the interface of steel and rust, and color is darker, and tack is good, and structure is finer and close; Outer rusty scale color is slightly shallow, and structure is more loose.Can measure the thickness of interior rusty scale according to image rulers, be 7.8mm.
Embodiment 2:
The weathering steel sample of sample at Air of Guangzhou corrosion test station, carrying out exposure test.The pre-treatment of sample and the test of testing sample are as embodiment 1.The scanning electron microscope operating distance is 10mm, utilizes energy spectrometer ecto-entad under the accelerating potential 20kV of scanning beam condition to carry out line sweep to the rusty scale zone, and the Origin software data processing obtains energy spectrogram as shown in Figure 3.Wherein Cr element count rate intensity data amplifies 10 times of processing.As Fig. 3, spectrogram can be divided into to edge material, rusty scale and matrix three parts.The thickness of interior rusty scale is determined in the variation of the element of Fe element in rusty scale and Cr element count rate intensity per sample.It is starting point that the Cr element starts enrichment, and the low spot that the Fe element skyrockets is terminal, and the distance between starting point and terminal is interior rusty scale thickness.According to this kind of method, in embodiment 2 samples, rusty scale thickness is 10.5mm.
In the metal that application the present invention records, the rusty scale thickness results is accurate.
Utilize sem observation rusty scale zone xsect, as high-visible as Fig. 4, interior rusty scale is close proximity on the interface of steel and rust, and color is darker, and tack is good, and structure is finer and close; Outer rusty scale color is slightly shallow, and structure is more loose.The thickness that can measure interior rusty scale according to image rulers is 8.7mm.
Claims (2)
1. the measuring method of the interior rusty scale thickness of weathering steel, is characterized in that, concrete grammar is:
At first, adopt scanning electron microscope to be tested weathering steel rusty scale zone, scanning electron microscope vacuum tightness is 7 * 10
-3～10
-6pa; Utilize energy spectrometer to carry out line sweep to the rusty scale zone, the selected straight path of xsect that scanning beam is rusty scale along sample surfaces is that sweep trace is scanned, sweep trace is perpendicular to the boundary of rusty scale and base material, and scanning beam is perpendicular to the xsect of base material and rusty scale; Determine the thickness of rusty scale in metal by the variation of Fe element and Cr element count rate intensity, the Cr element of take starts enrichment place as starting point, the sample ecto-entad carries out line sweep to the rusty scale zone, the low spot that the Fe element skyrockets is matrix and rusty scale separation, be interior rusty scale terminal, the distance between starting point and terminal is interior rusty scale thickness.
2. the measuring method of rusty scale thickness in weathering steel according to claim 1, is characterized in that, the power spectrum signal drift amount of described energy spectrometer is not more than 0.1mm, and the accelerating potential of scanning beam is 20kV.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954243A (en) * | 2014-04-22 | 2014-07-30 | 北京理工大学 | Rotation seal boundary film thickness measuring method |
| CN105486252A (en) * | 2014-09-19 | 2016-04-13 | 鞍钢股份有限公司 | Compensation method for measured thickness of zinc aluminized layer |
| CN107271355A (en) * | 2017-05-27 | 2017-10-20 | 双登集团股份有限公司 | Grid corrosion degree quantitative determination method |
| CN109425315A (en) * | 2017-08-31 | 2019-03-05 | 长鑫存储技术有限公司 | test carrier and test method of semiconductor structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954243A (en) * | 2014-04-22 | 2014-07-30 | 北京理工大学 | Rotation seal boundary film thickness measuring method |
| CN105486252A (en) * | 2014-09-19 | 2016-04-13 | 鞍钢股份有限公司 | Compensation method for measured thickness of zinc aluminized layer |
| CN107271355A (en) * | 2017-05-27 | 2017-10-20 | 双登集团股份有限公司 | Grid corrosion degree quantitative determination method |
| CN109425315A (en) * | 2017-08-31 | 2019-03-05 | 长鑫存储技术有限公司 | test carrier and test method of semiconductor structure |
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