CN113533396A - Heavy rail sample iron scale phase detection method - Google Patents
Heavy rail sample iron scale phase detection method Download PDFInfo
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- CN113533396A CN113533396A CN202110695062.9A CN202110695062A CN113533396A CN 113533396 A CN113533396 A CN 113533396A CN 202110695062 A CN202110695062 A CN 202110695062A CN 113533396 A CN113533396 A CN 113533396A
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- ray diffractometer
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- 238000001514 detection method Methods 0.000 title claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims description 24
- 229910052742 iron Inorganic materials 0.000 title claims description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 238000007405 data analysis Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000843 powder Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/33—Accessories, mechanical or electrical features scanning, i.e. relative motion for measurement of successive object-parts
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a heavy rail sample iron oxide scale phase detection method, which comprises the following steps: sampling; preparing a sample: sequentially placing plasticine and a sample with a certain area on a flat bottom plate according to the sequence from bottom to top, and leveling the uneven part of the sample by using a flatting machine; disassembling an X-ray diffractometer OEC sample table, and putting the whole sample prepared in the first step into the OEC sample table; an X' PertPRO type X-ray diffractometer produced by Panakg is used for compiling a test program, the scanning range 2 theta is 10-110 degrees, the scanning stepping width is 0.03 degrees, and the scanning speed is 0.3 degrees/s; data analysis was performed using the H i ghScore application software. The invention aims to provide a method for detecting the oxide scale phase of a heavy rail sample, which is an important method in the field of phase detection of an X-ray diffractometer and is particularly suitable for the oxide scale phase analysis of a massive heavy rail sample with an uneven surface.
Description
Technical Field
The invention relates to the field of metal material detection, in particular to the field of large instrument testing, and relates to a method for detecting the oxide scale phase of a heavy rail sample by using an X-ray diffractometer.
Background
In the process of hot rolling of heavy rails, iron scales with certain thickness are usually formed on the surfaces of the steel rails, and the phase compositions of the iron scales are different due to the influence of various aspects of steel grade chemical components, cooling water media, a phosphorus removal system and the like. The iron scale is generally composed of Fe3O4, Fe2O3, FeO and other impurities, and the surface of the iron scale is preferably formed into compact iron scale which is not easy to fall off, so that the iron scale can play a good role in corrosion resistance. Therefore, the method has important significance for phase research on the iron scale on the surface of the heavy rail.
X-ray diffractometry (XRD) in performing phase analysis, it is generally required to prepare a sample into a powder having a particle size of about 200 mesh. The sample preparation device comprises from bottom to top: sample pieces, tabletting plates. The powder sample is placed into the groove of the sample piece, then a technician pushes the pressing flat plate on the sample piece in a finger pressing mode, so that the powder sample in the groove of the sample piece is molded and the purpose of leveling is achieved, and finally the powder sample is placed on a spring clamp sample table for detection, thereby ensuring the accuracy of data.
The surface of a massive heavy rail sample (with the height of about 20mm) has radian (because the finished material has shape requirement), the requirement of XRD on the surface smoothness of the sample cannot be met, and a spring clamp (with the maximum thickness of 5mm) sample table cannot be used, so that the phase analysis of the steel rail sample iron oxide scale has limitation.
Disclosure of Invention
The invention aims to provide a method for detecting the oxide scale phase of a heavy rail sample, which is an important method in the field of phase detection of an X-ray diffractometer and is particularly suitable for the oxide scale phase analysis of a massive heavy rail sample with an uneven surface.
In order to solve the technical problems, the invention adopts the following technical scheme:
a heavy rail sample scale phase detection method mainly comprises the following steps:
1) and (6) sampling. And (4) performing representative sampling according to the performance requirement of the heavy rail product on the surface iron scale. The sample is taken from the circular arcs on two sides of the tread of the railhead, and the size is as follows: 20 to 30mm × 20 to 30 mm.
2) And (5) preparing a sample. The first step is as follows: a leveling bottom plate is taken and placed on an objective table of a flattening machine, then plasticine and a sample with a certain area are sequentially placed on the leveling bottom plate according to the sequence from bottom to top, and the flattening machine is used for compensating the uneven part of the sample, so that the problem that the detection surface of the sample is uneven is solved. The second step is that: the sample stage of the X-ray diffractometer OEC (texture) is disassembled, and the sample prepared in the first step is integrally placed in the sample stage of the OEC (texture), so that the use height of the sample can be increased, and the problems of high block sample and large volume are solved.
3) And (5) detecting a phase. An X' Pert PRO type X-ray diffractometer produced by Panakg is used for programming a test program, the scanning range 2 theta is 10-110 degrees, the scanning stepping width is 0.03 degrees, and the scanning speed is 0.3 degrees/s.
4) And (6) analyzing results. Data analysis was performed using High Score application software to generate results.
Further, the X-ray tube of the X' PertPRO type X-ray diffractometer used a cobalt target, and the phase detection voltage was 35KV and the current was 50 mA.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention overcomes the difficulties of large block sample and uneven detection surface in the sample preparation process, and limits the phase detection to the detection range of the powdery sample. Meanwhile, the sample in-situ detection replaces the powder sample preparation, so that the sample preparation error caused by the fact that a steel base of the powder sample preparation is easy to mix is reduced.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is a photomicrograph of a heavy rail sample.
FIG. 2 is a diagram of a sample preparation process.
FIG. 3 is a diagram showing the overall effect after sample preparation.
FIG. 4 is a graph showing the effect of the sample after being loaded into the OEC sample stage.
FIG. 5 shows the results of phase detection.
Detailed Description
Examples
The sample was taken from the U71Mn railhead arc, the dimensions of which were 20mm X30 mm X20 mm, as shown in FIG. 1, and the test surface was a tread (with radian). A piece of plasticine is taken and placed on a flat bottom plate, a sample is placed above the plasticine, a flatting machine is used for slightly pressing downwards, the position where the sample is not flat is filled, and the filled sample is shown in figure 3. The whole was placed in a disassembled sample stage of an X-ray diffractometer OEC (texture), see fig. 4.
Setting a test program: the X-ray tube uses a cobalt target, the phase detection voltage is 35KV, the current is 50mA, the scanning range 2 theta is 10-110 degrees, the scanning stepping width is 0.03 degrees, and the scanning speed is 0.3 degrees/s.
After the measurement, the data was imported using High Score application software to analyze the phase composition. The results are shown in FIG. 5. The result shows that the iron scale composition substances (the content is from high to low) at the rail head arc of the U71Mn are as follows: fe3O4，Fe2O3FeO. The detection result provides data support for parameter setting, cooling water medium adjustment and the like of the U71Mn hot-rolling dephosphorization system.
The preferred embodiments of the present invention are described without limiting the scope of the present invention, and various modifications and improvements of the technical solution of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, which is defined by the claims.
Claims (2)
1. A heavy rail sample scale phase detection method is characterized by comprising the following steps:
1) sampling
Performing representative sampling according to the performance requirement of the heavy rail product on the surface iron scale; the sample is taken from the circular arcs on two sides of the tread of the railhead, and the size is as follows: 20-30 mm × 20-30 mm;
2) sample preparation
The first step is as follows: placing a flat bottom plate on an objective table of a flattening machine, sequentially placing plasticine and a sample with a certain area on the flat bottom plate from bottom to top, and flattening the uneven part of the sample by using the flattening machine;
the second step is that: disassembling an X-ray diffractometer OEC sample table, and putting the whole sample prepared in the first step into the OEC sample table;
3) phase detection
An X' PertPRO type X-ray diffractometer produced by Panakg is used for programming a test program, the scanning range 2 theta is 10-110 degrees, the scanning stepping width is 0.03 degrees, and the scanning speed is 0.3 degrees/s.
4) Analysis of results
Data analysis was performed using the HighScore application software to generate results.
2. The method for detecting the oxide scale phase of the heavy rail sample according to claim 1, wherein: the X-ray tube of the X' PertPRO type X-ray diffractometer uses a cobalt target, and the phase detection voltage is 35KV and the current is 50 mA.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110695062.9A CN113533396A (en) | 2021-06-23 | 2021-06-23 | Heavy rail sample iron scale phase detection method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110695062.9A CN113533396A (en) | 2021-06-23 | 2021-06-23 | Heavy rail sample iron scale phase detection method |
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| CN113533396A true CN113533396A (en) | 2021-10-22 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001281175A (en) * | 2000-03-31 | 2001-10-10 | Kawasaki Steel Corp | Measuring method for metal surface oxide and x-ray diffraction device |
| CN203053897U (en) * | 2013-01-12 | 2013-07-10 | 山东轻工业学院 | Block sample table for x-ray diffractometer |
| CN104713759A (en) * | 2015-02-13 | 2015-06-17 | 东北大学 | Method for detecting surface oxidized scale sample of hot rolled steel plate |
| CN108709516A (en) * | 2018-05-11 | 2018-10-26 | 首钢集团有限公司 | A method of measuring steel surface iron scale thickness |
| CN111678927A (en) * | 2020-06-08 | 2020-09-18 | 首钢集团有限公司 | Method for analyzing oxide on surface of steel |
| KR20210037113A (en) * | 2019-09-27 | 2021-04-06 | 현대제철 주식회사 | Method of fabricating specimens for electron backscattering diffraction (ebsd) and analysis method of scale structure of hot rolled steel sheet using the same |
-
2021
- 2021-06-23 CN CN202110695062.9A patent/CN113533396A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001281175A (en) * | 2000-03-31 | 2001-10-10 | Kawasaki Steel Corp | Measuring method for metal surface oxide and x-ray diffraction device |
| CN203053897U (en) * | 2013-01-12 | 2013-07-10 | 山东轻工业学院 | Block sample table for x-ray diffractometer |
| CN104713759A (en) * | 2015-02-13 | 2015-06-17 | 东北大学 | Method for detecting surface oxidized scale sample of hot rolled steel plate |
| CN108709516A (en) * | 2018-05-11 | 2018-10-26 | 首钢集团有限公司 | A method of measuring steel surface iron scale thickness |
| KR20210037113A (en) * | 2019-09-27 | 2021-04-06 | 현대제철 주식회사 | Method of fabricating specimens for electron backscattering diffraction (ebsd) and analysis method of scale structure of hot rolled steel sheet using the same |
| CN111678927A (en) * | 2020-06-08 | 2020-09-18 | 首钢集团有限公司 | Method for analyzing oxide on surface of steel |
Non-Patent Citations (2)
| Title |
|---|
| 席艳君等: "磨损对U71Mn 材料表面高温氧化行为的影响", 《表面技术》, vol. 50, no. 5, pages 292 - 293 * |
| 贾志芳;张贵杰;胡德红;: "热轧带钢表面及炉辊氧化铁皮的分析", 钢铁钒钛, no. 06 * |
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Application publication date: 20211022 |