CN102279199A - Quantitative detection method for precipitated phases in grain-oriented silicon steel based on component classification - Google Patents
Quantitative detection method for precipitated phases in grain-oriented silicon steel based on component classification Download PDFInfo
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- CN102279199A CN102279199A CN2011101945283A CN201110194528A CN102279199A CN 102279199 A CN102279199 A CN 102279199A CN 2011101945283 A CN2011101945283 A CN 2011101945283A CN 201110194528 A CN201110194528 A CN 201110194528A CN 102279199 A CN102279199 A CN 102279199A
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Abstract
The invention relates to a quantitative detection method for precipitated phases in grain-oriented silicon steel based on component classification. The method comprises the following steps: extracting the precipitated phases in a sample and preparing the precipitated phases into a transmission electron microscope sample; observing the transmission electron microscope sample in a transmission electron microscope and randomly selecting and analyzing a field coverage; running a feature analysis program in impurity analysis software and collecting high contrast images of the precipitated phases; running an X-ray energy spectrum analysis program of the feature analysis program, finishing the information collection for all the precipitated phases in the selected field coverage and storing the information as a database file; and inputting the weight percent or concentration of chemical elements in a condition setting frame of the feature analysis program and running an impurity classifying program, thereby acquiring quantitative detection results of different precipitated phases. Under the condition of using the quantitative detection method provided by the invention, the precipitated phases become colorful and the carbon support films become off-white so that the precipitated phases and the carbon support films can be easily identified, and the information of the precipitated phases is stored as the database file so that statistical classification becomes convenient. The quantitative detection method provided by the invention has the advantages that the collected information of the precipitated phases is comprehensive and accurate and the detection is quick and convenient.
Description
Technical field
The present invention relates to quantitative detecting method, is the quantitative detecting method that precipitated phase is pressed the composition classification in a kind of orientation silicon steel specifically.
Background technology
Type, size, form and the distribution of each production process stage precipitated phase of orientation silicon steel is the key factor of its texture of control, performance.But the precipitated phase quantity in the orientation silicon steel is many, size is tiny, type is complicated, and the precipitated phase of wherein any two or three type is usually compound separates out.Classic method is in the face of hundreds of nanoscale precipitated phase in each visual field under the transmission electron microscope, screen according to its shape characteristic, with energy spectrometer (EDS) precipitated phase of selecting is carried out the power spectrum point analysis one by one, the range of size of complicate statistics precipitated phase type, measurement precipitated phase is assessed its primary and secondary then.Not only workload is huge, and be difficult to distinguish type form identical, range of size is close but quantity, precipitated phase that ratio is different.
Japanese patent application JP6073453 discloses a kind of image (ICP) analytical approach that adopts and has determined anneal for the first time content of back Mn and Al of the unidirectional electric steel plate of high flux density, thereby determine the method for MnS and AlN precipitated phase content, its shortcoming is to observe pattern and measurement size, and type may be omitted.
Japanese patent application JP2004177266 discloses a kind of detection method of utilizing the defective that is caused by precipitated phase in the ultrasound examination steel plate production run, and its shortcoming is precipitated phase not to be classified quantitatively by composition, and is not accurate and comprehensive enough.
The inclusion analysis software of Oxford instrument company (THE INCLUSION CLASSIFIRE) is applicable under the scanning electron microscope micron order in the metallographic specimen carried out the classification analysis of composition, size to millimetre-sized snotter, but nano level precipitated phase is differentiated difficulty even can't be analyzed.Therefore, in a kind of orientation silicon steel that can comprehensively accurately collect precipitated phase information and efficient and convenient detection of design precipitated phase to press the quantitative detecting method of composition classification very necessary.
Summary of the invention
The purpose of this invention is to provide in a kind of orientation silicon steel that can comprehensively accurately collect precipitated phase information and efficient and convenient detection precipitated phase and press the quantitative detecting method of composition classification.
For achieving the above object, the present invention adopts following technical scheme: precipitated phase is pressed the quantitative detecting method of composition classification in a kind of orientation silicon steel, may further comprise the steps:
A. extract the precipitated phase in the orientation silicon steel sample, be prepared into transmission electron microscope sample, select the supporting network different to support carbon film with the precipitated phase chemical constitution;
B. in transmission electron microscope, observe sample, regulate enlargement factor to clearly differentiating precipitated phase, for the sample that precipitated phase is evenly distributed, 2～3 visual fields of picked at random are analyzed, for the sample of precipitated phase non-uniform Distribution, concentrating the zone that distributes and disperse to distribute respectively to choose 2 visual fields analyses;
C. in THE INCLUSION CLASSIFIRE software, move INCA FEATURE program, collect the high contrast image of orientation silicon steel precipitated phase, regulate the gray-scale value scope observation image change that characteristics of image detects, become colour and carbon support membrane maintenance canescence up to all precipitated phases;
D. move the X-ray energy spectrum routine analyzer of INCA FEATURE program, finish all precipitated phases in the selected visual field information such as composition, size automatic collection and save as database file;
E. import the percent by weight or the concentration of chemical element at the condition setting frame of INCA FEATURE program, move the snotter sort program, obtain quantity and number percent, area and number percent, the average-size of precipitated phase and the detection by quantitative results such as precipitated phase quantity in the different size scope of dissimilar precipitated phases.
Further, the precipitated phase in the described extraction orientation silicon steel sample adopts the secondary carbon replica method.
Adopt the present invention, setting gray-scale value scope makes and separates out the colour that coordinates, the carbon support membrane becomes canescence to distinguish easily, avoids omitting; Information such as the composition of all precipitated phases, size are saved as database file, be convenient to statistical classification to obtain objective and accurate detection data.It is accurate comprehensively that the present invention collects precipitated phase information, detects efficient and convenient.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment, but this embodiment should not be construed as limitation of the present invention.
Embodiment 1
A. with 5% nital corrosion metallographic specimen, precipitated phase in the metallic matrix is partly protruded, putting into vacuum coater then is carbon film more than the 20nm at direct spraying plating one layer thickness of specimen surface, again sample is put in 5%～20% the nital and carries out the deep etch second time, carbon film is separated with matrix together with the precipitated phase that protrudes specimen surface, carbon film after separating transferred in 20% the nital and wash, moltenly remove residual matrix, move on in the alcohol at last and wash, pick up with the nickel supporting network;
B. observe sample in JEM2100F type transmission electron microscope, regulate enlargement factor to 20000 and times can clearly differentiate precipitated phase, the precipitated phase in this sample is evenly distributed, and 2 visual fields of picked at random are analyzed;
C. in the NCA energy spectrometer, open THEINCLUSION CLASSIFIRE software, operation INCA FEATURE program, collect the high contrast image of orientation silicon steel precipitated phase, regulate the gray-scale value scope observation image change that characteristics of image detects, all precipitated phases become colour and carbon support membrane maintenance canescence when gray-scale value is 3.02～64.83;
D. move the X-ray energy spectrum routine analyzer of INCA FEATURE program, finish all precipitated phases in the selected visual field information such as composition, size automatic collection and save as database file;
E. import the percent by weight of chemical element at the condition setting frame of INCA FEATURE program, operation snotter sort program, obtain the quantity and the number percent of dissimilar precipitated phases, area and number percent, detection by quantitative results such as precipitated phase quantity in the average-size of precipitated phase and the different size scope: the precipitated phase total amount is 477 in this visual field, main type is AlN+Cu2S, quantity accounts for 60.8%, secondly be AlN and AlN+MnS+Cu2S, account for 14.7% and 13% respectively, Cu2S+AlN accounts for 1.7%, MnS+Cu2S+AlN accounts for 3.6%, main chemical elements Al in the precipitated phase, Cu, the percentage by weight mean value of Mn is respectively 86.11%, 7.88%, 6.01%, precipitated phase total area number percent is 2.651%, average equivalent diameter is 0.05 μ m, what 70nm was following has 375, account for have 42 of 78.6%, 70～110nm, account for 8.8%.
Embodiment 2
A. with 5% nital corrosion metallographic specimen, precipitated phase in the metallic matrix is partly protruded, putting into vacuum coater then is carbon film more than the 20nm at direct spraying plating one layer thickness of specimen surface, again sample is carried out electropolishing, carbon film is separated with matrix together with the precipitated phase that protrudes specimen surface, the carbon film after separating is transferred in 20% the nital and washed, moltenly remove residual matrix, move on in the alcohol at last and wash, pick up with the nickel supporting network;
B. observe sample in JEM2100F type transmission electron microscope, regulate enlargement factor to 50000 and times can clearly differentiate precipitated phase, the precipitated phase in this sample is evenly distributed, and 2 visual fields of picked at random are analyzed;
C. in the NCA energy spectrometer, open THEINCLUSION CLASSIFIRE software, operation INCA FEATURE program, collect the high contrast image of orientation silicon steel precipitated phase, regulate the gray-scale value scope observation image change that characteristics of image detects, all precipitated phases become colour and carbon support membrane maintenance canescence when gray-scale value is 3.81～84.25;
D. move the X-ray energy spectrum routine analyzer of INCA FEATURE program, finish all precipitated phases in the selected visual field information such as composition, size automatic collection and save as database file;
E. import the percent by weight of chemical element at the condition setting frame of INCA FEATURE program, operation snotter sort program, obtain the quantity and the number percent of dissimilar precipitated phases, area and number percent, detection by quantitative results such as precipitated phase quantity in the average-size of precipitated phase and the different size scope: the precipitated phase total amount is 242 in this visual field, main type is AlN+Cu2S, quantity accounts for 73.3%, secondly be AlN and AlN+MnS+Cu2S, account for 20.2% and 5.3% respectively, Cu2S+AlN accounts for 1.2%, MnS+Cu2S+AlN accounts for 0.4%, main chemical elements Al in the precipitated phase, Cu, the percentage by weight mean value of Mn is respectively 83.52%, 15.57%, 0.91%, precipitated phase total area number percent is 4.786%, average equivalent diameter is 0.04 μ m, what 70nm was following has 210, account for have 15 of 86.8%, 70～110nm, account for 6.2%.
Embodiment 3
A. with 5% nital corrosion metallographic specimen, precipitated phase in the metallic matrix is partly protruded, dripping acetone at specimen surface then sticks acetate fibre paper, after the standing and drying acetate fibre paper uncovered together with the precipitated phase that protrudes specimen surface and put into vacuum coater and spray carbon, obtain the compound replica of secondary, again should compound replica put into acetone soln primary cellulose acetate film is dissolved, finally obtain the extraction carbon replica of precipitated phase, pick up with the nickel supporting network;
B. in JEM2100F type transmission electron microscope, observe sample, regulate enlargement factor to 20000 and times can clearly differentiate precipitated phase.Larger-size precipitated phase is the zonal arrangement feature in this sample, and the precipitated phase distribution uniform that size is tiny is concentrating the zone that distributes and disperse to distribute respectively to choose 2 visual fields analyses;
C. in the NCA energy spectrometer, open THE INCLUSION CLASSIFIRE running software INCA FEATURE program, collect the high contrast image of orientation silicon steel precipitated phase, regulate the gray-scale value scope observation image change that characteristics of image detects, all precipitated phases become colour and carbon support membrane maintenance canescence when gray-scale value is 8.51～81.43;
D. move the X-ray energy spectrum routine analyzer of INCA FEATURE program, finish all precipitated phases in the selected visual field information such as composition, size automatic collection and save as database file;
E. import the percent by weight of chemical element at the condition setting frame of INCA FEATURE program, operation snotter sort program, obtain the quantity and the number percent of dissimilar precipitated phases, area and number percent, detection by quantitative results such as precipitated phase quantity in the average-size of precipitated phase and the different size scope: the precipitated phase total amount is 285 in this visual field, main type is AlN+Cu2S, quantity accounts for 51.2%, secondly be AlN and AlN+MnS+Cu2S, account for 19.3% and 18.2% respectively, AlN+MnS accounts for 9.8%, Cu2S+AlN accounts for 1.4%, main chemical elements Al in the precipitated phase, Cu, the percentage by weight mean value of Mn is respectively 96.25%, 1.85%, 1.90%, precipitated phase total area number percent is 4.099%, average equivalent diameter is 0.07 μ m, what 70nm was following has 230, account for have 25 of 80%, 70～110nm, account for 8.8%.
The content that is not described in detail in this instructions belongs to the those skilled in the art known prior art.
Claims (2)
1. precipitated phase is pressed the quantitative detecting method of composition classification in the orientation silicon steel, may further comprise the steps:
A. extract the precipitated phase in the orientation silicon steel sample, be prepared into transmission electron microscope sample, select the supporting network different to support carbon film with the precipitated phase chemical constitution;
B. in transmission electron microscope, observe sample, regulate enlargement factor to clearly differentiating precipitated phase, for the sample that precipitated phase is evenly distributed, 2～3 visual fields of picked at random are analyzed, for the sample of precipitated phase non-uniform Distribution, concentrating the zone that distributes and disperse to distribute respectively to choose 2 visual fields analyses;
C. in THE INCLUSION CLASSIFI RE software, move INCA FEATURE program, collect the high contrast image of orientation silicon steel precipitated phase, regulate the gray-scale value scope observation image change that characteristics of image detects, become colour and carbon support membrane maintenance canescence up to all precipitated phases;
D. move the X-ray energy spectrum routine analyzer of INCA FEATURE program, finish all precipitated phases in the selected visual field information such as composition, size automatic collection and save as database file;
E. import the percent by weight or the concentration of chemical element at the condition setting frame of INCA FEATURE program, move the snotter sort program, obtain quantity and number percent, area and number percent, the average-size of precipitated phase and the detection by quantitative results such as precipitated phase quantity in the different size scope of dissimilar precipitated phases.
2. precipitated phase is pressed the quantitative detecting method of composition classification in the orientation silicon steel according to claim 1, it is characterized in that: the precipitated phase in the described extraction orientation silicon steel sample adopts the secondary carbon replica method.
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Cited By (6)
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| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN103411990A (en) * | 2013-08-23 | 2013-11-27 | 武汉钢铁(集团)公司 | Detection method for precipitated phases of nitride and oxide in steel-iron material |
| CN103674664A (en) * | 2013-10-21 | 2014-03-26 | 广东电网公司电力科学研究院 | Quantitative metallographic analysis method for phase M23C6 of Super 304H steel |
| CN105067649A (en) * | 2015-08-24 | 2015-11-18 | 首钢总公司 | Method for quantitative analysis on material organization through scanning electron microscope and energy disperse spectrometer |
| CN112415029A (en) * | 2020-11-23 | 2021-02-26 | 中国华能集团有限公司 | Method for directly testing volume fraction of precipitated phase in alloy |
| CN113203764A (en) * | 2021-05-07 | 2021-08-03 | 北京科技大学 | Material tissue quantitative analysis system using scanning electron microscope and energy spectrometer |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN103123329B (en) * | 2012-12-31 | 2015-07-29 | 上海大学 | The method for quick of non-metallic inclusion and device for fast detecting in metal |
| CN103411990A (en) * | 2013-08-23 | 2013-11-27 | 武汉钢铁(集团)公司 | Detection method for precipitated phases of nitride and oxide in steel-iron material |
| CN103674664A (en) * | 2013-10-21 | 2014-03-26 | 广东电网公司电力科学研究院 | Quantitative metallographic analysis method for phase M23C6 of Super 304H steel |
| CN105067649A (en) * | 2015-08-24 | 2015-11-18 | 首钢总公司 | Method for quantitative analysis on material organization through scanning electron microscope and energy disperse spectrometer |
| CN112415029A (en) * | 2020-11-23 | 2021-02-26 | 中国华能集团有限公司 | Method for directly testing volume fraction of precipitated phase in alloy |
| CN113203764A (en) * | 2021-05-07 | 2021-08-03 | 北京科技大学 | Material tissue quantitative analysis system using scanning electron microscope and energy spectrometer |
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