CN102095622A - Method for quick detection of grain orientation of oriented silicon steel - Google Patents
Method for quick detection of grain orientation of oriented silicon steel Download PDFInfo
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- CN102095622A CN102095622A CN 201110008621 CN201110008621A CN102095622A CN 102095622 A CN102095622 A CN 102095622A CN 201110008621 CN201110008621 CN 201110008621 CN 201110008621 A CN201110008621 A CN 201110008621A CN 102095622 A CN102095622 A CN 102095622A
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 title abstract description 4
- 229920000742 Cotton Polymers 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 23
- 238000001887 electron backscatter diffraction Methods 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 238000001493 electron microscopy Methods 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 claims description 3
- 230000003628 erosive effect Effects 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 abstract 2
- 235000019580 granularity Nutrition 0.000 abstract 1
- 239000008213 purified water Substances 0.000 abstract 1
- 235000019587 texture Nutrition 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 238000001953 recrystallisation Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000005162 X-ray Laue diffraction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
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Abstract
The invention discloses a method for quick detection of grain orientation of oriented silicon steel, and belongs to the technical field of detection of oriented electrical steel. The method comprises the following steps that: an oriented silicon steel sample which is annealed at a high temperature is polished by waterproof abrasive paper with different granularities according to the standard that thick scratches do not exist, and the sample is corroded in nitric acid alcohol, quickly washed by purified water, wiped by absorbent cotton and blown by a blower. A sample texture diagram is obtained by scanning through a scanner, and the sample is numbered by a pencil. The sample is placed into a scanning electron microscope, the orientation of each grain is quickly detected through scattered points of Flamenco software of electron back scattered diffraction (EBSD), and the orientation of each grain, the ideal Gaussian orientation difference and the polar diagram of each grain are obtained by processing through project manager data software of HKL Channel 5. The method has the advantages that: the method is easy and convenient to operate, the experiment efficiency is high, and the cost is saved.
Description
Technical field
The invention belongs to oriented electrical steel detection technique field, particularly provide a kind of fast detecting orientation silicon steel grain-oriented method.Detect the orientation of the little crystal grain of not growing up fully and depart from desirable Gauss's misorientation, it is the experimental technique that a kind of lower cost, high-level efficiency detect orientation silicon steel secondary recrystallization sample grain orientation and misorientation, by orientation and the misorientation that detects a large amount of crystal grain, the relation of research silicon steel texture and magnetic property, to formulate reasonable process, improve inhibitor, eliminate little crystal grain, improve the magnetic property of product.
Background technology
Orientation silicon steel utilize secondary recrystallization develop strong 110}＜100〉Goss texture, thereby obtain along roll to fine magnetic property.In the production run of orientation silicon steel, factors such as crystallite dimension and texture all have material impact to the finished product magnetic property, are effectively controlled magnetic property thereby need research and analyse.The crystal orientation micro-imaging technique of EBSD interrelates microstructure, micro-area composition and crystallography data analysis, can to the crystal boundary feature of orientation silicon steel, microcell orientation, position to poor, microtextured etc. carry out quantitatively, sxemiquantitative research, so the EBSD technology becomes the important means that orientation silicon steel is studied.
In addition, the typical technology that can obtain crystalline material microcell inner structure orientation also has SEAD (SAD) technology under etch method, Laue method, the transmission electron microscope (TEM) etc., compare the EBSD analytical technology with other technologies, operate easier, the analysis efficiency height, it is more accurate to measure absolute orientation, and lower than other technologies cost.
But for the sample behind the high annealing has taken place (the especially bigger sample of crystal grain), traditional E BSD way more complicated by orientation silicon steel, need pass through electropolishing (8～10% the perchloric acid alcoholic solution of mechanical polishing, polishing and 30～60s successively, decomposition voltage is controlled at 30～40V, electric current is 0.6～1A), also will slightly corrode at the nitric acid alcohol with 3～4% at last.Because the step complexity, the success ratio of sample is restricted on the one hand, on the other hand owing to need electropolishing, the size of the sample of producing is restricted and (is generally 12 * 10mm's, sample is too big, and surface quality is poor, causes Kikuchi lines bad, the demarcation rate is low, influenced imaging effect), and EBSD experimental expenses height, per hour be generally 300～500 yuan at present, above-mentioned reason causes the sample preparation efficiency ratio lower, and cost is higher.And the crystallite dimension of orientation silicon steel secondary recrystallization is bigger, if do great deal of experiment data, it is a lot of that the sample that need produce is wanted, and so just increased cost, wasted a large amount of time.In order to give full play to the advantage that the EBSD orientation is analyzed, the present invention changes the method for orientation silicon steel grain orientation analysis.
Summary of the invention
The object of the invention is to provide a kind of fast detecting orientation silicon steel grain-oriented method.Detect the orientation of the little crystal grain of not growing up fully and depart from desirable Gauss's misorientation, it is the experimental technique that a kind of lower cost, high-level efficiency detect orientation silicon steel secondary recrystallization sample grain orientation and misorientation, by orientation and the misorientation that detects a large amount of crystal grain, the relation of research silicon steel texture and magnetic property, to formulate reasonable process, improve inhibitor, eliminate little crystal grain, improve the magnetic property of product.Realized detecting more simply grain orientation, helped saving experimental period, reduced cost.
The common orientation silicon steel of sample of the present invention for producing through the low temperature slab heating of high annealing after the polishing of sample process, corrodes naked eyes and can see the crystal grain of growing up.
The present invention carries out Scatter plot with EBSD equipment successively to each crystal grain, and the gained data are handled on specific EBSD data processing software, draw each crystal grain orientation, with the misorientation and the utmost point figure of desirable goss texture.
The composition of common orientated electrical steel plate of the present invention is: C:0.04-0.06wt%, Si:2.5-6.5wt%, Mn:0.01-0.2wt%, Al:0.001-0.04wt%, N:0.005-0.015wt%, S≤0.04wt%, surplus is iron and unavoidable impurities.The operation steps that detects is as follows:
(1) use sand paper that the high annealing sample of 70mm * 10mm is polished;
(2) sample is corroded in the nitric acid alcohol of 2%-10% volume fraction, erosion time is 3-8 minute, corrodes tangible crystal grain to occur;
(3) sample is cleaned up with pure water, dry, dry up, guarantee the clean of surface with hair-dryer with absorbent cotton;
(4) sample is put into Electron Microscopy Room, with the Flamenco software break-up point of EBSD;
(5) use software processes draw grain orientation, with desirable Gauss's the misorientation and the utmost point figure of each crystal grain.
The used sand paper of polishing is respectively the silicon carbide paper of 240#, 400#, 600#, 800#, 1000#, 1200#, 1500#., 2000#, and standard is not for there being tangible cut.
Use the step of purified rinse water to require fast, and dry, then dry up with absorbent cotton.
Before putting into Electron Microscopy Room, need to use pencil that sample number into spectrum is carried out label.
The described use handled the Project manager data software of grain-oriented software as HKL Channel5.
Advantage of the present invention exists: simple to operate, the conventional efficient height is saved cost.
Description of drawings
Fig. 1 is the macrostructure of the high annealing plate that takes with scanner, among the figure each crystal grain has been done mark, the R representative roll to.
Numbered the utmost point figure of crystal grain sample in Fig. 2 representative graph 1, the orientation that representative is represented with a form is divided into { 200}, { 111} and { 110} utmost point figure.
Numbered the utmost point figure of crystal grain sample in Fig. 3 representative graph 1, the orientation that representative is represented with the level line form.
Embodiment
Sample behind the high annealing is slitting, be cut into the rectangular of 70mm * 10mm, with sample in 240#, 400#, 600#, 800#, 1000#, 1200#, 1500# and 2000# sand papering, standard is not have thick cut, then sample is corroded in the nitric acid alcohol of 2%-10% volume fraction, corrodes tangible crystal grain to occur, time is about 3-8 minute, fast use purified rinse water, and dry, dry up with hair-dryer then with absorbent cotton.Obtain sample tissue figure with scanner scanning, and with pencil with sample number into spectrum, organization chart is printed, also do corresponding mark (see figure 1), purpose is the accuracy that guarantees the Scatter plot of back.The sample of the 1-2 that mark is good 70 * 10mm is placed on the EBSD sample stage, uses the orientation of each crystal grain of Flamenco software break-up point fast measuring of EBSD.Then with the Project manager data software processes of HKLChannel5 draw each grain orientation, with desirable Gauss's misorientation, table 1 for the orientation of each crystal grain of Fig. 1 of handling and depart from the misorientation of Gauss's orientation the result (by and the ascending series arrangement of the misorientation of Goss), orientation with each crystal grain merges among three utmost point figure, shown in Fig. 2 and 3 at last.
The single grain orientation of table 1 sample reaches the misorientation with desirable Goss
Claims (4)
1. grain-oriented method of fast detecting orientation silicon steel is characterized in that operation steps is as follows:
(1) use sand paper that the high annealing sample of 70mm * 10mm is polished;
(2) sample is corroded in the nitric acid alcohol of 2%-10% volume fraction, erosion time is 3-8 minute, corrode tangible crystal grain to occur,
(3) sample is cleaned up with pure water, dry, dry up, guarantee the clean of surface with hair-dryer with absorbent cotton;
(4) sample is put into Electron Microscopy Room, with the Flamenco software break-up point of EBSD;
(5) use software processes draw grain orientation, with desirable Gauss's the misorientation and the utmost point figure of each crystal grain.
2. method according to claim 1 is characterized in that, the used sand paper of polishing is respectively the silicon carbide paper of 240#, 400#, 600#, 800#, 1000#, 1200#, 1500#, 2000#, and standard is not for there being tangible cut.
3. method according to claim 1 is characterized in that, before putting into Electron Microscopy Room, needs to use pencil that sample number into spectrum is carried out label.
4. method according to claim 1 is characterized in that, the described use handled the Project manager data software of grain-oriented software as HKL Channel5.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102519777A (en) * | 2011-12-15 | 2012-06-27 | 北京工业大学 | Method for preparing section sample used for analyzing evolution process of cubic texture |
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
| CN103278517A (en) * | 2013-05-29 | 2013-09-04 | 钢铁研究总院 | Method for measuring orientation differences of orientation silicon steel crystal particles |
| CN103323472A (en) * | 2012-03-20 | 2013-09-25 | 通用汽车环球科技运作有限责任公司 | Method for determining recovery state of metal alloy |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN109254022A (en) * | 2018-10-24 | 2019-01-22 | 首钢智新迁安电磁材料有限公司 | A method of measurement crystallite dimension |
| CN111220633A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院金属研究所 | Method for extracting specific crystal face in crystal by EBSD technology |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101210947A (en) * | 2006-12-27 | 2008-07-02 | 鞍钢股份有限公司 | A method for measuring the electromagnetic properties of electrical steel sheets |
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2011
- 2011-01-16 CN CN 201110008621 patent/CN102095622A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101210947A (en) * | 2006-12-27 | 2008-07-02 | 鞍钢股份有限公司 | A method for measuring the electromagnetic properties of electrical steel sheets |
Non-Patent Citations (1)
| Title |
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| 《电子显微学报》 20100228 付勇军 等 取向硅钢高温退火样品晶粒尺寸、取向及磁性能关系的研究 第704-706页 1-4 第29卷, 第1期 2 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102519777A (en) * | 2011-12-15 | 2012-06-27 | 北京工业大学 | Method for preparing section sample used for analyzing evolution process of cubic texture |
| CN103323472A (en) * | 2012-03-20 | 2013-09-25 | 通用汽车环球科技运作有限责任公司 | Method for determining recovery state of metal alloy |
| CN103323472B (en) * | 2012-03-20 | 2016-05-18 | 通用汽车环球科技运作有限责任公司 | Be used for the method for the recoil state of determining metal alloy |
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
| CN103278517A (en) * | 2013-05-29 | 2013-09-04 | 钢铁研究总院 | Method for measuring orientation differences of orientation silicon steel crystal particles |
| CN103278517B (en) * | 2013-05-29 | 2016-03-02 | 钢铁研究总院 | A kind of method measuring orientation silicon steel grain orientation difference |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN105136629B (en) * | 2015-08-24 | 2017-11-17 | 首钢总公司 | A kind of display methods of zinc-plated plate surface zinc crystal grain |
| CN109254022A (en) * | 2018-10-24 | 2019-01-22 | 首钢智新迁安电磁材料有限公司 | A method of measurement crystallite dimension |
| CN111220633A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院金属研究所 | Method for extracting specific crystal face in crystal by EBSD technology |
| CN111220633B (en) * | 2018-11-26 | 2022-09-16 | 中国科学院金属研究所 | Method for extracting specific crystal planes in crystals by EBSD technique |
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Application publication date: 20110615 |