CN114371185A - Method for measuring surface defect depth of stainless steel plate - Google Patents
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- CN114371185A CN114371185A CN202210056233.8A CN202210056233A CN114371185A CN 114371185 A CN114371185 A CN 114371185A CN 202210056233 A CN202210056233 A CN 202210056233A CN 114371185 A CN114371185 A CN 114371185A
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- 230000007547 defect Effects 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000010935 stainless steel Substances 0.000 title claims abstract description 34
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 34
- 238000005259 measurement Methods 0.000 claims abstract description 16
- 238000005498 polishing Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 230000002950 deficient Effects 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000005520 cutting process Methods 0.000 claims abstract description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 58
- 238000001035 drying Methods 0.000 claims description 8
- 238000003384 imaging method Methods 0.000 claims description 8
- 230000001133 acceleration Effects 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005098 hot rolling Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 201000009310 astigmatism Diseases 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002436 steel type Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- G01N23/22—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 measuring secondary emission from the material
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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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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Abstract
The invention relates to the technical field of analysis and detection of stainless steel materials, in particular to a method for measuring the surface defect depth of a stainless steel plate. The method comprises the following steps: the method comprises the following steps: cutting a stainless steel plate with a defective surface into a sample; step two: cleaning the sample with absolute ethyl alcohol by using an ultrasonic cleaning machine; step three: horizontally placing the sample on a sample table of a scanning electron microscope; step four: observing all defects on the surface of the sample, and searching 5-10 defects with deeper defect depth as candidate points for depth measurement; step five: calculating the difference value of the working distances respectively corresponding to the clear bottom and upper edge images of the defect, wherein the difference value is the depth value of the candidate defect; step six: carrying out defect depth measurement on the candidate points one by one; step seven: and comparing the depth values of all candidate defects, wherein the maximum depth value is used as a reference value of the polishing depth of the surface defects of the steel plate. The method can realize rapid and accurate defect depth measurement, and the precision can reach micron level.
Description
Technical Field
The invention relates to the technical field of analysis and detection of stainless steel materials, in particular to a method for measuring the surface defect depth of a stainless steel plate.
Background
Stainless Steel (Stainless Steel) is a short name for acid-resistant Stainless Steel, and Steel types which are resistant to weak corrosive media such as air, steam and water or have Stainless properties are called Stainless Steel. In the production process of the stainless steel plate, the requirement on the surface quality of the stainless steel plate is high, and a smooth and defect-free surface is expected to be obtained, however, in the actual production process, no matter the surface is subjected to hot rolling pickling or cold rolling annealing pickling, some surface defects always exist, the appearance is not only influenced, and the subsequent processing, detection and use of the stainless steel plate are also influenced in the serious case. Some defects have certain depths, such as acid pickling corrosion pits caused by inclusions, pits left by falling of iron scales pressed in by hot rolling and the like, when the defects are distributed more and have deeper depths on the surface of the steel plate, the surface needs to be polished and polished, in order to improve polishing efficiency and guarantee polishing effect, the depth of the surface defects needs to be accurately measured, the surface polishing amount is determined according to the depth of the defects, and accurate polishing is achieved.
Because the surface defect depth of the stainless steel plate is in the micron order, the defect forms are different, and the defect depths are different, no proper measurement method standard is available all the time, the actual grinding operation is purely empirical, the phenomenon of insufficient grinding or excessive grinding exists, and the grinding quality and efficiency cannot be guaranteed.
The observation of the surface defects of the stainless steel plate is divided into macroscopic observation and microscopic observation, the macroscopic observation generally depends on direct observation of human eyes or observation by means of a magnifying glass, and the sheet production also has online detection equipment, but the methods generally only observe and judge whether the defects exist, the number of the defects and the distribution characteristics, and cannot give the depth value of the defects. The microscopic observation means comprises a stereoscopic microscope, an optical microscope and a scanning electron microscope, wherein the stereoscopic microscope has a magnification of several to dozens of times and is relatively macroscopic, and the scanning electron microscope becomes a main instrument for analyzing and testing the surface defects of the stainless steel plate by virtue of the characteristics of high resolution and large depth of field, and is mainly used for observing the appearance of the defects.
Disclosure of Invention
The invention aims to solve the problems and provides a method for measuring the surface defect depth of a stainless steel plate.
The purpose of the invention is realized as follows: a method for measuring the surface defect depth of a stainless steel plate comprises the following steps:
the method comprises the following steps: cutting a stainless steel plate with a defective surface into a sample;
step two: cleaning the surface of the sample with absolute ethyl alcohol for 2-5 minutes by using an ultrasonic cleaning machine, and naturally drying or drying by using a blower after taking out;
step three: horizontally placing the sample on a sample table of a scanning electron microscope, wherein the surface with defects faces upwards;
step four: after the sample chamber is vacuumized, adjusting the Z axis of the sample stage to a height position, so that the distance between the observation surface of the sample and the pole shoe of the objective lens is 8.5-12 mm, keeping the Z axis height of the sample stage unchanged, loading appropriate accelerating voltage according to a scanning electron microscope secondary electron imaging method, adjusting the current, brightness and contrast of a probe to obtain a clear image, horizontally moving the sample stage under a lower magnification, observing all defects on the surface of the sample, and searching 5-10 defects with deeper defect depth as candidate points for depth measurement;
step five: selecting one candidate point defect, amplifying the candidate point defect, firstly carrying out focusing adjustment on a secondary electronic image on the upper edge of the defect, repeatedly carrying out under-focusing and over-focusing operations to find an ideal clear image which is opposite to the positive focus, recording a working distance value at the moment, then carrying out focusing adjustment on the secondary electronic image on the bottom position of the defect, similarly adopting the repeatedly carrying out under-focusing and over-focusing operations to find a clear image which is the positive focus, also recording the working distance value at the moment, and calculating corresponding working distance difference values respectively when the images at the bottom and the upper edge of the defect are clear, wherein the difference value is the depth value of the candidate defect;
step six: performing defect depth measurement on the candidate points one by adopting the same method;
step seven: and comparing the depth values of all candidate defects, wherein the maximum depth value is used as a reference value of the polishing depth of the surface defects of the steel plate.
Further, the suitable accelerating voltage in the fourth step is 15KV or 20 KV.
Furthermore, the absolute ethyl alcohol in the second step is analytically pure absolute ethyl alcohol with the concentration of more than or equal to 99.7 percent.
Further, the size of the sample in the first step is not more than 50mmX50mm at most.
Furthermore, in the fourth step, the probe current is 100pA-1500pA, the brightness is 50-80%, and the contrast is 30-90%.
Further, the lower magnification in step four is less than 300 times.
The invention has the beneficial effects that: the traditional measuring method for the depth of the surface defect of the stainless steel plate mainly adopts the steps of polishing the section of a sample and observing and measuring the polished section under an optical microscope or a scanning electron microscope, and has the defects that a certain chamfer angle cannot be generated inevitably no matter the section is polished directly or after being inlaid, if the surface defect is shallow, the chamfer angle cannot be observed possibly, and even if the section can be observed, the chamfer angle also brings a large error. In addition, cross-sectional polishing does not guarantee an accurate cut to the deepest depth of the defect, and therefore the depth measured from the cross-section is not necessarily the true depth. If the number of surface defects is large, the section polishing needs to be cut and polished for many times to measure the depths of the defects, and the workload is large. The measuring method provided by the patent can realize rapid and accurate defect depth measurement, and the precision can reach the micron order.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a graph of the depth of a defect of the present invention, about 33 microns, with the upper edge of the defect.
Figure 2 is a graph of the bottom of a defect of the present invention having a depth of about 33 microns.
Fig. 3 is a graph of the upper edge of a defect of the present invention having a depth of about 22 microns.
Fig. 4 is a graph of the bottom of a defect of the present invention having a depth of about 22 microns.
Detailed Description
The invention mainly aims to find a simple, accurate and quick method for measuring the surface defect depth of a stainless steel plate and provide accurate grinding amount for surface grinding.
The technology is realized based on the gathering imaging observation technology of the secondary electron image of the scanning electron microscope.
Scanning Electron Microscope (SEM) is a large precision instrument for high resolution micro-topography analysis, an observation tool between transmission electron microscope and optical microscope. The method utilizes a focused narrow high-energy electron beam to scan a sample, excites various physical information through the interaction between the electron beam and a substance, and collects, amplifies and re-images the information to achieve the purpose of characterizing the microscopic morphology of the substance. The method has the characteristics of large depth of field, large visual field, high resolution, visual imaging, strong stereoscopic impression, wide amplification factor range and the like.
The scanning electron microscope has a plurality of imaging modes, wherein secondary electron images are most widely applied and are mainly used for observing the three-dimensional appearance of the surface of a sample. The surface defect appearance observation of the stainless steel plate is carried out by adopting a secondary electron imaging technology.
When the surface defect appearance of the stainless steel plate is observed by using a scanning electron microscope, a clear image is formed by using secondary electrons under certain accelerating voltage, probe current, magnification and working distance. A sharp image is an image that is well focused (in a state of being in focus), free of astigmatism (or with proper astigmatism correction), and with proper contrast and brightness adjustment.
This patent utilizes when surface defect bottom and top edge (sample surface) obtain the clear image of focus, because defect bottom and top edge have the difference in height, consequently these two positions obtain the focus of clear image different, and the Working Distance (WD) that shows is just different in scanning electron microscope, and the depth of this defect just can be measured out through the difference of the working distance when comparing the clear image of acquisition of defect bottom and top edge. The difference in working distance at which a sharp image is obtained for the bottom and upper edge of the defect, while maintaining the height of the sample, is the depth of the defect.
The specific implementation operation process is as follows:
a piece of a representative sample having a maximum of 50mmX50mm is cut out from a stainless steel plate having a defective surface.
And cleaning the surface of the sample by using an ultrasonic cleaner and analytically pure absolute ethyl alcohol for 2-5 minutes, and naturally drying or drying by using a blower after taking out.
The sample is placed flat on a sample stage of a scanning electron microscope (fixed if necessary) with the defective surface facing upwards.
After the sample chamber is vacuumized, adjusting the Z axis of the sample stage to a proper height position to enable the distance between the observation surface of the sample and the pole shoe of the objective lens to be 8.5mm-12mm, then keeping the Z axis height of the sample stage unchanged, loading proper accelerating voltage (commonly 15KV or 20 KV) according to a scanning electron microscope secondary electron imaging method, adjusting proper probe current (100 pA-1500 pA), brightness (50% -80%) and contrast (30% -90%), obtaining a clear image, then horizontally moving the sample stage under a lower magnification (less than 300 times), observing all defects on the surface of the sample, and searching 5-10 defects with deeper defect depth as candidate points for depth measurement.
Selecting one candidate point defect, amplifying, firstly carrying out focusing adjustment on a secondary electronic image on the upper edge of the defect, repeatedly carrying out under-focus and over-focus operations, finding an ideal clear image which is in relative focus, and recording the working distance value at the moment. And then, carrying out focusing adjustment on a secondary electronic image on the bottom position of the defect, similarly adopting repeated under-focus and over-focus operations to find a clear image of the positive focus, and recording the working distance value at the moment. And calculating working distance difference values respectively corresponding to the clear images of the bottom and the upper edge of the defect. The difference is the depth value of the candidate defect.
And performing defect depth measurement on the candidate points one by adopting the same method.
And comparing the depth values of all candidate defects, wherein the maximum depth value can be used as a reference value of the polishing depth of the surface defects of the steel plate.
Example one
Example (b): surface defect depth measurement of duplex stainless steel 1Cr21Ni5Ti hot-rolled annealed pickled plate.
A representative sample of 40mmX40mm was cut out from a duplex stainless steel sheet 1Cr21Ni5Ti having a defective surface.
And (3) cleaning the surface of the sample by using an ultrasonic cleaner and analytically pure absolute ethyl alcohol for 3 minutes, and naturally drying or drying by using a blower after taking out.
And (4) flatly placing the sample on a sample table of a scanning electron microscope, wherein the surface with the defects faces upwards.
After the sample chamber is vacuumized, adjusting the Z axis of the sample stage to a proper height position to enable the distance between the observation surface of the sample and the pole shoe of the objective lens to be 9.5mm, then keeping the Z axis height of the sample stage unchanged, loading an accelerating voltage of 20KV according to a scanning electron microscope secondary electron imaging method, adjusting the current of a probe to be 400pA, adjusting the brightness to be 80% and the contrast to be 50% to obtain a clear image, then horizontally moving the sample stage under 200 times to observe all defects on the surface of the sample, and searching 8 defects with deeper defect depth as candidate points for depth measurement.
Selecting one candidate point defect, amplifying, firstly carrying out focusing adjustment on a secondary electronic image on the upper edge of the defect, repeatedly carrying out under-focus and over-focus operations, finding an ideal clear image which is in relative focus, and recording the working distance value at the moment. And then, carrying out focusing adjustment on a secondary electronic image on the bottom position of the defect, similarly adopting repeated under-focus and over-focus operations to find a clear image of the positive focus, and recording the working distance value at the moment. And calculating working distance difference values respectively corresponding to the clear images of the bottom and the upper edge of the defect. The difference is the depth value of the candidate defect.
And performing defect depth measurement on the candidate points one by adopting the same method.
And comparing the depth values of all candidate defects, wherein the maximum depth value can be used as a reference value of the polishing depth of the surface defects of the steel plate.
In the production process of the duplex stainless steel 1Cr21Ni5Ti plate, after hot rolling, annealing and pickling, because the surface has more defects with certain depth, the ultrasonic bottom wave noise is larger in the ultrasonic flaw detection process of the steel plate, so that the ultrasonic flaw detection of the steel plate cannot be normally carried out, the surface needs to be polished, the maximum depth of the surface defects is measured by adopting the method, and accurate polishing amount is provided for surface polishing. In order to avoid the surface defects of the hot-rolled sheet from being inherited to the cold-rolled surface, it is also necessary to perform thinning treatment of the hot-rolled surface defects.
The following fig. 1 and 2, fig. 3 and fig. 4 show clear images of positive focuses at the upper edge and the bottom of a defect and corresponding working distance values of the positive focuses taken by the depth measurement process of two typical defects on the surface of a 1Cr21Ni5Ti hot rolled plate, wherein the working distance difference is 0.033053mm and 0.021654mm respectively, namely, the depths of the two defects are about 33 microns and 22 microns respectively. The top edge of the fig. 1 defect is clear, WD =9.343442mm, the bottom of the fig. 2 defect is clear, WD =9.376495 mm. The fig. 3 defect is clear at the upper edge, WD =9.328548mm, the fig. 4 defect is clear at the bottom, WD =9.350202 mm.
When the scanning electron microscope is used for observing the surface defects of the stainless steel plate, the focal lengths of the positive-focus clear images are different due to the fact that the heights of the surface of the sample and the bottoms of the defects are different, and the working distances of the corresponding electron microscopes are different. And calculating the difference value of the corresponding working distances when the surface of the sample and the bottom of the defect are in positive focus, namely the depth of the defect.
The patent provides a simple, convenient, fast and accurate method for measuring the depth of a defect on the surface of a stainless steel plate, and the theoretical basis is that when a scanning electron microscope is used for observing an image, the working distances of clear images obtained at different heights on the surface of a sample are different, and the difference values of the working distances respectively corresponding to the clear images at the bottom and the upper edge (surface) of the defect are calculated, so that the depth value of the defect can be obtained. The method is particularly suitable for depth measurement of various defects on the surface of a plate sample, and the measurement precision can reach the micron level.
The above description is only an embodiment of the present invention, but the structural features of the present invention are not limited thereto, and any changes or modifications within the scope of the present invention by those skilled in the art are covered by the present invention.
Claims (6)
1. A method for measuring the surface defect depth of a stainless steel plate is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: cutting a stainless steel plate with a defective surface into a sample;
step two: cleaning the surface of the sample with absolute ethyl alcohol for 2-5 minutes by using an ultrasonic cleaning machine, and naturally drying or drying by using a blower after taking out;
step three: horizontally placing the sample on a sample table of a scanning electron microscope, wherein the surface with defects faces upwards;
step four: after the sample chamber is vacuumized, adjusting the Z axis of the sample stage to a height position, so that the distance between the observation surface of the sample and the pole shoe of the objective lens is 8.5-12 mm, keeping the Z axis height of the sample stage unchanged, loading appropriate accelerating voltage according to a scanning electron microscope secondary electron imaging method, adjusting the current, brightness and contrast of a probe to obtain a clear image, horizontally moving the sample stage under a lower magnification, observing all defects on the surface of the sample, and searching 5-10 defects with deeper defect depth as candidate points for depth measurement;
step five: selecting one candidate point defect, amplifying the candidate point defect, firstly carrying out focusing adjustment on a secondary electronic image on the upper edge of the defect, repeatedly carrying out under-focusing and over-focusing operations to find an ideal clear image which is opposite to the positive focus, recording a working distance value at the moment, then carrying out focusing adjustment on the secondary electronic image on the bottom position of the defect, similarly adopting the repeatedly carrying out under-focusing and over-focusing operations to find a clear image which is the positive focus, also recording the working distance value at the moment, and calculating corresponding working distance difference values respectively when the images at the bottom and the upper edge of the defect are clear, wherein the difference value is the depth value of the candidate defect;
step six: performing defect depth measurement on the candidate points one by adopting the same method;
step seven: and comparing the depth values of all candidate defects, wherein the maximum depth value is used as a reference value of the polishing depth of the surface defects of the steel plate.
2. The method for measuring the surface defect depth of the stainless steel plate according to claim 1, wherein the method comprises the following steps: the acceleration voltage in step four is suitably 15KV or 20 KV.
3. The method for measuring the surface defect depth of the stainless steel plate according to claim 1, wherein the method comprises the following steps: the absolute ethyl alcohol in the second step is analytically pure absolute ethyl alcohol with the concentration of more than or equal to 99.7 percent.
4. The method for measuring the surface defect depth of the stainless steel plate according to claim 1, wherein the method comprises the following steps: the size of the sample in the first step is not more than 50mmX50mm at most.
5. The method for measuring the surface defect depth of the stainless steel plate according to claim 1, wherein the method comprises the following steps: in the fourth step, the probe current is 100pA-1500pA, the brightness is 50-80%, and the contrast is 30-90%.
6. The method for measuring the surface defect depth of the stainless steel plate according to claim 1, wherein the method comprises the following steps: the lower magnification in step four is less than 300 times.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030006372A1 (en) * | 2001-06-19 | 2003-01-09 | Seiko Instruments, Inc. | Automatic focusing system for scanning electron microscope equipped with laser defect detection function |
| JP2009111318A (en) * | 2007-11-01 | 2009-05-21 | Sii Nanotechnology Inc | Defect recognizing method, defect observing method, and charged particle beam system |
| CN101581571A (en) * | 2009-06-19 | 2009-11-18 | 武汉钢铁(集团)公司 | Method for measuring pit depth with scanning electronic microscope |
| CN107607570A (en) * | 2017-08-31 | 2018-01-19 | 武汉钢铁有限公司 | Galvanized plate surface defect in-situ study method |
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- 2022-01-18 CN CN202210056233.8A patent/CN114371185A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030006372A1 (en) * | 2001-06-19 | 2003-01-09 | Seiko Instruments, Inc. | Automatic focusing system for scanning electron microscope equipped with laser defect detection function |
| JP2009111318A (en) * | 2007-11-01 | 2009-05-21 | Sii Nanotechnology Inc | Defect recognizing method, defect observing method, and charged particle beam system |
| CN101581571A (en) * | 2009-06-19 | 2009-11-18 | 武汉钢铁(集团)公司 | Method for measuring pit depth with scanning electronic microscope |
| CN107607570A (en) * | 2017-08-31 | 2018-01-19 | 武汉钢铁有限公司 | Galvanized plate surface defect in-situ study method |
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