CN103048345B - Test method for detecting inclusions in steel - Google Patents
Test method for detecting inclusions in steel Download PDFInfo
- Publication number
- CN103048345B CN103048345B CN201210553604.XA CN201210553604A CN103048345B CN 103048345 B CN103048345 B CN 103048345B CN 201210553604 A CN201210553604 A CN 201210553604A CN 103048345 B CN103048345 B CN 103048345B
- Authority
- CN
- China
- Prior art keywords
- sample
- scanning
- steel
- contrast
- pressure electronic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of inclusion detection and provides a test method for detecting inclusions in steel. The method comprises the following steps: after a test sample to be detected is ground by using a piece of abrasive paper, polishing the test sample to be detected; preparing a common alloy steel similar to the test sample to be detected in size and bonding an aluminum foil on the upper surface of the common alloy steel to finish the preparation of a contrast calibration sample; simultaneously putting the test sample to be detected and the contrast calibration sample into a sample chamber of a scanning electron microscope and vacuumizing the sample chamber; starting the scanning electron microscope, setting a scanning range of the test sample to be detected, scanning the surface of the test sample to be detected by using a high-voltage electron beam and stopping the scanning of the high-voltage electron beam to the test sample to be detected after the scanning lasts for a period of time; and scanning the surface of the contrast calibration sample by using a high-voltage electron beam and stopping the scanning of the high-voltage electron beam to the contrast calibration sample after the scanning lasts for a period of time. The test method for detecting the inclusions in the steel, provided by the invention, has the advantages that the inclusions in the steel can be detected more simply and accurately, the stability is good and the detection time is short.
Description
Technical field
The detection technique field of steel inclusion of the present invention, specifically a kind of test method for detecting steel inclusion.
Background technology
Except needing except the existence of non-metallic inclusion in specific steel, the existence of snotter in general iron and steel, should be avoided, improving the cleanliness factor of steel as far as possible.Nonmetallic inclusionsin steel all can have a negative impact to the load-bearing capacity of steel, plasticity, impact flexibility and corrosion stability etc., especially becomes formation of crack and causes product made from steel to produce fatigure failure.Therefore, in actual production, the content to nonmetallic inclusionsin steel, shape, size and distribution is needed strictly to be controlled.
The detection method of nonmetallic inclusionsin steel generally has following a few class: (1) metaloscope observation method: metaloscope observation method is a kind of traditional method, by observing shape, the optical signature of snotter or assisting with chemical method, snotter type can be measured, the size of direct observation snotter and distribution situation, this method relies on the direct visual perception of people, manual operation, and error is larger, the factor such as professional knowledge, experience simultaneously by operating personnel affects, and is easy to erroneous judgement; (2) electrolytic process: using steel sample as the anode of electrolytic cell, electrolytic tank is negative electrode, generally takes the steel sample of 2 ~ 3kg to its electrolysis, then eluriates and magnetic separation electrolytic slime, finally weighs classification, obtains the percentage composition of snotter different grain size distribution; The method degree of accuracy is high but time-consuming, and a general sample will spend 1-2 month, and generally can only analyze the situation of larger snotter, be difficult to tell, and the test period is very long to microinclusions.(3) in-situ analyzer method: the chemistry of analyzed object virgin state and structure are analyzed, by to without pre-burning, the spectral signal that the spark discharge that continuous sweep excites produces carries out data acquisition at a high speed and parsing, chemical constituents analysis under the virgin state of working sample surface diverse location, defect estimation and be mingled with state analysis, the amount of inclusions can be obtained, many-sided information such as distribution and granularity, though its speed is fast, but to the information error in the quantitative square faces such as the composition of snotter, situation only for larger defect is more applicable, the information such as the distribution characteristics of snotter cannot be shown, requirement for high cleanliness steel can not meet far away.
Application number is in " quantitative analyzing " patent of 200510013187.X, metaloscope, automatic carrier are connected with video camera, computing machine by it, from metaloscope, gather snotter image by video camera and send into the process of computing machine metallic phase image, realize the identification to snotter and parameter measurement, measurement result quantitative model is calculated or is analyzed with standard diagram, quantitative evaluation result.The method utilizes metallograph method to analyze, if specimen surface sample preparation defectiveness, easily causes erroneous judgement, and this patent can only to the analysis of sample holder foreign material, and size and geometric is measured, and cannot carry out instant analysis to the chemical composition of snotter.
Summary of the invention
Technical matters to be solved by this invention is, overcomes the shortcoming of prior art, proposes a kind of test method for detecting steel inclusion, and the detection of steel inclusion can be made more simple accurately, and good stability, detection time is short.
The technical scheme that the present invention solves above technical matters is:
For detecting a test method for steel inclusion, carry out according to the following steps:
(i) carry out polishing after being ground by sample sand paper to be checked, with surface without obvious cut for standard;
(ii) prepare a block size and the similar common alloy steel of sample to be checked, be attached on common alloy steel upper surface by one piece of aluminium foil, aluminium foil area is less than common alloy steel upper surface area, completes the preparation of contrast calibration sample;
(iii) sample to be checked and contrast sample are put into simultaneously the sample chamber of scanning electron microscope, sample to be checked and contrast sample are fitted side by side placement in sample chamber, and are vacuumized sample chamber;
(iv) start scanning electron microscope, set the sweep limit of sample to be checked, undertaken until complete whole sweep limit by following 1.-step cycle 2.:
1. utilize high-pressure electronic bundle to treat inspection specimen surface to scan, after scanning continues for some time, stop high-pressure electronic bundle to treat the scanning inspecting sample;
2. utilize high-pressure electronic bundle to scan contrast calibration sample surface, after scanning continues for some time, stop high-pressure electronic bundle to the scanning in contrast calibration sample face.
Like this, method of the present invention is when detecting for steel inclusion, both by the detection means supporting with scanning electron microscope and software, the size of steel inclusion in scanning process, form, distribution and composition were detected automatically, contrast difference can be obtained again, according to contrast difference, the physical function parameter of snotter and chemical composition are judged, accuracy is high, can not cause erroneous judgement to because of sample preparation problem.Present invention uses contrast calibration sample, when detecting for steel inclusion, because whole testing process is owing to applying contrast sample, it is made up of two kinds of different materials, itself there is a specific contrast scope, cover the contrast scope of steel inclusion, when scanning measuring samples, snotter within the scope of this contrast will be detected, and lower than or super going beyond the scope namely be not normal snotter in steel, its Stability and veracity of detection therefore for snotter is all fine.
The technical scheme that the present invention limits further is:
The aforesaid test method for detecting steel inclusion, step 1. in, utilize high-pressure electronic bundle to treat inspection specimen surface and scan, scanning continued after 0.5-20 hour, stopped high-pressure electronic bundle to treat the scanning inspecting sample.
The aforesaid test method for detecting steel inclusion, step 2. in, utilize high-pressure electronic bundle to scan contrast calibration sample surface, scanning continued after 0.5-2 minute, stopped high-pressure electronic bundle to the scanning in contrast calibration sample face.
Embodiment
embodiment 1
It is a kind of test method for detecting steel inclusion that the present embodiment provides, and carries out according to the following steps:
(i) carry out polishing after being ground by sample sand paper to be checked, with surface without obvious cut for standard;
(ii) prepare a block size and the similar common alloy steel of sample to be checked, be attached on common alloy steel upper surface by one piece of aluminium foil, aluminium foil area is less than common alloy steel upper surface area, completes the preparation of contrast calibration sample;
(iii) sample to be checked and contrast sample are put into simultaneously the sample chamber of scanning electron microscope, sample to be checked and contrast sample are fitted side by side placement in sample chamber, and are vacuumized sample chamber;
(iv) start scanning electron microscope, set the sweep limit of sample to be checked, undertaken until complete whole sweep limit by following 1.-step cycle 2.:
1. utilize high-pressure electronic bundle to treat inspection specimen surface to scan, scanning continued after 0.5-20 hour, stopped high-pressure electronic bundle to treat the scanning inspecting sample;
2. utilize high-pressure electronic bundle to scan contrast calibration sample surface, scanning continued after 0.5-2 minute, stopped high-pressure electronic bundle to the scanning in contrast calibration sample face.
The present embodiment is when the detection for steel inclusion, and the setting threshold value of snotter and minimum detection width, make the contrast of steel substrate and snotter in a suitable scope; Set the scope that whole sample needs Scanning Detction; Scanning area can be divided into several zonules and analyze by snotter trace routine automatically, and terminate the rear size to all snotteres, form, distribution and composition and carry out statistical study, partial results is as following table:
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1., for detecting a test method for steel inclusion, comprising:
(i) carry out polishing after being ground by sample sand paper to be checked, with surface without obvious cut for standard;
It is characterized in that: further comprising the steps of:
(ii) prepare a block size and the similar common alloy steel of sample to be checked, be attached on common alloy steel upper surface by one piece of aluminium foil, aluminium foil area is less than common alloy steel upper surface area, completes the preparation of contrast calibration sample;
(iii) sample to be checked and contrast sample are put into simultaneously the sample chamber of scanning electron microscope, sample to be checked and contrast sample are fitted side by side placement in sample chamber, and are vacuumized sample chamber;
(iv) start scanning electron microscope, set the sweep limit of sample to be checked, undertaken until complete whole sweep limit by following 1.-step cycle 2.:
1. utilize high-pressure electronic bundle to treat inspection specimen surface to scan, after scanning continues for some time, stop high-pressure electronic bundle to treat the scanning inspecting sample;
2. utilize high-pressure electronic bundle to scan contrast calibration sample surface, after scanning continues for some time, stop high-pressure electronic bundle to the scanning in contrast calibration sample face.
2. as claimed in claim 1 for detecting the test method of steel inclusion, it is characterized in that: described step 1. in, utilize high-pressure electronic bundle to treat inspection specimen surface to scan, scanning continued after 0.5-20 hour, stopped high-pressure electronic bundle to treat the scanning inspecting sample.
3. as claimed in claim 1 for detecting the test method of steel inclusion, it is characterized in that: described step 2. in, utilize high-pressure electronic bundle to scan contrast calibration sample surface, scanning continued after 0.5-2 minute, stopped high-pressure electronic bundle to the scanning in contrast calibration sample face.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210553604.XA CN103048345B (en) | 2012-12-19 | 2012-12-19 | Test method for detecting inclusions in steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210553604.XA CN103048345B (en) | 2012-12-19 | 2012-12-19 | Test method for detecting inclusions in steel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103048345A CN103048345A (en) | 2013-04-17 |
| CN103048345B true CN103048345B (en) | 2015-01-21 |
Family
ID=48061060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210553604.XA Active CN103048345B (en) | 2012-12-19 | 2012-12-19 | Test method for detecting inclusions in steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103048345B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107782653A (en) * | 2016-08-31 | 2018-03-09 | 中国科学院上海硅酸盐研究所 | The Statistical Measurement of Radial Void of the thermal barrier coating porosity and Size Distribution |
| CN108593649B (en) * | 2018-06-12 | 2020-04-24 | 钢铁研究总院 | Method for qualitatively and quantitatively testing and analyzing inclusions in steel |
| CN115774036B (en) * | 2023-02-15 | 2023-04-14 | 西南科技大学 | Method, system and device for detecting sand inclusion rate of blade surface |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB973322A (en) * | 1962-04-04 | 1964-10-21 | Huettenwerk Oberhausen Ag | Method of and equipment for the non-destructive testing of steel products |
| CN101105456A (en) * | 2007-08-13 | 2008-01-16 | 攀钢集团攀枝花钢铁研究院 | Analysis method for rapidly determining impurity content of alloy steel sample |
| WO2010049640A1 (en) * | 2008-10-27 | 2010-05-06 | Snecma | Counting inclusions on alloys by image analysis |
| CN102636507A (en) * | 2012-05-04 | 2012-08-15 | 东北电力科学研究院有限公司 | SEM-based method for qualitative and quantitative analysis of TiN inclusions in steel |
-
2012
- 2012-12-19 CN CN201210553604.XA patent/CN103048345B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB973322A (en) * | 1962-04-04 | 1964-10-21 | Huettenwerk Oberhausen Ag | Method of and equipment for the non-destructive testing of steel products |
| CN101105456A (en) * | 2007-08-13 | 2008-01-16 | 攀钢集团攀枝花钢铁研究院 | Analysis method for rapidly determining impurity content of alloy steel sample |
| WO2010049640A1 (en) * | 2008-10-27 | 2010-05-06 | Snecma | Counting inclusions on alloys by image analysis |
| CN102203591A (en) * | 2008-10-27 | 2011-09-28 | 斯奈克玛 | Counting inclusions on alloys by image analysis |
| CN102636507A (en) * | 2012-05-04 | 2012-08-15 | 东北电力科学研究院有限公司 | SEM-based method for qualitative and quantitative analysis of TiN inclusions in steel |
Non-Patent Citations (1)
| Title |
|---|
| 《钢中非金属夹杂物含量的测定标准评级图显微检验法》;何群雄等;《中华人民共和国国家标准》;20050513;1-7 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103048345A (en) | 2013-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103048345B (en) | Test method for detecting inclusions in steel | |
| CN103868780B (en) | The preparation method of the colour metallograpy sample of Al-Mg system and Al-Mg-Si-type aluminum alloy | |
| CN105021641A (en) | Method for rapidly measuring content of SO2 in cement clinker | |
| CN102023171B (en) | Nondestructive testing method for characterizing inclusion defect types in composite material quantitatively by using CT value | |
| CN105466998B (en) | A method of utilizing frequency conversion varying magnetic field exciting test Testing of Ferromagnetic Material Hardness characteristic | |
| CN112986298B (en) | In-situ statistical distribution characterization method for dendrite structure of single-crystal superalloy | |
| CN105572152B (en) | A kind of alternative assay method of composite material x-ray imaging sensitivity | |
| CN102954976A (en) | Quantitative detection method for center segregation of wire rod | |
| CN105509630B (en) | A kind of measurement apparatus and method of uneven electrical conductivity conductive material overburden cover | |
| CN103293226A (en) | Method for determining flaw detection benchmark sensitivity of steel plate by single crystal probe | |
| CN103604824A (en) | Method for quantitative detection on steel wire rod carbon segregation | |
| CN103399083A (en) | Method for restraining lift-off effect of impulse eddy current testing | |
| CN101644676B (en) | Aluminium bronze alloy composition rapid-measuring method | |
| CN104515810A (en) | Ultrasonic detection analysis method for defect type of laser cladding remanufactured component | |
| CN104297280A (en) | Method for quantitatively evaluating oil washing effect of rock core by using nuclear magnetic resonance (NMR) technology | |
| CN103969128A (en) | Method for detecting bending mechanical property of sample | |
| CN111189923A (en) | Variable frequency comparison quantitative detection method for defects of metallurgical plate | |
| CN106353340A (en) | Surface defect detection method for rod-like high-reflectance part | |
| CN103954691B (en) | Nondestructive testing method for material component fraction | |
| CN107389753A (en) | Cracks of metal surface detection method based on electrochemistry the cannot-harm-detection device | |
| CN110455840A (en) | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD | |
| CN102042809B (en) | Medicinal liquid for coating film thickness layer detection and detection method | |
| Haghi et al. | Measuring Instruments for Characterization of Intermediate Products in Electrode Manufacturing of Lithium‐Ion Batteries | |
| CN105158202A (en) | Quick and nondestructive sesame oil brand identification method | |
| CN103822928A (en) | Comparison atlas for performing fluorescent-penetrant inspection on defect size and manufacturing method for comparison atlas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |