CN102221352A - Method for measuring depth of alloy steel decarbonized layer - Google Patents
Method for measuring depth of alloy steel decarbonized layer Download PDFInfo
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Abstract
The invention belongs to physico-chemical test technology, and relates to a method for measuring depth of an alloy steel decarbonized layer. In the invention, the method for measuring the depth of the alloy steel decarbonized layer is characterized in that an image signal output terminal of a scanning electron microscope is connected with an input terminal of an X-ray energy spectrometer, the scanning electron microscope is used for measurement and analysis; and the X-ray energy spectrometer is used for analysis and verification. The method comprises the following steps of firstly cutting a sample; carrying out surface treatment on the sample; cleaning the sample; subsequently placing the sample in the scanning electron microscope and vacuuming the scanning electron microscope; adjusting parameters of the scanning electron microscope and carrying out organization form analysis; subsequently collecting images to carrying out energy spectrum analysis at two sides of a measuring point at a half position of a transition area; verifying a carbon ingredient; and finally completing the measurement on the depth of the decarbonized layer. The method can carry out exact analysis on the depth of the alloy steel decarbonized layer, can be operated simply and conveniently, and can meet the requirement of practical scientific research production and failure analysis.
Description
Technical field
The invention belongs to the physical and chemical testing technology, relate to a kind of measuring method of alloy steel decarburized layer deepness.
Background technology
In the testing process of alloy steel decarburized layer deepness, mainly carry out GB/224 and ISO3887 standard, only stipulated the general assay method of decarburized layer in the standard, metallographic method, microhardness method, chemical method (chemical analysis and spectral analysis).Metallographic method is intuitively simple, but personal error is bigger; The microhardness method, the accuracy height, decarburized layer deepness control is too strict; Chemical method (chemical analysis and spectral analysis), feasible theoretically, but operability is poor, is difficult to detect, and the direct-reading spectrometer sensing range is big, can't accomplish that fixed point detects.
Summary of the invention
The objective of the invention is: propose the measuring method of a kind of accuracy of measurement height, easy to operate alloy steel decarburized layer deepness, to satisfy the needs of research and production and failure analysis.
Technical scheme of the present invention is: a kind of measuring method of alloy steel decarburized layer deepness, its image signal output end with scanning electron microscope is connected with the input end of X-ray energy spectrometer, utilize scanning electron microscope to carry out Measurement and analysis, carry out analysis verification with X-ray energy spectrometer again, concrete steps are as follows:
1.1, sample cutting: cut the vertical material surface of alloy steel material to be analyzed, the maximal side of sample is not more than 20mm, and the reserved materials initial surface;
1.2, surface treatment: metallographic sample preparation, polishing are carried out in the pre-detection surface, and carry out etching, clean then and remove surface dust;
1.3, lay sample and vacuumize: the sample after will cleaning, put into the sample chamber of scanning electron microscope and vacuumize;
1.4, adjust the scanning electron microscope parameter: after vacuumizing end, add high pressure, adjust the scanning electron microscope parameter, make scanning electron microscope image be in clear state;
1.5, carry out electronic microscope photos: watch window is adjusted to the sample edge, then enlargement factor is transferred to 200 to 500 times, make the clear demonstration of organizing after the edge etching, carry out electronic microscope photos again, distinguish decarburization district, edge, organize zone of transition and the non-decarburization of even tissue district;
1.6, measure decarburized layer: from the sample edge gradually vertically entad portion observe to microstructure no change position, measurement from the edge to the depth dimensions of microstructure zone of transition 1/2nd, select zones of different to measure some points, calculating mean value is decarburized layer deepness;
1.7, image acquisition: adjust the magnifier multiple, use X-ray energy spectrometer to gather the surface image at detected sample edge;
1.8, carry out energy spectrum analysis checking: respectively energy spectrum analysis is carried out in above-mentioned decarburized layer deepness everywhere both sides on the image of X-ray energy spectrometer collection, verify the above-mentioned result who records, chemical analysis fluctuates and 20% is considered as no change;
1.9 the depth value after the empirical tests is final decarburized layer deepness.
During surface treatment, the detection surface nital etching after the polishing.
After the etching, sample is put into anhydrous alcohol soak after 0.5～2 minute and take out, be placed in the clean glass disc air dry in air.
After vacuumizing end, add high pressure is 20KV, and the light beam of selection is φ 4.0, and enlargement factor is 100 times.
Enlargement factor during image acquisition is 100 times.
Advantage of the present invention is: alloy steel decarburized layer deepness measuring method of the present invention is by being used in combination scanning electron microscope and X-ray energy spectrometer, can accurately analyze decarburized layer deepness, and verify by energy spectrum analysis, its precision can satisfy the needs of research and production and failure analysis, and it is simple to operate, convenient, have bigger actual application value.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further details.
The image signal output end that the measuring method of alloy steel decarburized layer deepness of the present invention is adopted scanning electron microscope is connected with the input end of X-ray energy spectrometer, utilize scanning electron microscope to carry out analysis to measure, verify by X-ray energy spectrometer again, realization is to the accurate measurement of alloy steel decarburized layer deepness, and it is as follows that it measures the concrete analysis step:
1, sample cutting: cut the vertical material surface of alloy steel material to be analyzed, the maximal side of sample is not more than 20mm, and the reserved materials initial surface;
2, surface treatment: the sample of well cutting is inlayed or the anchor clamps clamping, metallographic sample preparation, polishing are carried out in the pre-detection surface, the detection surface nital etching after the polishing;
3, washed samples: sample is put into anhydrous alcohol soak after 0.5～2 minute and take out,, be placed in the clean glass disc air dry in air then to remove the specimen surface dust;
4, lay sample: the sample after will cleaning, put into the sample chamber of scanning electron microscope;
5, scanning electron microscope vacuumizes: select the high vacuum pattern, the equipment automatic vacuum;
6, adjust the scanning electron microscope parameter: after vacuumizing end, the 20KV that adds high pressure, selecting light beam is φ 4.0, enlargement factor is 100 times, adjusts focal length, brightness and contrast, makes scanning electron microscope image be in clear state;
7, carry out electronic microscope photos: watch window is adjusted to the sample edge, then enlargement factor is transferred to 200 to 500 times, reaching tissue after the edge etching can distinguish clear and be as the criterion to carry out electronic microscope photos, because the difference of sample carbon content, there is evident difference in surface texture, can clearly distinguish decarburization district, edge, organize zone of transition and the non-decarburization of even tissue district;
8, measure decarburized layer deepness: from the sample edge gradually vertically entad portion observe to microstructure no change position, the depth dimensions of measurement from the sample edge to microstructure zone of transition 1/2nd, similarly, select zones of different to measure some points, calculating mean value;
9, image acquisition: the Electronic Speculum enlargement factor is returned 100 times, use X-ray energy spectrometer to gather the surface texture image at detected sample edge;
10, energy spectrum analysis checking: on the image that X-ray energy spectrometer is gathered, respectively energy spectrum analysis is carried out in above-mentioned decarburized layer deepness everywhere (microstructure zone of transition 1/2nd places) both sides, the carbon content of analyzing both sides distributes, verify the above-mentioned result who records, wherein, carbon content fluctuation 20% is considered as no change;
Depth value after 11 empirical tests is final decarburized layer deepness.
Embodiment 1
To 15CDV6 φ 40 * 1, the steel pipe internal-surface decarburized layer deepness of R980 is measured
1, sample cutting: in the present embodiment, the vertical material surface of steel pipe of 15CDV6 φ 40 * 1 is cut into square sample, specimen size 10 * 10mm, the whole wall thickness of thickness, make that the test samples surface is vertical with the cross section, thereby be convenient to the scanning survey analysis, and the original inside surface of reserved materials;
2, preparation test piece: the sample of well cutting is inlayed, with sample edge saturating and guarantee the vertical pointing machine mould of the sample of inlaying, carry out metallographic sample preparation, polishing to detecting a side surface, the nital etching is used on the detection surface after the polishing, shows that more clearly microstructure is good.
3, washed samples: sample is put into the anhydrous alcohol immersion take out after 1 minute, remove the specimen surface dust, be placed in the clean glass disc air dry in air;
4, lay sample: the sample after will cleaning, put into the sample chamber of scanning electron microscope, detection faces upwards, in the present embodiment, the scanning electron microscope model that is adopted is FEI Inspect, can certainly be for satisfying other model scanning electron microscope that scanning accuracy requires;
5, scanning electron microscope vacuumizes: select the high vacuum pattern, the equipment automatic vacuum;
6, adjust the scanning electron microscope parameter: after vacuumizing end, the 20KV that adds high pressure, selecting light beam is φ 4.0, enlargement factor is 100 times, adjusts focal length, brightness and contrast, makes scanning electron microscope image be in clear state;
7, carry out electronic microscope photos: watch window is adjusted to the sample edge carries out the Electronic Speculum fabric analysis, enlargement factor is transferred to 300 times then, organize clear and legible knowledge after the edge etching;
8, measure decarburized layer deepness: from the vertically entad portion's observation gradually of the more ferrite in sample edge, ferrite reduces gradually, tempered sorbite increases gradually, until microstructure is the tempered sorbite position more than 90%, measurement from the edge to the depth dimensions of microstructure zone of transition 1/2nd, select diverse location to measure 3 points (situations when wherein the different marginal points of diverse location point expression are to its respective organization zone of transition 1/2nd places), measured value is respectively 0.17mm, 0.19mm 0.20mm, calculating mean value are 0.19mm, certainly, according to practical measurement requirement, the measuring position of selection is not limited to 3 points, and it measures number can increase or reduce;
9, image acquisition; The Electronic Speculum enlargement factor is returned 100 times, use X-ray energy spectrometer to gather the surface image at detected sample edge;
10, carry out the energy spectrum analysis checking; Respectively energy spectrum analysis is carried out in decarburized layer deepness both sides, above-mentioned 3 place on the image of X-ray energy spectrometer collection, chemical analysis fluctuates in 20%, and the above-mentioned result who records is accurate;
11, decarburized layer deepness is 0.19mm after the empirical tests.
Alloy steel decarburized layer deepness measuring method of the present invention in sum is by being used in combination scanning electron microscope and X-ray energy spectrometer, can accurately analyze decarburized layer deepness, and verify by energy spectrum analysis, its precision can satisfy the needs of research and production and failure analysis, and it is simple to operate, convenient, have bigger actual application value.
Claims (5)
1. the measuring method of an alloy steel decarburized layer deepness, it is characterized in that, the image signal output end of scanning electron microscope is connected with the input end of X-ray energy spectrometer, utilize scanning electron microscope to carry out Measurement and analysis, carry out analysis verification with X-ray energy spectrometer again, its concrete steps are as follows:
1.1, sample cutting: cut the vertical material surface of alloy steel material to be analyzed, the maximal side of sample is not more than 20mm, and the reserved materials initial surface;
1.2, surface treatment: metallographic sample preparation, polishing are carried out in the pre-detection surface, and carry out etching, clean then and remove surface dust;
1.3, lay sample and vacuumize: the sample after will cleaning, put into the sample chamber of scanning electron microscope and vacuumize;
1.4, adjust the scanning electron microscope parameter: after vacuumizing end, add high pressure, adjust the scanning electron microscope parameter, make scanning electron microscope image be in clear state;
1.5, carry out electronic microscope photos: watch window is adjusted to the sample edge, then enlargement factor is transferred to 200 to 500 times, make the clear demonstration of organizing after the edge etching, carry out electronic microscope photos again, distinguish decarburization district, edge, organize zone of transition and the non-decarburization of even tissue district;
1.6, measure decarburized layer: from the sample edge gradually vertically entad portion observe to microstructure no change position, measurement from the edge to the depth dimensions of microstructure zone of transition 1/2nd, select zones of different to measure some points, calculating mean value is decarburized layer deepness;
1.7, image acquisition: adjust the magnifier multiple, use X-ray energy spectrometer to gather the surface image at detected sample edge;
1.8, carry out energy spectrum analysis checking: respectively energy spectrum analysis is carried out in above-mentioned decarburized layer deepness everywhere both sides on the image of X-ray energy spectrometer collection, verify the above-mentioned result who records, chemical analysis fluctuates and 20% is considered as no change;
1.9 the depth value after the empirical tests is final decarburized layer deepness.
2. the measuring method of alloy steel decarburized layer deepness according to claim 1 is characterized in that: during surface treatment, and the detection surface nital etching after the polishing.
3. the measuring method of alloy steel decarburized layer deepness according to claim 2 is characterized in that: after the etching, sample is put into anhydrous alcohol soak after 0.5～2 minute and take out, be placed in the clean glass disc air dry in air.
4. the measuring method of alloy steel decarburized layer deepness according to claim 3 is characterized in that: after vacuumizing end, add high pressure is 20KV, and the light beam of selection is φ 4.0, and enlargement factor is 100 times.
5. the measuring method of alloy steel decarburized layer deepness according to claim 4 is characterized in that: the enlargement factor during image acquisition is 100 times.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104165971A (en) * | 2014-08-07 | 2014-11-26 | 国家电网公司 | Method for analyzing power linking metal fitting failure |
| CN105387824A (en) * | 2015-11-20 | 2016-03-09 | 武汉钢铁(集团)公司 | Quenched steel decarburized layer depth measuring method |
| CN106197330A (en) * | 2016-07-08 | 2016-12-07 | 首钢总公司 | A kind of assay method of steel decarburized layer deepness |
| CN107543820A (en) * | 2017-08-31 | 2018-01-05 | 洛阳鼎辉特钢制品股份有限公司 | A kind of detection method of hot rolling bearing steel wire rod decarburized layer deepness |
| CN108535304A (en) * | 2018-04-27 | 2018-09-14 | 暨南大学 | Macroscopical metallographic detection method of fatiguability break bolt |
| CN111024738A (en) * | 2019-12-12 | 2020-04-17 | 首钢集团有限公司 | Method for measuring depth of decarburization layer on surface of TRIP steel |
| CN111487272A (en) * | 2020-04-21 | 2020-08-04 | 中国航发沈阳发动机研究所 | Analysis method for surface product layer of turbine blade of aero-engine |
| CN112179261A (en) * | 2020-09-24 | 2021-01-05 | 桂林理工大学 | Method for detecting thickness of steel rail decarburized layer based on electromagnetic response |
| CN112648932A (en) * | 2020-12-04 | 2021-04-13 | 武汉锐科光纤激光技术股份有限公司 | Method for detecting stripe depth of laser cutting surface |
| 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 |
| CN115236110A (en) * | 2022-07-21 | 2022-10-25 | 江苏丰东热处理及表面改性工程技术研究有限公司 | Precision measurement method for micro-area carbon concentration distribution of gear carburization part |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104165971A (en) * | 2014-08-07 | 2014-11-26 | 国家电网公司 | Method for analyzing power linking metal fitting failure |
| CN105387824A (en) * | 2015-11-20 | 2016-03-09 | 武汉钢铁(集团)公司 | Quenched steel decarburized layer depth measuring method |
| CN105387824B (en) * | 2015-11-20 | 2018-07-10 | 武汉钢铁有限公司 | Hardened steel decarburized layer deepness measuring method |
| CN106197330B (en) * | 2016-07-08 | 2019-01-18 | 首钢集团有限公司 | A kind of measuring method of steel decarburized layer deepness |
| CN106197330A (en) * | 2016-07-08 | 2016-12-07 | 首钢总公司 | A kind of assay method of steel decarburized layer deepness |
| CN107543820A (en) * | 2017-08-31 | 2018-01-05 | 洛阳鼎辉特钢制品股份有限公司 | A kind of detection method of hot rolling bearing steel wire rod decarburized layer deepness |
| CN108535304A (en) * | 2018-04-27 | 2018-09-14 | 暨南大学 | Macroscopical metallographic detection method of fatiguability break bolt |
| CN108535304B (en) * | 2018-04-27 | 2020-06-30 | 暨南大学 | Macroscopic metallographic detection method for bolts easy to fatigue fracture |
| CN111024738A (en) * | 2019-12-12 | 2020-04-17 | 首钢集团有限公司 | Method for measuring depth of decarburization layer on surface of TRIP steel |
| CN111487272A (en) * | 2020-04-21 | 2020-08-04 | 中国航发沈阳发动机研究所 | Analysis method for surface product layer of turbine blade of aero-engine |
| CN112179261A (en) * | 2020-09-24 | 2021-01-05 | 桂林理工大学 | Method for detecting thickness of steel rail decarburized layer based on electromagnetic response |
| CN112179261B (en) * | 2020-09-24 | 2022-09-23 | 桂林理工大学 | Method for detecting thickness of steel rail decarburized layer based on electromagnetic response |
| CN112648932A (en) * | 2020-12-04 | 2021-04-13 | 武汉锐科光纤激光技术股份有限公司 | Method for detecting stripe depth of laser cutting surface |
| 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 |
| CN115236110A (en) * | 2022-07-21 | 2022-10-25 | 江苏丰东热处理及表面改性工程技术研究有限公司 | Precision measurement method for micro-area carbon concentration distribution of gear carburization part |
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Application publication date: 20111019 |