CN105067649A - Method for quantitative analysis on material organization through scanning electron microscope and energy disperse spectrometer - Google Patents
Method for quantitative analysis on material organization through scanning electron microscope and energy disperse spectrometer Download PDFInfo
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- CN105067649A CN105067649A CN201510524776.8A CN201510524776A CN105067649A CN 105067649 A CN105067649 A CN 105067649A CN 201510524776 A CN201510524776 A CN 201510524776A CN 105067649 A CN105067649 A CN 105067649A
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Abstract
The invention discloses a method for quantitative analysis on material organization through a scanning electron microscope and an energy disperse spectrometer and belongs to the technical field of metal material detection. The method specifically includes the steps that a sample is prepared, wherein the surface of the sample is cleaned and polished; the sample is observed, wherein the prepared sample is put into an electron microscope sample room, and a clearly-focusing electronic image is obtained; data collecting and processing are conducted, wherein the area percentage of a tested phase in the field is displayed; thresholds are selected, wherein selection of the thresholds affects the measuring accuracy; data is output, wherein an experiment result is output in the mode of a color bitmap or a form report. The method has the advantages that the method is suitable for various metal materials, iron and steel products, minerals and fireproof materials and is fast in measuring operation and convenient to use.
Description
Technical field
The invention belongs to technical field of detection of metal, particularly a kind of scanning electron microscope and energy spectrometer of utilizing is to the method for material structure quantitative test.
Background technology
Material is generally made up of mutually one or more, and the ratio that wherein each composition is shared is mutually the basic problem that material circle is paid close attention to always.The method forming phase in microcosmic quantitatively analyzing material has a lot, conventional as quantitative metallographic analysis method, X ray back scattering diffraction analytic approach (EBSD), X-ray diffraction analysis method (XRD) etc.Analysis of metallographic method is conventional one relatively more directly perceived, principle does certain dimensional measurement to the microstructure of different contrast on two dimensional surface (sample surface polishing or analysis surface), then extrapolates the method for microstructure value in three dimensions.The equipment mainly relied on due to analysis of metallographic is optical metallographic microscope, and the resolution limit of optical microscope is about 200nm, usually it is just very poor that the optical metallographic microscope normally used is amplified to 2000 times of picture qualities, and the details of many tissues is still differentiated unclear under this enlargement factor, therefore in delicate tissues carry out quantitative test mutually time still Shortcomings.
EBSD quantitative phase analysis is the diffraction carrying out spatial resolution submicron order while the conventional feature retaining scanning electron microscope, EBSD resolution high (spatial resolution reaches 0.1 μm), become a kind of effective analysis means in investigation of materials, be widely used in the material such as industrial metal and alloy, pottery, semiconductor, superconductor, ore.But, EBSD analyze to sample to prepare relative requirement higher, equipment user also must possess quite high crystallographic theory knowledge, and poor to the material discrimination ability that phase place is close, therefore also comes with some shortcomings.
The material phase analysis of X-ray diffraction analysis method (XRD) is X-ray diffraction aspect with the most use in a metal, and quantitative test is the intensity according to diffraction pattern, determines the content of each phase in material.Shortcoming has higher requirements to analyst, and micro-zone analysis ability is poor, relative analysis of metallographic result, and the result of XRD is directly perceived not.
Generally speaking, above quantitative analysis method has respective applicability, but also has certain drawback, or lack of resolution, or sample preparation difficulty, or test process is complicated.
Summary of the invention
The object of the present invention is to provide a kind of scanning electron microscope and energy spectrometer of utilizing to the method for material structure quantitative test, solve the fast quantitative analysis problem of delicate tissues and component difference phase under high magnification.Utilize the contrast difference of each phase in scanning electron microscope tissue to carry out (comprising secondary electron image and backward scattering composition picture) method of quantitative test under the support of the areal calculation function of energy spectrometer, accurately, intuitively, fast, applicability is wide, workable.
Utilize scanning electron microscope and energy spectrometer to a method for material structure quantitative test, concrete steps and parameter as follows:
1, sample preparation: sample surfaces cleans, and grinding polishing, carrying out chemistry or electrochemical etching to needing the metal material of display organization; Mineral, fire resistive material, the material that phase constituent difference to be analyzed is large need not carry out etch;
2, sample observation: the sample prepared is put into electron microscopic sample room, vacuumizes, add filament current, centering disappearing image falls apart, and regulates brightness, contrast, keeps operating distance 10mm, obtains the electronic image of focus; Open X-ray energy spectrometer, after filament current emission current is stable, enter energy spectrum analysis program; Regulate the contrast difference of secondary electron image or backscattered electron image, capture electronic image with energy spectrometer; When tested phase quantitative measurment is carried out to backward scattering picture, directly can measure as composition contrast difference according to backward scattering;
When adjusting secondary electron image or backscattered electron image, it is clear when not losing details to organize, and adopts large contrast;
3, data acquisition and process: after image acquisition, use " area measurement data " key of the Oxford INCAIE250-450 analytic system in computer, color is chosen out mutually by tested, regulate contrast threshold value bar, make measuredly to be shown as colored Gao Guang mutually, now on the right side of dialog box, automatically show this tested area percentage shared in this visual field; Other phases select other colors in dialog box to measure;
4, the choosing of threshold value: the accuracy chosen measuring of threshold value has impact, left side when choosing, and the threshold value bar of right both sides is positioned flex point place, tested phase brightness parabolical left and right two; Keep the luminance threshold of this phase, mobile visual field, takes multiple measurements mutually to this;
5, data export: export experimental result for Color Bitmap or tabular report.
The invention has the advantages that: scanning electron microscope resolution is high, can on submicron order yardstick display organization details (metaloscope because of resolution low, the situation being difficult to when delicate tissues is analyzed realize can realize by scanning electron microscope), contrast is obvious, and measuring accuracy is high.Utilize the composition contrast of scanning electron microscope backward scattering picture poor, quantitative test can be carried out mutually directly to heterogeneity under the condition of non-etch.Applicability is wide, is applicable to various metal material, steel products, mineral and fire resistive material, measures swift to operate, convenient.
Embodiment
Embodiment 1
A kind of scanning electron microscope and energy spectrometer of utilizing is to the specific implementation method of the method for material structure quantitative test:
For the quantitative test of slag phase in titanium ore pelletizing.
(1) sample preparation
Sample is the titanium ore pelletizing that diameter is about 1cm, after being used bakelite powder heat to inlay, grinds polishing, prepares smooth sightingpiston.
(2) sample observation
The sample prepared is put into electron microscopic sample room, vacuumizes, add filament current, centering disappearing image falls apart, and operating distance is 10mm, obtains the electronic image of focus.This sample adopts backward scattering picture to become merotype to observe, under the backscatter mode of scanning electron microscope, in sample titanium phase with slag because the differential disply of atomic mass goes out the different contrast of light and shade, wherein titanium is mutually bright, slag presents Dark grey mutually, regulate the contrast of scanning electron microscope, strengthen the contrast difference of two kinds of phases further.
Open X-ray energy spectrometer, after filament current emission current is stable, enter energy spectrum analysis program.Electronic image is captured with energy spectrometer.
(3) data acquisition and process
After image acquisition, use " area measurement data " key of the Oxford INCAIE250-450 analytic system in computer, slag phase (Dark grey) is chosen out color, regulate brightness contrast threshold value bar (left side when threshold value is chosen for energy spectrometer, the threshold value bar of right both sides is positioned flex point place, slag phase brightness parabolical left and right two), make slag be all shown as colored Gao Guang mutually, now showing this tested area percentage shared in this visual field on the right side of dialog box is 24.3%.Choose other visual fields to take multiple measurements, measurement result is stablized.
(4) data export
Experimental result is quoted with the form of Color Bitmap or tabular report.
Claims (2)
1. utilize scanning electron microscope and energy spectrometer to a method for material structure quantitative test, it is characterized in that, a kind of scanning electron microscope and energy spectrometer of utilizing to the method for material structure quantitative test, concrete steps and parameter as follows:
1) sample preparation: sample surfaces cleans, and grinding polishing, carrying out chemistry or electrochemical etching to needing the metal material of display organization; Mineral, fire resistive material, the material that phase constituent difference to be analyzed is large need not carry out etch;
2) sample observation: the sample prepared is put into electron microscopic sample room, vacuumizes, add filament current, centering disappearing image falls apart, and regulates brightness, contrast, keeps operating distance 10mm, obtains the electronic image of focus; Open X-ray energy spectrometer, after filament current emission current is stable, enter energy spectrum analysis program; Regulate the contrast difference of secondary electron image or backscattered electron image, capture electronic image with energy spectrometer; When tested phase quantitative measurment is carried out to backward scattering picture, directly can measure as composition contrast difference according to backward scattering;
3) data acquisition and process: after image acquisition, use " area measurement data " key of the Oxford INCAIE250-450 analytic system in computer, color is chosen out mutually by tested, regulate contrast threshold value bar, make measuredly to be shown as colored Gao Guang mutually, now on the right side of dialog box, automatically show this tested area percentage shared in this visual field; Other phases select other colors in dialog box to measure;
4) the choosing of threshold value: the accuracy chosen measuring of threshold value has impact, left side when choosing, and the threshold value bar of right both sides is positioned flex point place, tested phase brightness parabolical left and right two; Keep the luminance threshold of this phase, mobile visual field, measures mutually to this;
5) data export: export experimental result for Color Bitmap or tabular report.
2. analytical approach according to claim 1, is characterized in that, when adjusting secondary electron image or backscattered electron image, it is clear when not losing details to organize, and adopts large contrast.
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| CN105424909A (en) * | 2015-11-26 | 2016-03-23 | 中国石油天然气股份有限公司 | Recognition method of supracrustal rock pore filler |
| WO2017092120A1 (en) * | 2015-11-30 | 2017-06-08 | 江苏大学 | Method for determining puncture position of probe during measurement of concentration of ions in leaf |
| CN107620593A (en) * | 2017-08-08 | 2018-01-23 | 中国科学院地质与地球物理研究所 | Scanning system and method are considered to be worth doing with rock drilling in a kind of oil gas field scene |
| CN108318515A (en) * | 2018-01-09 | 2018-07-24 | 南京大学 | A kind of individual particle mineral facies automatic identification and quantitative analysis method based on sem energy spectrum analysis |
| CN108645763A (en) * | 2018-05-15 | 2018-10-12 | 首钢集团有限公司 | A method of to martensite island quantitatively characterizing in dual phase steel |
| CN108918564A (en) * | 2018-08-09 | 2018-11-30 | 陕西延长石油(集团)有限责任公司研究院 | A kind of analysis method quantitative suitable for mud shale mineralogical composition |
| CN110186942A (en) * | 2018-02-23 | 2019-08-30 | 台湾电镜仪器股份有限公司 | Film assembly examines container and electron microscope |
| CN110646455A (en) * | 2019-07-25 | 2020-01-03 | 广东韶钢松山股份有限公司 | Method for rapidly analyzing oxide scale structure on surface of hot-rolled wire rod |
| CN111678932A (en) * | 2020-06-09 | 2020-09-18 | 首钢集团有限公司 | Analysis method of electron back scattering diffraction |
| CN111812138A (en) * | 2020-06-08 | 2020-10-23 | 河北省产品质量监督检验研究院 | Method for measuring asbestos content in brake pad by scanning electron microscope-energy spectrometer |
| CN113189104A (en) * | 2021-05-11 | 2021-07-30 | 福建工程学院 | Rapid observation method for phase conversion rate of aluminum alloy ingot casting homogenization treatment |
| 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 |
| CN113252418A (en) * | 2021-05-19 | 2021-08-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample |
| CN113933330A (en) * | 2021-09-23 | 2022-01-14 | 包头钢铁（集团）有限责任公司 | Method for representing distribution state of rare earth in pellet |
| CN117147601A (en) * | 2023-10-31 | 2023-12-01 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
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Cited By (21)
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| CN105424909A (en) * | 2015-11-26 | 2016-03-23 | 中国石油天然气股份有限公司 | Recognition method of supracrustal rock pore filler |
| CN105424909B (en) * | 2015-11-26 | 2018-06-01 | 中国石油天然气股份有限公司 | A kind of recognition methods of supracrustal rocks slit charges |
| WO2017092120A1 (en) * | 2015-11-30 | 2017-06-08 | 江苏大学 | Method for determining puncture position of probe during measurement of concentration of ions in leaf |
| CN107620593A (en) * | 2017-08-08 | 2018-01-23 | 中国科学院地质与地球物理研究所 | Scanning system and method are considered to be worth doing with rock drilling in a kind of oil gas field scene |
| US11041383B2 (en) | 2017-08-08 | 2021-06-22 | Institute Of Geology And Geophysics, Chinese Academy Of Sciences | System and method for scanning while-drilling rock fragments in an oil and gas field |
| CN108318515A (en) * | 2018-01-09 | 2018-07-24 | 南京大学 | A kind of individual particle mineral facies automatic identification and quantitative analysis method based on sem energy spectrum analysis |
| CN110186942A (en) * | 2018-02-23 | 2019-08-30 | 台湾电镜仪器股份有限公司 | Film assembly examines container and electron microscope |
| CN108645763A (en) * | 2018-05-15 | 2018-10-12 | 首钢集团有限公司 | A method of to martensite island quantitatively characterizing in dual phase steel |
| CN108918564A (en) * | 2018-08-09 | 2018-11-30 | 陕西延长石油(集团)有限责任公司研究院 | A kind of analysis method quantitative suitable for mud shale mineralogical composition |
| CN110646455A (en) * | 2019-07-25 | 2020-01-03 | 广东韶钢松山股份有限公司 | Method for rapidly analyzing oxide scale structure on surface of hot-rolled wire rod |
| CN111812138A (en) * | 2020-06-08 | 2020-10-23 | 河北省产品质量监督检验研究院 | Method for measuring asbestos content in brake pad by scanning electron microscope-energy spectrometer |
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| CN111678932A (en) * | 2020-06-09 | 2020-09-18 | 首钢集团有限公司 | Analysis method of electron back scattering diffraction |
| CN111678932B (en) * | 2020-06-09 | 2023-09-15 | 首钢集团有限公司 | Analysis method of electron back scattering diffraction |
| 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 |
| CN113189104A (en) * | 2021-05-11 | 2021-07-30 | 福建工程学院 | Rapid observation method for phase conversion rate of aluminum alloy ingot casting homogenization treatment |
| CN113252418A (en) * | 2021-05-19 | 2021-08-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample |
| CN113933330A (en) * | 2021-09-23 | 2022-01-14 | 包头钢铁（集团）有限责任公司 | Method for representing distribution state of rare earth in pellet |
| CN113933330B (en) * | 2021-09-23 | 2024-03-08 | 包头钢铁（集团）有限责任公司 | Method for representing distribution state of rare earth in pellet ore |
| CN117147601A (en) * | 2023-10-31 | 2023-12-01 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
| CN117147601B (en) * | 2023-10-31 | 2024-01-30 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
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Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Applicant after: Shougang Group Co. Ltd. Address before: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Applicant before: Capital Iron & Steel General Company |
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