CN104634800A - Quantitative determination method for thickness of transition layer of titanium-steel composite plate - Google Patents
Quantitative determination method for thickness of transition layer of titanium-steel composite plate Download PDFInfo
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- CN104634800A CN104634800A CN201510058139.6A CN201510058139A CN104634800A CN 104634800 A CN104634800 A CN 104634800A CN 201510058139 A CN201510058139 A CN 201510058139A CN 104634800 A CN104634800 A CN 104634800A
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Abstract
The invention relates to the technical field of electronic speculum testing of a titanium-steel composite plate in a metallographic detection technology, and discloses a quantitative determination method for the thickness of a transition layer of a titanium-steel composite plate. The quantitative determination method comprises the following steps: by utilizing the characteristic of different components of two composite materials, performing component analysis on the middle part of the titanium-steel composite plate by a scanning electron microscope and an energy disperse spectroscopy, and then quantitatively determining the transition layer according to the relationship between the component concentration gradient and distance of the two materials with different components. According to the quantitative determination method, the thickness of the transition layer of the titanium-steel composite plate can be accurately determined, and compared with other technologies, the quantitative determination method is more intuitive, faster, more convenient, more efficient and more accurate, can be used for determining the thickness of the transition layer of a sample accurately and quantitatively, and can meet the continuous determination requirement.
Description
Technical field
The present invention relates to titanium steel composite board Electronic Speculum inspection technology field in metallographic detection technique, the method for especially a kind of titanium steel composite board transition region thickness quantitative measurement.
Background technology
Compound substance has excellent combination property, thus its research and production development very rapid.With regard to titanium steel composite board, this plate had both had the excellent decay resistance of titanium cladding, had again intensity and the plasticity of basic unit's carbon steel, found broad application in fields such as oil, chemical industry, ocean, the energy.The manufacture method of titanium steel composite board has Explosion composite method, diffusion composite algorithm, Explosion composite-rolling and roll-bonding method, wherein rolling can utilize the composite plate that large-sized rolling mills produces steady quality, with low cost, manufacturing schedule is short, large scale, thickness are controlled of producing slab, tool has a broad prospect of the use, but the slab compound working procedure of these two kinds of different materials is comparatively complicated, need constantly explore and improve its production technology in actual production.
The complex method of current rolling titanium steel composite board is mainly sandwich like way, half sandwich like way, empty sandwich like way, in its hollow sandwich or in midair interlayer complex method, the multiple material material of mother metal is different, the phenomenon such as plate benging, surface oxidation can be produced, affect composite quality, and in interlayer complex method, multiple material can not be separated from each other, suitable isolation can only be carried out, the selection of isolated material is comparatively large to composite plate quality influence, and transition bed parameter is an important parameter in composite plate. and its restricts and affects various physical property and the chemical composition of composite plate.So-called transition bed, namely refer to titanium layer and iron layer in titanium steel composite board in conjunction with excessive portion, it mixes titanium elements and ferro element.The transition region thickness of composite plate is controlled by Controlling Technology condition and molecular structure, it is an important topic of composite plate research, because the transition bed boundary of composite plate is indefinite, so the method for quantitative measurment transition bed measures except the change of phase except utilizing X-ray diffraction, additive method can not quantitative measurement.In sum, how the quality condition, process based prediction model etc. of transition region thickness to matrix in research titanium steel composite board and cladding, cladding and cladding interface fine structure and both sides calmodulin binding domain CaM of Measurement accuracy cladding have great significance.At present, the thickness of composite plate mainly measured by existing document, there are the mensuration such as conventional β ray backscattering principle, X-ray spectrometer, micro-metallographic method, hardness method according to different composite plate material and the optional conventional method of thickness, and small angle X ray scattering assay method is only had to the mensuration of transition bed.Small angle x-ray scattering (SAXS) assay method uses X diffractometer, and advantage measures area greatly, and determination data is mean value, and requires higher to the precision of equipment and the operant level of experimenter, and its pattern can not directly be observed in the position of mensuration.
Summary of the invention
Technical matters to be solved by this invention be to provide a kind of easy, accurately, titanium steel composite board transition region thickness method for quantitatively determining intuitively.
Titanium steel composite board transition region thickness method for quantitatively determining disclosed by the invention, comprises the following steps:
A, intercept and comprise the metallographic specimen at titanium steel composite board Interface of Rolling position;
B, polishing is carried out to sample composite plate Interface of Rolling;
C, sample is put into scanning electron microscope, select sample composite plate Interface of Rolling imaging also to amplify;
D, open energy spectrometer acquisition scans sem image, draw straight line perpendicular to composite plate Interface of Rolling to be measured, collect and the relation of composition on analytical line region and line length, two " Z " shapes obtaining the ferrotianium component distributing on straight line are schemed;
E, in " Z " shape figure, changing to from zero the length that peak projects at straight line by analyzing titanium and ferrous components, can transition region thickness be drawn.
Preferably, after step a, adopt organic solvent to clean specimen surface, then carry out step b.
Preferably, after step b, adopt clear water clean sample and dry up, then carry out step c.
Preferably, in stepb, first sample is carried out on abrasive paper for metallograph roughly grinding, fine grinding, then use polishing disk and antiscuffing paste polishing.
Preferably, described abrasive paper for metallograph granularity is 6.5 μm ~ 120 μm, described antiscuffing paste granularity≤2.5 μm.
Preferably, in step c, scanning electron microscope electron beam voltage is 15kV ~ 30kV, and bundle spot size is 20 μm ~ 40 μm.
Preferably, in step c, image magnification is 500 times ~ 5000 times.
Preferably, carrying out in c, Step d process, experimental situation temperature requirement is 20 DEG C ± 3 DEG C.
The invention has the beneficial effects as follows: the feature that the present invention utilizes two kinds of composite material compositions different, application surface sweeping Electronic Speculum+energy spectrometer carries out constituent analysis in the middle of titanium steel composite board, then according to the relational implementation of component concentration gradient and distance on the material of two heterogeneities to transition bed quantitative measurement.Energy Accurate Measurement titanium steel composite board transition region thickness of the present invention, compared with other technologies, less demanding to the operant level of experimenter, measurement site is microcell, it is more directly perceived, quick and easy, efficient, accurate, accurately quantitative measurement sample transition region thickness can be realized, and reach the requirement of METHOD FOR CONTINUOUS DETERMINATION, and selection area experimentally can be required to take a picture and measure.。
Accompanying drawing explanation
Fig. 1 is ferrotianium component distributing " Z " shape figure in the present invention.
Wherein, in figure, namely dotted line A is iron content change line, and namely solid line B is titanium elements content line, and namely heavy line C is compound interface line.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Titanium steel composite board transition region thickness method for quantitatively determining disclosed by the invention, comprises the following steps:
A, intercept and comprise the metallographic specimen at titanium steel composite board Interface of Rolling position;
B, polishing is carried out to sample composite plate Interface of Rolling;
C, sample is put into scanning electron microscope, select sample composite plate Interface of Rolling imaging also to amplify;
D, open energy spectrometer acquisition scans sem image, draw straight line perpendicular to composite plate Interface of Rolling to be measured, collect and the relation of composition on analytical line region and line length, two " Z " shapes obtaining the ferrotianium component distributing on straight line are schemed;
E, in " Z " shape figure, changing to from zero the length that peak projects at straight line by analyzing titanium and ferrous components, can transition region thickness be drawn.
In a step, Linear cut or machine work can be adopted to intercept sample, sample size remains on 10 ~ 20 × 10 ~ 20mm, the operations such as follow-up polishing are convenient to for removing specimen surface greasy dirt, as optimal way, after step a, organic solvent is adopted to clean specimen surface, carry out step b again, cleaning can adopt the organic solvent such as acetone or alcohol.
For ensureing the smooth of titanium steel composite board transition bed sample, after a step, carry out b step: polishing.Heat can be used to inlay, cold edge method inlays sample to be tested, or apply other mechanical implements clamping sample, polishing is carried out to it, and for concrete polishing process, as optimal way, in stepb, first sample is carried out on abrasive paper for metallograph roughly grinding, fine grinding, then use polishing disk and antiscuffing paste polishing.So, both can ensure polishing efficiency, can polishing effect be ensured again.And described abrasive paper for metallograph granularity is 6.5 μm ~ 120 μm, described antiscuffing paste granularity≤2.5 μm.After polishing completes, clear water can be adopted to clean sample and dry up, then carry out step c.
Step c is the process adopting scanning electron microscope sample composite plate Interface of Rolling to be measured to be carried out to imaging, ready sample to be tested is put on the stand of ready scanning electron microscope example room, then close sample chamber door and vacuumize, reach after requirement until vacuum tightness and open electron beam, select electron-beam voltage and bundle spot size, select image pattern (secondary electron figure or backscattered electron image), wherein electron-beam voltage is preferably 15kV ~ 30kV, and bundle spot size is preferably 20 μm ~ 40 μm.Then select the composite plate Interface of Rolling region that need measure, be amplified to certain multiple and image is adjusted clear till, because enlargement factor is larger, the one-tenth-value thickness 1/10 measured is more accurate, but the focal length of image is less, adjustment sharpness is more difficult, and therefore, image magnification is preferably 500 times ~ 5000 times.
After imaging specimens completes, can steps d be carried out, open energy spectrometer acquisition scans sem image, draw straight line perpendicular to composite plate Interface of Rolling to be measured, collect and the relation of composition and line length on analytical line region, two " Z " shapes obtaining the ferrotianium component distributing on straight line are schemed; Finally, carry out step e, in " Z " shape figure, change to the length of the projection of peak on straight line by analysis titanium and ferrous components from zero, can transition region thickness be drawn.As shown in Figure 1, in " Z " shape figure, the peak of the corresponding titanium composition of minimum point of ferrous components, the peak of the corresponding ferrous components of minimum point of titanium composition, so, be equal from zero length changing to the projection of peak on straight line in " Z " shape figure of titanium and ferrous components, this segment length is titanium steel composite board transition region thickness.As shown in Figure 1, be an example of " Z " shape figure of ferrotianium component distributing of the present invention, wherein namely X-coordinate is the above-mentioned straight line perpendicular to composite plate Interface of Rolling to be measured, and Y-coordinate is representation element cellulose content then, is then composite plate Interface of Rolling line perpendicular to the vertical curve of X-coordinate in figure.The X negative direction side being positioned at parting line is iron layer, and iron content is higher, and the X positive dirction side being positioned at parting line is titanium layer, and its titanium elements content is higher.As can be seen from the figure, titanium composition rises from being similar to zero when X-coordinate is 4 μm, and meanwhile, ferrous components declines from mxm., during to 8 μm, ferrous components is similar to zero, and titanium composition reaches mxm., so, from 4 μm to 8 μm, this scope is transition bed (namely figure two double dot dash lines), its width D is transition region thickness, and therefore, the titanium steel composite board transition region thickness shown in Fig. 1 is 4 μm.
In addition, for ensureing to measure accurately, as optimal way, carrying out in c, Step d process, experimental situation temperature requirement is 20 DEG C ± 3 DEG C.
Be two embodiments of the present invention below:
Embodiment 1
Intercept TA1 (2mm plate) and Q235 (3mm plate) titanium steel composite board Interface of Rolling position metallographic specimen (10 × 20mm), after inlaying with the happy hot mounting press of mark, cast for being roughly ground by 150 order sand paper (namely granularity is the sand paper of 106 μm) successively with the happy mill with brake of mark, 1500 order sand paper (namely granularity is 9 μm of sand paper) fine grinding, finally employing granularity is the antiscuffing paste polishing of 2 μm, ensure that composite plate Interface of Rolling is smooth, clear, nothing comes off and cut; The metallographic specimen ground is put into (laboratory ambient temperature is 20 DEG C) in JSM5600-LV scanning electron microscope, the composite plate Interface of Rolling region that need measure is found after utilizing secondary electron imaging, be amplified to 1200 times, adjustment image makes it clear, open energy spectrometer and gather district to be measured image, enter line analysis software program, press beginning key after vertical transition bed to be measured draws straight line and then constituent analysis is carried out to drawn area, obtain two " Z " shapes figure of the ferrotianium component distributing on straight line.Due to titanium composition from the peak titanium plate to transition bed on distance increase and progressively decline, Q235 steel plate is zero; Otherwise ferrous components is from progressively declining according to increasing with distance on titanium and ferrous components are from peak to transition bed Q235 steel plate, almost nil on titanium plate.Derive composition and air line distance figure, analyze titanium and ferrous components from zero to peak distance, then obtain the one-tenth-value thickness 1/10 of transition bed.According to circumstances can measure 1 or several transition region thickness value in zones of different, be then the last thickness of transition bed after average.Three times measurement result is 4 μm.
Embodiment 2
Intercept TA1 (2mm plate) and Q235 (10mm plate) titanium steel composite board Interface of Rolling position metallographic specimen (10 × 20mm), after inlaying with the happy hot mounting press of mark, cast for being roughly ground by 150# sand paper successively with the happy mill with brake of mark, the fine grinding of 1500# sand paper, finally employing granularity is the antiscuffing paste polishing of 2 μm, ensure that composite plate Interface of Rolling is smooth, clear, nothing comes off and cut; The metallographic specimen ground is put into (laboratory ambient temperature is 20 DEG C) in JSM5600-LV scanning electron microscope, the composite plate Interface of Rolling region that need measure is found after utilizing backscattered electron imagine, be amplified to 1000 times, adjustment image makes it clear, open energy spectrometer and gather district to be measured image, enter line analysis software program, press beginning key after vertical transition bed to be measured draws straight line and then constituent analysis is carried out to drawn area, obtain two " Z " shapes figure of the ferrotianium component distributing on straight line.Derive composition and air line distance figure, analyze titanium and ferrous components from zero to peak distance, then obtain the one-tenth-value thickness 1/10 of transition bed.According to circumstances can measure 1 or several transition region thickness value in zones of different, be then the last thickness of transition bed after average.Three times measurement result is 5 μm.
Claims (8)
1. titanium steel composite board transition region thickness method for quantitatively determining, is characterized in that, comprises the following steps:
A, intercept and comprise the metallographic specimen at titanium steel composite board Interface of Rolling position;
B, polishing is carried out to sample composite plate Interface of Rolling;
C, sample is put into scanning electron microscope, select sample composite plate Interface of Rolling imaging also to amplify;
D, open energy spectrometer acquisition scans sem image, draw straight line perpendicular to composite plate Interface of Rolling to be measured, collect and the relation of composition on analytical line region and line length, two " Z " shapes obtaining the ferrotianium component distributing on straight line are schemed;
E, in " Z " shape figure, changing to from zero the length that peak projects at straight line by analyzing titanium and ferrous components, can transition region thickness be drawn.
2. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1, is characterized in that: after step a, adopts organic solvent to clean specimen surface, then carries out step b.
3. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1 or 2, is characterized in that: after step b, adopts clear water clean sample and dry up, then carries out step c.
4. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1, is characterized in that: in stepb, is first carried out by sample roughly grinding on abrasive paper for metallograph, fine grinding, then uses polishing disk and antiscuffing paste polishing.
5. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 4, is characterized in that: described abrasive paper for metallograph granularity is 6.5 μm ~ 120 μm, described antiscuffing paste granularity≤2.5 μm.
6. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1, it is characterized in that: in step c, scanning electron microscope electron beam voltage is 15kV ~ 30kV, and bundle spot size is 20 μm ~ 40 μm.
7. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1, it is characterized in that: in step c, image magnification is 500 times ~ 5000 times.
8. titanium steel composite board transition region thickness method for quantitatively determining as claimed in claim 1, is characterized in that: carrying out in c, Step d process, experimental situation temperature requirement is 20 DEG C ± 3 DEG C.
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| CN106643592A (en) * | 2016-12-14 | 2017-05-10 | 西安交通大学 | Method and apparatus for measuring thickness of intermediate layer of three-layer composite plate |
| CN108535304A (en) * | 2018-04-27 | 2018-09-14 | 暨南大学 | Macroscopical metallographic detection method of fatiguability break bolt |
| CN109425315A (en) * | 2017-08-31 | 2019-03-05 | 长鑫存储技术有限公司 | The test loaded tool and test method of semiconductor structure |
| CN110132774A (en) * | 2019-06-12 | 2019-08-16 | 攀钢集团攀枝花钢铁研究院有限公司 | The test method of α pollution layer thickness |
| CN110687150A (en) * | 2019-10-28 | 2020-01-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for measuring thickness of magnesium-based composite powder coating layer |
| CN113916924A (en) * | 2021-10-11 | 2022-01-11 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
| CN114688981A (en) * | 2022-03-15 | 2022-07-01 | 中南大学 | Method, equipment and medium for identifying thickness of composite steel bar coating and evaluating thickness uniformity |
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| CN113916924A (en) * | 2021-10-11 | 2022-01-11 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
| CN113916924B (en) * | 2021-10-11 | 2023-02-17 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
| CN114688981A (en) * | 2022-03-15 | 2022-07-01 | 中南大学 | Method, equipment and medium for identifying thickness of composite steel bar coating and evaluating thickness uniformity |
| CN114688981B (en) * | 2022-03-15 | 2023-01-31 | 中南大学 | Method, equipment and medium for identifying thickness of composite steel bar coating and evaluating thickness uniformity |
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