CN105806867A - Analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy - Google Patents
Analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy Download PDFInfo
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Abstract
The invention discloses an analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy. The method includes: an energy dispersive spectrometer for determining main components of a grain boundary precipitate; by a spectrum area scanning function of an electronic probe, distinguishing grain boundary distribution and transgranular distribution of corresponding elements; extracting data of an element area profile; analyzing the data, calculating grain boundary and transgranular element concentration distribution coefficients and drawing a graph of relation to finally realize quantitative evaluation of alloy element segregation in high-temperature alloy. By the analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy, quantitative distinction of distribution of alloy elements at different grain boundary and transgranular positions of the high-temperature alloy can be realized without consumption of a great quantity of standard samples, and extensive application range and evaluation reasonability are realized.
Description
Technical field
The invention belongs to high-temperature alloy material component analysis technical field, relate to a kind of analysis method of segregation in quantitative assessment high temperature alloy.
Background technology
In order to improve alloy high-temp intensity, corrosion resisting property and structure stability, the research of high temperature alloy tends to the variation of alloying element kind and the increase of quantity.Different alloying elements, plays a different role, such as solution strengthening, second-phase strength and intercrystalline strengthening etc..The quantity of various phases, composition, size, distribution situation and alloying element have very big relation in the distribution condition of crystal boundary with the mechanical property of high temperature alloy and corrosion resisting property, so research alloying element Rule of Segregation in high temperature alloy, prediction segregation status, the process optimization produced for high temperature alloy has very big meaning.
In the traditional analysis of high temperature alloy element segregation, element segregation behavior mainly characterizes indirectly with precipitated phase, by scanning electron microscope, X-ray diffractometer, transmission electron microscope, energy disperse spectroscopy etc., the pattern of precipitated phase, thing phase, composition are analyzed, carry out Indirect evaluation element segregation behavior with this.
Miao Lede etc. go out precipitated phase mainly by chemical method electrolysis in " metallurgical analysis " the 35th volume the 1st phase disclosed " under different heat treatment state the qualitative and quantitative analysis of abros precipitated phase ", and obtain the quantitative result of its composition.But this method is only capable of obtaining the composition of precipitated phase, it is impossible to demonstrate each element distributing position in the sample.Precipitated phase has been studied mainly by transmission electron microscope and scanning electron microscope by Guo Yan etc. in " China Power " the 45th volume the 1st phase disclosed " the high-temperature aging precipitated phase of INCONEL617 alloy ", cannot draw each element segregation situation at diverse location equally.
Finding out from above-mentioned document patent, existing analysis segregation technique exists needs standard specimen, and constituent content is restricted, and result is not directly perceived；The defects such as the distribution in the sample of each element is indefinite.
Summary of the invention
For the deficiency that prior art exists, it is an object of the invention to provide a kind of analysis method of segregation in quantitative assessment high temperature alloy, by electron probe spectrometer, sample is carried out element surface analysis, take the average result of multiple surface analysis, calculate the mean concentration partition coefficient of crystal boundary and intracrystalline element, quantitative assessment Rule of Segregation.
For achieving the above object, present invention employs following technical scheme:
A kind of analysis method of segregation in quantitative assessment high temperature alloy, processing step includes:
1) sample through overheated inlaying, grinding and polishing, after corrosion, prepare the replica sample of to be analyzed, the precipitated phase obtained after replica carried out energy spectrum composition analysis, according to analyzing the element that need to select when result determines electron probing analysis；
2) sample after polishing is carried out the experiment of electron probe wave spectrum surface analysis, extract the compositional data of each element of crystal boundary and intracrystalline in experimental result respectively, calculate the concentration partition coefficient of crystal boundary and the element of intracrystalline, make the change curve of concentration partition coefficient, the Rule of Segregation of quantitative assessment alloying element.
Preferably, in described quantitative assessment high temperature alloy in the analysis method of segregation, electron probe wave spectrum surface analysis region is corresponding with replica region.
Preferably, in described quantitative assessment high temperature alloy in the analysis method of segregation, when carrying out the test of electron probe wave spectrum surface analysis, step footpath selects 0.05 μm.
Preferably, in described quantitative assessment high temperature alloy in the analysis method of segregation, the concentration partition coefficient of each element is the average result of multiple area surface analytical data.
Compared with the prior art, the present invention at least has the advantages that
1. the method is by the process to electron probe wave spectrum surface analysis data, draws concentration partition coefficient, can realize crystal boundary in high temperature alloy and distinguish with the quantitative of intracrystalline diverse location Elemental redistribution, it is not necessary to use substantial amounts of standard sample.
2. the concentration partition coefficient that the present invention proposes, can show Rule of Segregation by comparing, applied widely, evaluation method is reasonable.
Accompanying drawing explanation
Fig. 1 is the secondary electron image that in embodiment, sample surfaces observed by electron probe；
Fig. 2 is the wave spectrum Surface scan result figure of electron probe in embodiment；
Fig. 3 is the concentration partition coefficient graph of relation with heat treatment time of four kinds of essential elements in embodiment.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
1) 825 alloy samples are carried out heat to inlay, utilize polished machine to carry out 180#, 800# sand paper corase grind, 1200#, 1500# sand paper fine grinding, it is then passed through 5 μm, 1 μm diamond polishing agent, it is polished to without, after obvious cut, cleaning in dehydrated alcohol rapidly, and electricity consumption dries up；
2) by copper sulfate, hydrochloric acid, distilled water according to mCuSO4:VHCl:VH2OThe proportions corrosive liquid of=1:5:5, sample is soaked in the solution, burnishing surface is towards container side wall, observe sample surfaces state, take out sample after 2.5 minutes, clean in dehydrated alcohol rapidly, and electricity consumption dries up, and in the distribution of scanning electron microscopic observation precipitated phase, as it is shown in figure 1, white particle is precipitated phase；
3) utilize fine vacuum spray carbon instrument at sample surfaces sputtering carbon, demoulding in above-mentioned corrosive liquid, it is placed in distilled water and repeatedly cleans carbon film, finally carbon film is dried；
4) replica sample is placed in scanning electron microscope, utilizes the composition of energy spectrometer analysis precipitated phase, it is determined that the required alloying element analyzed of electron probe；
5) sample is processed by shot blasting with 5 μm, 1 μm diamond polishing agent again, until the evidence of corrosion on surface disappears.By electron probe, the sample after polishing again is carried out surface observation, specimen surface is carried out wave spectrum surface analysis, as in figure 2 it is shown, electron probe wave spectrum surface analysis region is corresponding with replica region；
6) during electron probe data acquisition, the parameter of setting is as follows: accelerating potential is 15kV, and electric current is 100nA, and analysis step footpath is 0.05 μm, extracts the compositional data multiple crystal grain of test of crystal boundary and the alloying element of intracrystalline, averages；
Analysis result treatment is as follows:
Extract the crystal boundary in multiple region and the data of intracrystalline respectively, take its meansigma methods, calculate the concentration partition coefficient K of crystal boundary and the element of intracrystalline, and make the graph of relation with heat treatment time, as shown in Figure 3:
K=crystal boundary average counter (element)/intracrystalline average counter (element)
Quantitative evaluating along with the change of heat treatment temperature is got final product according to curve chart, in 825 selected alloy samples, alloying element is at the Rule of Segregation of crystal boundary Yu intracrystalline: element Cr, Mo first move to intracrystalline to crystal boundary migration along with the increase of heat treatment temperature again, and element of Fe, Ni contrast, move to crystal boundary again along with the increase of heat treatment temperature first migrates to intracrystalline.
Embodiment described above only have expressed the specific embodiment of the present invention, but can not therefore understands that be the restriction to the scope of the claims of the present invention.Any variation that the present invention is done by those skilled in the art under the enlightenment of present inventive concept all falls within protection scope of the present invention.
Claims (4)
1. the analysis method of segregation in a quantitative assessment high temperature alloy, it is characterised in that processing step includes:
1) sample through overheated inlaying, grinding and polishing, after corrosion, prepare the replica sample of to be analyzed, the precipitated phase obtained after replica carried out energy spectrum composition analysis, according to analyzing the element that need to select when result determines electron probing analysis；
2) sample after polishing is carried out the experiment of electron probe wave spectrum surface analysis, extract the compositional data of each element of crystal boundary and intracrystalline in experimental result respectively, calculate the concentration partition coefficient of crystal boundary and the element of intracrystalline, make the change curve of concentration partition coefficient, the Rule of Segregation of quantitative assessment alloying element.
2. the analysis method of segregation in quantitative assessment high temperature alloy according to claim 1, it is characterised in that electron probe wave spectrum surface analysis region is corresponding with replica region.
3. the analysis method of segregation in the quantitative assessment high temperature alloy according to claim 1,3 or 4, it is characterised in that when carrying out the test of electron probe wave spectrum surface analysis, step footpath selects 0.05 μm.
4. the analysis method of segregation in quantitative assessment high temperature alloy according to claim 1, it is characterised in that the concentration partition coefficient of each element is the average result of multiple area surface analytical data.
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Cited By (6)
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| CN106596615A (en) * | 2016-12-25 | 2017-04-26 | 首钢总公司 | Quantitative analysis method for continuous casting billet dendritic segregation |
| CN110470687A (en) * | 2019-07-22 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Properties of Heavy Rail Steel microsegregation quickly positions evaluation method |
| CN111060544A (en) * | 2019-12-10 | 2020-04-24 | 中国科学院金属研究所 | Preparation method of electron probe sample of Ti-Al alloy powder and microsegregation detection method |
| CN113777115A (en) * | 2021-09-10 | 2021-12-10 | 西安热工研究院有限公司 | Quantitative statistical method for precipitated phase in alloy |
| CN114137010A (en) * | 2021-11-05 | 2022-03-04 | 上海交通大学 | Method for measuring distribution state of trace elements in high-temperature alloy |
| CN114252466A (en) * | 2021-12-16 | 2022-03-29 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method of solid solubility in alloy crystal and comparison method of alloying element content in alloy |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596615A (en) * | 2016-12-25 | 2017-04-26 | 首钢总公司 | Quantitative analysis method for continuous casting billet dendritic segregation |
| CN110470687A (en) * | 2019-07-22 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Properties of Heavy Rail Steel microsegregation quickly positions evaluation method |
| CN111060544A (en) * | 2019-12-10 | 2020-04-24 | 中国科学院金属研究所 | Preparation method of electron probe sample of Ti-Al alloy powder and microsegregation detection method |
| CN113777115A (en) * | 2021-09-10 | 2021-12-10 | 西安热工研究院有限公司 | Quantitative statistical method for precipitated phase in alloy |
| CN114137010A (en) * | 2021-11-05 | 2022-03-04 | 上海交通大学 | Method for measuring distribution state of trace elements in high-temperature alloy |
| CN114137010B (en) * | 2021-11-05 | 2024-02-13 | 上海交通大学 | Determination method for trace element distribution state of high-temperature alloy |
| CN114252466A (en) * | 2021-12-16 | 2022-03-29 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method of solid solubility in alloy crystal and comparison method of alloying element content in alloy |
| CN114252466B (en) * | 2021-12-16 | 2024-01-12 | 昆山晶微新材料研究院有限公司 | Quantitative analysis method and comparison method for intra-crystal solid solubility of alloy |
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