CN103454296A - Method for improving quality of energy spectrum face distribution image of inorganic non-metal material sample - Google Patents
Method for improving quality of energy spectrum face distribution image of inorganic non-metal material sample Download PDFInfo
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Abstract
The invention relates to a method for improving the quality of an energy spectrum face distribution image of an inorganic non-metal material sample. The method comprises the following steps: (1) mounting a sample; (2) sticking a conductive adhesive; (3) electrically freezing the energy spectrum face distribution image of a collection element of an X-ray energy spectrum detector by using silicon drifting. According to an image acquisition method, the gray difference of a chemical constitution close phase in an element energy spectrum image can be increased, phenomena such as grain inner pixel lacking, grain edge blurring and image whole drifting are remitted, and the image acquisition time is shortened. The method is good for reducing the sample preparing difficulty and shortening time needed by an electric mirror observation condition optimizing test; during a shooting process, liquid nitrogen is not needed for cooling.
Description
Technical field
The present invention relates to the material analysis field, relate in particular to a kind of method that improves Inorganic Non-metallic Materials sample power spectrum mapping image quality.
Background technology
In the phase composition and the research that distributes of Inorganic Non-metallic Materials, the method that adopts backscattered electron image to look like to combine with element power spectrum mapping is a kind of very effective microcosmic means of testing.If be aided with again Digital Image Processing, can also obtain area fraction, girth mark and the related function of various phases.Especially form complicated and material pockety for phases such as cement, accurately grasp above-mentioned information, particularly important to the course of reaction of Knowing material.If employing the method, determine that the key factor of analysis result is the quality of power spectrum image.
Because the Inorganic Non-metallic Materials majority is non-conductive, this type of sample will be inlayed with epoxy resin, after it solidifies, through polishing, polishing, obtain smooth, smooth inspection surface, and then the spraying plating conductive layer, by the lithium silicon X-ray energy spectrum detector that drifts about, gather the power spectrum mapping picture of element.While adopting above-mentioned traditional image-pickup method, the quality of power spectrum image depends on two factors, the one, and the preparation effect of sample, the 2nd, the parameter setting of scanning electron microscope.
In order to improve the preparation effect of sample, the measure of usually taking is mainly repeatedly the series of parameters such as fineness of pressure, rotating speed, running time and grinding and polishing medium of blending ratio, solidification temperature, the polished machine of adjustment ring epoxy resins and sample.But, because the materials such as cement are heterogeneous, heterogeneous often, a granule interior may comprise the phase that several hardness does not wait simultaneously, therefore, the inspection surface of this type of sample is ground to smooth smooth difficulty very large, and also very consuming time.
In the electron microscopy observation link, all multiparameters such as accelerating potential, electron beam scanning pattern, image acquisition time, image enlargement factor all can affect image quality, and simultaneously, the effect of each factor to imaging, the image such as only have all to gather after complete and just manifested.At present, at least need 2.5h with traditional eds detector at the element power spectrum mapping of 500 times or the 1000 times a certain kens of lower collected specimens.Sample the phenomenons such as electric discharge, image drift, grain edges virtualization very easily occur after standing the long-time bombardment of electron beam.Therefore, if will improve by optimizing the Electronic Speculum condition of work quality of power spectrum image, not only consuming time, difficulty is large, and testing expense costliness.In addition, the highest C of content in cement
3s and C
2in two kinds of phases of S, cement mixture (as flyash), the various phase chemical compositions that are rich in Al and Si element are very approaching, and the optimization of this electron microscopy observation condition is for strengthening the gray difference effect of above-mentioned phase in the power spectrum image not obvious.
Summary of the invention
The purpose of this invention is to provide a kind of method that improves Inorganic Non-metallic Materials sample power spectrum mapping image quality, it can increase the gray difference of phase in the power spectrum mapping that chemical composition is close, alleviate the phenomenons such as granule interior pixel disappearance, edge virtualization, integral image drift, shorten the image acquisition time.In addition, the method contributes to reduce the sample preparation difficulty, shorten the test duration of optimizing the electron microscopy observation condition, and shooting process is without cooled with liquid nitrogen.
The method of the raising Inorganic Non-metallic Materials powdered sample power spectrum mapping image quality that the present invention proposes, concrete steps are as follows:
(1) sample is installed: sample is put into to the non-magnetic rustproof steel bracket, and inspection surface upwards, is installed firmly, and then, the bolt by the magnetism-free stainless steel frame bottom is fixed on sample and non-magnetic rustproof steel bracket integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: be connected with 3-4 root conducting resinl between sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that gathers essential element in sample with silicon drift electricity refrigeration X-ray energy spectrum detector, accelerating potential used is 15-30kV, test duration is 1-2h, in image acquisition process without cooled with liquid nitrogen;
Wherein: the potpourri that described sample is Inorganic Non-metallic Materials powder or block and epoxy resin composition.
In the present invention, sample described in step (1) the has been evaporation sample of carbonaceous conductive layer.
In the present invention, Inorganic Non-metallic Materials be in the materials such as cement, flyash or slag any.
With traditional image-pickup method, compare, the present invention has following characteristics:
(1) sample installation method: do not adopt conducting resinl directly sample to be adhered to the conventional way on the electron microscopy observation platform, and adopt the special stand fixed sample, then by the bolt attachment bracket of frame bottom and the installation method of electron microscopy observation platform.It is more firm that this not only can make sample install, and avoided the image drift produced because of the conducting resinl temperature distortion in the observation process, and after making off-test, the sample dismounting is more convenient;
(2) the sample inspection surface is pasted the method for conducting resinl: strengthen conductive capability by the quantity that increases conducting resinl, reduce the charge accumulated on inspection surface;
(3) power spectrum image-pickup method: with silicon drift electricity refrigeration X-ray energy spectrum detector, substitute traditional lithium drift detector.Because counting rate that can spectrum signal significantly improves, therefore, the image acquisition time shorten, the factors such as the grinding and polishing quality of sample inspection surface, electron microscopy observation condition weaken the impact of picture quality, in the power spectrum image, the gray difference of the close phase of chemical composition increases, and the phenomenons such as granule interior pixel disappearance, edge virtualization, integral image drift are alleviated.
The accompanying drawing explanation
Fig. 1 is the Ca element power spectrum mapping picture of embodiment 1 by the cement clinker-gypsum mixtures of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 2 is the Ca element power spectrum mapping picture of embodiment 1 by the cement clinker-gypsum mixtures of lithium drift silicon X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 3 is the Ca element power spectrum mapping picture of embodiment 2 by the I type portland cement of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 1000 times.
Fig. 4 is the Si element power spectrum mapping picture of embodiment 2 by the I type portland cement of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 1000 times.
Fig. 5 is the Al element power spectrum mapping picture of embodiment 3 by the flyash of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 6 is the Si element power spectrum mapping picture of embodiment 3 by the flyash of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 7 is the Ca element power spectrum mapping picture of embodiment 4 by the slag of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 8 is the Si element power spectrum mapping picture of embodiment 4 by the slag of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Fig. 9 is the Al element power spectrum mapping picture of embodiment 4 by the slag of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Figure 10 is the Mg element power spectrum mapping picture of embodiment 4 by the slag of silicon drift electricity refrigeration X-ray energy spectrum detector collection, and the image enlargement factor is 500 times.
Embodiment
Further illustrate the present invention below by embodiment.
Embodiment 1, and the phase of observing a kind of cement clinker-gypsum mixtures with the power spectrum mapping forms and distributes, and according to following steps, carries out image acquisition:
(1) sample is installed: will complete polishing, polishing, and evaporation the cement clinker-gypsum of carbonaceous conductive layer-epoxy resin samples put into the non-magnetic rustproof steel bracket, inspection surface upwards, install firmly, then, the bolt by frame bottom is fixed on sample and support integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: with 3 conducting resinls, connect sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that gathers the Ca element with silicon drift electricity refrigeration X-ray energy spectrum detector.Accelerating potential used is 20kV, and the image enlargement factor is 500 times, and the test duration is 2h.
Embodiment 2, and the phase of observing a kind of I type portland cement with the power spectrum mapping forms and distributes, and according to following steps, carries out image acquisition:
(1) sample is installed: will complete polishing, polishing, and evaporation the portland cement-epoxy resin samples of carbonaceous conductive layer put into the non-magnetic rustproof steel bracket, inspection surface upwards, install firmly, then, the bolt by frame bottom is fixed on sample and support integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: with 3 conducting resinls, connect sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that simultaneously gathers Ca and Si element with silicon drift electricity refrigeration X-ray energy spectrum detector.Accelerating potential used is 20kV, and the image enlargement factor is 1000 times, and the test duration is 2h.
Embodiment 3, and the phase of observing a kind of flyash with the power spectrum mapping forms and distributes, and according to following steps, carries out image acquisition:
(1) sample is installed: will complete polishing, polishing, and evaporation the flyash-epoxy resin samples of carbonaceous conductive layer put into the non-magnetic rustproof steel bracket, inspection surface upwards, install firmly, then, the bolt by frame bottom is fixed on sample and support integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: with 4 conducting resinls, connect sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that simultaneously gathers Al and Si element with silicon drift electricity refrigeration X-ray energy spectrum detector.Accelerating potential used is 20kV, and the image enlargement factor is 500 times, and the test duration is 2h.
Embodiment 4, and the phase of observing a kind of slag with the power spectrum mapping forms and distributes, and according to following steps, carries out image acquisition:
(1) sample is installed: will complete polishing, polishing, and evaporation the slag-epoxy resin samples of carbonaceous conductive layer put into the non-magnetic rustproof steel bracket, inspection surface upwards, is installed firmly, then, the bolt by frame bottom is fixed on sample and support integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: with 4 conducting resinls, connect sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that simultaneously gathers Ca, Si, Al and Mg element with silicon drift electricity refrigeration X-ray energy spectrum detector.Accelerating potential used is 20kV, and the image enlargement factor is 500 times, and the test duration is 2h.
Fig. 1 is the Ca element power spectrum image with the cement clinker-gypsum mixtures of method collection of the present invention.In figure, to form between different particles gray difference large for phase, and the gray difference between each pixel of same granule interior is little.This phenomenon is the highest C of content in cement clinker
3in the S phase, embody very obviously.If carry out Digital Image Processing with this original image, by making phase form different particles, more easily distinguish, and, can also reduce the noise of granule interior.By contrast, using the power spectrum image of traditional lithium drift silicon X-ray energy spectrum detector collection same sample instead finds, phase forms gray difference between different particles and reduces, gray difference between each pixel of same granule interior increases on the contrary, and also there is pixel disappearance (Fig. 2) in various degree in the part granule interior.
The power spectrum mapping picture of essential element Ca and Si in employing silicon drift electricity refrigeration X-ray energy spectrum detector collection I type portland cement, result as shown in Figure 3 and Figure 4.Therefrom can find out, in image, the grain edges corner angle are clearly demarcated, and between the various phases of same granule interior, boundary is clear, without virtualization, drift phenomenon, of particular concern is C
3s and C
2the S contrast is obvious.
In addition, in the test of carrying out in the present invention, no matter be at 500 times or at 1000 times of lower photographic images, adopt the test duration of silicon drift electricity refrigeration X-ray detector to be 2h, want 2.5h with lithium drift silicon X-ray detector, and image effect is slightly inferior.
Above-mentioned application example shows that Phase Analysis of the present invention forms for phases such as grog, cement that to take crystalline state be that main material is suitable for.In addition, when analyzing the abundant Inorganic Non-metallic Materials (as flyash, slag etc.) of glassy state phase content, the present invention also has clear superiority.It has solved that the conventional test methodologies such as X-ray diffraction in the past can only generally judge whether amorphous substance exists but the problem that can't detect concrete compound type and distribution thereof is pushed ahead the amorphous state material phase analysis greatly.
For example, Fig. 5 and Fig. 6 are the power spectrum mapping pictures of two kinds of essential element Al and Si in flyash.Therefrom can find out, in flyash, most of particle all contains abundant Al and Si element, but its content is not quite similar, and even if, same granule interior, it is also comparatively general that phase forms inhomogeneous phenomenon.By contrast, from the power spectrum image of slag main composition Elements C a, Si, Al and Mg, in slag between variable grain and the phase of same granule interior form difference much smaller than flyash (Fig. 7-Figure 10).In the power spectrum image of this bi-material, the phenomenons such as electric discharge, image drift all occur, and the grain edges corner angle are clearly demarcated, it is very little that the granule interior phase forms between consistent area pixel gray difference.As can be seen here, method of the present invention can shorten the image acquisition time, increases the gray difference of the close phase of chemical composition in the power spectrum image, alleviates the phenomenons such as granule interior pixel disappearance, grain edges virtualization, integral image drift.In addition, the impact of the factors such as sample grinding and polishing quality, electron microscopy observation condition on picture quality can also be weakened, therefore, time cost and the financial cost of groping sample preparation technique and optimizing the electron microscopy observation condition can be reduced.And method of the present invention is all effective for the crystalline state phase in material and amorphous state phase.
Claims (2)
1. a method that improves Inorganic Non-metallic Materials sample power spectrum mapping image quality is characterized in that concrete steps are as follows:
(1) sample is installed: sample is put into to the non-magnetic rustproof steel bracket, and inspection surface upwards, is installed firmly, and then, the bolt by the magnetism-free stainless steel frame bottom is fixed on sample and non-magnetic rustproof steel bracket integral body on the measuring platform of scanning electron microscope;
(2) paste conducting resinl: be connected with 3-4 root conducting resinl between Inorganic Non-metallic Materials powdered sample inspection surface and rack side wall;
(3) power spectrum mapping picture gathers: the power spectrum mapping picture that gathers essential element in sample with silicon drift electricity refrigeration X-ray energy spectrum detector, accelerating potential used is 15-30kV, test duration is 1-2h, in image acquisition process without cooled with liquid nitrogen;
Wherein: the potpourri that described sample is Inorganic Non-metallic Materials powder or block and epoxy resin composition.
2. method according to claim 1, is characterized in that the sample of carbonaceous conductive layer that has been evaporation of sample described in step (1).
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| CN105241904A (en) * | 2015-09-22 | 2016-01-13 | 同济大学 | Energy dispersion X-ray spectrum-based analysis method for phases of fly ash |
| CN114199919A (en) * | 2021-10-11 | 2022-03-18 | 中国航发北京航空材料研究院 | Image processing method based on X-ray energy spectrum micro-area surface scanning |
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| CN114199919A (en) * | 2021-10-11 | 2022-03-18 | 中国航发北京航空材料研究院 | Image processing method based on X-ray energy spectrum micro-area surface scanning |
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Application publication date: 20131218 |