JP3869988B2 - Spectral display device for surface analysis equipment - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention is an electron probe microanalyzer (abbreviated as EPMA) equipped with both a wavelength dispersive X-ray spectrometer (abbreviated as WDS) and an energy dispersive X-ray spectrometer (abbreviated as EDS). It is related with the spectrum display apparatus in surface analysis equipment.
[0002]
[Prior art]
In general, surface analysis equipment such as an electron probe microanalyzer equipped with both a wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer is quickly included on the surface of a sample using the energy dispersive X-ray spectrometer. An outline of the existing elements is analyzed, and a more detailed and precise analysis is performed using a wavelength dispersive X-ray spectrometer. Since the wavelength dispersive X-ray spectrometer performs spectroscopy using a spectroscopic crystal, the spectrum of the wavelength dispersive X-ray spectrometer has n = 2 or more, as is apparent from the Bragg equation shown in the following equation (1). So-called higher order lines appear. 2d · sinθ = nλ (1)
Here, d is the lattice spacing of the spectral crystal, θ is the incident angle of the X-ray to the spectral crystal, λ is the wavelength of the X-ray, n is a natural number and represents the diffraction order.
[0003]
On the other hand, since such higher-order lines do not appear in the spectrum of the energy dispersive X-ray spectrometer, conventionally, the spectrum used in the wavelength dispersive X-ray spectrometer is on the spectrum of the energy dispersive X-ray spectrometer. A marker or the like for displaying the position of the higher-order line of the characteristic X-ray that appears as a spectrum by the crystal is not displayed. For this reason, when a detailed and precise analysis is performed using a wavelength dispersive X-ray spectrometer based on the result of a rough analysis using an energy dispersive X-ray spectrometer, other characteristics X are present in the vicinity of the primary X-ray of the target element. Even when higher-order lines appear, and corresponding processing must be performed, such higher-order lines do not appear in the spectrum of the energy-dispersive X-ray spectrometer. At present, it is not known from the spectrum of the spectroscope whether or not such higher-order lines appear in the analysis of the wavelength dispersive X-ray spectrometer.
[0004]
[Problems to be solved by the invention]
In a surface analysis instrument equipped with both a conventional wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer, the spectrum of the energy dispersive X-ray spectrometer is the wavelength dispersive X-ray spectrometer as described above. Since no high-order line information peculiar to is displayed, even if a high-order line of another characteristic X-ray appears in the vicinity of the target primary line used in the wavelength dispersive X-ray spectrometer, the energy Such an aspect cannot be known only from the spectrum of a dispersive X-ray spectrometer, and therefore, necessary information can be obtained as quickly as possible when performing detailed and precise analysis using a wavelength dispersive X-ray spectrometer. This is not sufficient for the role as an energy dispersive X-ray spectrometer.
[0005]
The present invention has been made in order to solve the above-mentioned problems in a surface analysis instrument equipped with both a conventional wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer. It is an object of the present invention to provide a spectrum display device in a surface analysis instrument that can quickly obtain information necessary for performing detailed and precise analysis using a slab.
[0006]
[Means for Solving the Problems]
In order to solve the above problems, the invention according to claim 1 is a surface analysis instrument equipped with both a wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer, comprising a display means and a specifying means , with the said display means for displaying the spectrum obtained by energy dispersive X-ray spectrometer, on the spectrum, to display the energy range specified by the specifying means, further using a wavelength dispersive X-ray spectrometer spectroscopy A spectrum display device in a surface analysis instrument is configured to display on the same display surface a list of higher-order lines located within the specified range among the higher-order lines of characteristic X-rays that appear after being separated by crystals. Is .
[0007]
By configuring as this will become apparent information wavelength dispersive X-ray spectrometer specific higher-order lines in the given energy range is contrasted with energy dispersive X-ray spectrometer spectrum, wavelength dispersive X-ray It is possible to quickly obtain useful information when performing detailed and precise analysis with a spectroscope.
[0010]
The invention according to claim 2 is the spectrum display device in the surface analysis instrument according to claim 1 , wherein the list of higher-order lines to be displayed exists in the qualitative analysis based on the spectrum obtained by the energy dispersive X-ray spectrometer. It is a list of higher-order lines of characteristic X-rays of elements after adding confirmed elements or elements that may be present and then deleting elements that are misidentified. is there. With this configuration, in addition to what appears to possibly exist before Symbol confirmation element can display a list of higher-order lines in addition to the confirmation element, more efficiently wavelength dispersive Appropriate analysis processing of the X-ray spectrometer can be performed.
[0011]
The invention according to claim 3 is the spectrum display device in the surface analysis instrument according to claim 1 , wherein the list of higher-order lines to be displayed is not all elements that can be analyzed by the surface analysis instrument or the possibility of existence thereof. It is a list of high-order lines of characteristic X-rays of elements after the elements are deleted. This makes it possible to display a list of higher-order lines, excluding all elements that can be analyzed by the surface analysis instrument or elements that may not be present, and can efficiently and efficiently perform wavelength dispersive X-ray spectroscopy without leakage. It is possible to perform accurate analysis processing of the vessel.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
Next, embodiments will be described. FIG. 1 is a block configuration diagram showing an embodiment of a spectrum display device for a surface analysis instrument according to the present invention. In this embodiment, the present invention is applied to an electron probe microanalyzer. In FIG. 1, 1 is an electron beam, 2 is an objective lens, 3 is a sample, 4 is a wavelength dispersive X-ray spectrometer, and 5 is a spectroscope. Crystal, 6 is an X-ray detector, 7 is an energy dispersive X-ray spectrometer, 8 is an X-ray generation point of the sample irradiated with the electron beam, 9 is an X-ray detector 6 of the wavelength dispersive X-ray spectrometer 4 And a processing / control unit 10 for processing detection signals from the energy dispersive X-ray spectrometer 7 and controlling each part of each spectroscope, etc., and 10 is an energy dispersive X obtained by processing by the processing / control unit 9. X-ray spectrometer spectrum, energy dispersive X-ray spectrometer spectrum of elements that have been confirmed to exist , position of higher-order X-rays of characteristic X-rays appearing by spectral crystals used in wavelength-dispersive X-ray spectrometers, wavelength dispersion Type X-ray spectrometer spectrum, etc. Display unit, 11 to specify the energy range of the spectra obtained by energy dispersive X-ray spectrometer, an operation instructing section to be used for such as specifying the spectral crystal used in wavelength-dispersive X-ray spectrometer.
[0013]
First, prior to the description of the operation of the embodiment of the present invention, an X-ray spectrum detected by an energy dispersive X-ray spectrometer will be described with reference to FIG. In FIG. 2, the horizontal axis indicates energy (eV), and the vertical axis indicates the intensity (count value) of X-rays. In the figure, e is an X-ray spectrum, and e1 to e7 indicate characteristic X-rays (primary lines) of elements present in the sample. In an apparatus equipped only with an energy dispersive X-ray spectrometer, information on higher-order rays peculiar to the wavelength dispersive X-ray spectrometer is unnecessary. An electron probe microanalyzer equipped with both a wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer that performs detailed and precise analysis using a wavelength dispersive X-ray spectrometer based on the results of the rough analysis of If high-order line information unique to the X-ray spectrometer is revealed on the spectrum of the energy-dispersive X-ray spectrometer, the high-order line can be used for detailed and precise analysis using the wavelength-dispersive X-ray spectrometer. It is possible to eliminate or suppress the influence of and to perform an accurate analysis process.
[0014]
Therefore, in the present invention, characteristic X-rays appearing on the spectrum of the energy dispersive X-ray spectrometer on the element that has been confirmed to exist based on the spectrum and appearing as a spectrum by the spectroscopic crystal used in the wavelength dispersive X-ray spectrometer. 3 shows the position of the secondary line A (2 ) which appears when the spectral crystal (1) of the characteristic X-ray A is used on the spectrum e of the energy dispersive X-ray spectrometer. ), Cubic lines A (3) and quaternary lines A (4) appearing when using the spectral crystal (2) , quintic lines A (5) appearing when using the spectral crystal (3 ), and other The position of the secondary line B (2) that appears when using the spectroscopic crystal (2) of the characteristic X-ray B and the position of the tertiary line B (3) that appears when using the spectroscopic crystal (3) are displayed. An example is shown.
[0015]
Here, the difference in the type of spectral crystal is indicated by the difference in the type of marker line (solid line, dotted line, wavy line), but when displayed on a color display, it may be indicated by a difference in color. In addition, the type of characteristic X-ray to be displayed can be arbitrarily selected from one type or a plurality of types, the type of spectral crystal can be arbitrarily selected from one type or a plurality of types, and the order of higher-order lines can be one or more types. These can be arbitrarily selected, and these can be selected by an instruction from the operation instruction unit 11.
[0016]
FIG. 3 shows an example in which the order of the higher order line is 5th order or less. However, if the energy of the characteristic X-ray i displayed as the higher order line is Ei and the order of the higher order line is n, the energy is The position of the n-order marker of the characteristic X-ray i displayed on the horizontal axis (energy axis) of the dispersive X-ray spectrometer spectrum is the position of Ei / n.
[0017]
FIG. 4 shows an arbitrary energy range W on the spectrum e of the energy dispersive X-ray spectrometer, and the spectral crystal name for the characteristic X-ray whose nth-order marker position Ei / n is in the energy range W, X-ray name, higher-order line order (n), value obtained by dividing the X-ray energy by the order (Ei / n), and spectral position L (R is the Roland circle radius, θ is the X-ray to the spectroscopic crystal In the case of a linearly converging X-ray spectrometer, for example, an angle of incidence is represented on the energy dispersive X-ray spectrometer spectrum screen by a table showing, for example, L = 2R · sin θ. Show. FIG. 4 is an example showing a table below the quaternary line, whereby the information on the high-order line peculiar to the wavelength dispersive X-ray spectrometer in the specified energy range W is obtained as an energy dispersive X-ray spectrometer spectrum. As a result, it becomes clear that effective information can be obtained when a detailed / precise analysis is performed with a wavelength dispersion X-ray spectrometer.
[0018]
FIG. 5 shows a high-order line [secondary line of characteristic X-ray C2 that appears in the wavelength-dispersive X-ray spectrometer with respect to characteristic X-rays C1, C2, and C3 identified from the spectrum of the energy dispersive X-ray spectrometer. C2 (2) and tertiary line C2 (3), characteristic X-ray C3 secondary line C3 (2), tertiary line C3 (3), quaternary line C3 (4) and quintic line C3 (5)] Is displayed on the spectrum screen of the energy dispersive X-ray spectrometer. Depending on the type of spectral crystal (spectral crystal (1), (2), (3)) of the wavelength dispersive X-ray spectrometer capable of separating each higher order line, the type of the higher order line display marker line (solid line, (Dotted line, wavy line) are changed.
[0019]
As described above, according to the present invention, high-order information unique to a wavelength dispersive X-ray spectrometer is clarified on the spectrum of the energy dispersive X-ray spectrometer. It is possible to quickly obtain necessary information when performing a simple analysis, and to appropriately eliminate the influence of higher-order lines during the analysis. Furthermore, when performing analysis using a wavelength dispersive X-ray spectrometer, if there is a higher-order line of other characteristic X-rays near the primary line, the wave-height analyzer is changed to that based on that information. It is possible to easily set a high-order line and to determine a background measurement position so as to avoid the high-order line, thereby avoiding or reducing the influence of the high-order line in advance.
[0020]
【The invention's effect】
As described above based on the embodiments, according to the invention of 請 Motomeko 1, designated wavelength dispersive X-ray spectrometer specific higher-order lines of information energy dispersive X-ray spectroscopy in the energy range It becomes clear as compared with the spectrum of the instrument, and it is possible to quickly obtain effective information when performing detailed and precise analysis with the wavelength dispersive X-ray spectrometer . According to the invention of or claim 2, add the possible elements of an energy dispersive X-ray present in qualitative analysis based on spectrum obtained on the spectrometer was confirmed elemental or present in it, and then Since the list of higher-order X-rays of the characteristic X-rays of elements after the elements whose existence has been mistakenly deleted is displayed, efficient analysis processing of a wavelength dispersion X-ray spectrometer can be performed efficiently. Can do. According to the invention of claim 3 , a list of high-order lines of characteristic X-rays of elements after all elements that can be analyzed or elements that may not be present are deleted is displayed. Thus, it is possible to perform an accurate analysis process of the wavelength dispersion X-ray spectrometer efficiently without leakage.
[Brief description of the drawings]
FIG. 1 is a block configuration diagram showing an embodiment of a spectrum display device in a surface analysis instrument according to the present invention.
FIG. 2 is a diagram showing only an X-ray spectrum detected by an energy dispersive X-ray spectrometer.
FIG. 3 shows a mode in which the positions of higher-order lines in characteristic X-rays appearing on the X-ray spectrum detected by the energy dispersive X-ray spectrometer are separated by the spectroscopic crystal used in the wavelength dispersive X-ray spectrometer. FIG.
FIG. 4 designates an arbitrary energy range on the spectrum of the energy dispersive X-ray spectrometer, and is located within the specified range among the characteristic X-rays that appear after being dispersed by the spectroscopic crystal used in the wavelength dispersive X-ray spectrometer. It is a figure which shows the aspect which displayed the list | wrist of the high-order line on the same screen.
FIG. 5 shows the position of the higher-order line represented by the wavelength dispersive X-ray spectrometer on the spectrum of the energy dispersive X-ray spectrometer with respect to the characteristic X-ray identified from the spectrum of the energy dispersive X-ray spectrometer. It is a figure which shows the aspect displayed on.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Electron beam 2 Objective lens 3 Sample 4 Wavelength dispersive X-ray spectrometer 5 Spectroscopic crystal 6 X-ray detector 7 Energy dispersive X-ray spectrometer 8 X-ray generation point 9 Processing / control unit
10 Display section
11 Operation instruction section

Claims (3)

  A surface analysis instrument equipped with both a wavelength dispersive X-ray spectrometer and an energy dispersive X-ray spectrometer, comprising a display means and a specifying means, wherein the display means is a spectrum obtained by the energy dispersive X-ray spectrometer. The energy range designated by the designation means is displayed on the spectrum, and further, the designation among the higher-order lines of characteristic X-rays that appear after being dispersed by a spectral crystal used in a wavelength dispersive X-ray spectrometer. A spectrum display device in a surface analysis instrument characterized in that it is configured to display a list of higher-order lines located within a specified range on the same display surface. The list of higher-order lines to be displayed is added with elements that have been confirmed to exist by qualitative analysis based on the spectrum obtained by the energy dispersive X-ray spectrometer, or elements that may be present, and are then misidentified. The spectrum display device in the surface analysis instrument according to claim 1 , wherein the spectrum display device is a list of higher-order lines of characteristic X-rays of elements after the removed elements are deleted. The list of higher-order lines to be displayed is a list of higher-order lines of characteristic X-rays of elements after all elements that can be analyzed by the surface analysis instrument or elements that may not exist are deleted. A spectrum display device in a surface analysis instrument according to claim 1 .

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