JPH0744022B2 - X-ray micro analyzer - Google Patents

Description

TECHNICAL FIELD The present invention relates to an X-ray microanalyzer which detects characteristic X-rays emitted from a sample irradiation unit by irradiating a sample with an electron beam.

[Conventional technology]

The X-ray microanalyzer (EPMA) irradiates a sample with an extremely narrowed electron beam, measures the wavelength and intensity of the characteristic X-rays emitted from the sample irradiation part with an X-ray spectroscope, and measures the sample irradiation part. A device for qualitative or quantitative analysis of the elements contained in.

In general, characteristic X-rays of elements are Kα, Kβ, Lα, Lβ,
There are many types, such as ASTM Data Series
The wavelength table defined by DS37A describes the wavelengths of a few thousand X-rays. These X-rays are also observed by EPMA. On the other hand, in the wavelength dispersive spectrometer, diffraction occurs even at an integral multiple of the X-ray wavelength, and the X-ray is also observed. In EPMA, 10
The number of X-rays that can be observed and identified up to the next X-rays easily exceeds 10,000. Moreover, since the peak waveform of the observed X-rays has a certain spread, it is routine that the X-rays are observed to overlap each other.

[Problems to be Solved by the Invention]

As described above, each X-ray peak observed by EPMA contains various elements. Therefore, when focusing on a certain peak, it is determined which characteristic X-ray of which element the peak belongs to. Can often be difficult.

The present invention solves the above problems, and an object thereof is to provide an X-ray microanalyzer capable of easily determining which X-ray of which element an arbitrary X-ray spectrum belongs to. It is a thing.

[Means for Solving the Problems]

Therefore, the present invention is an X-ray microanalyzer for detecting characteristic X-rays emitted from an electron beam irradiation part of a sample, and a wavelength table including information such as the type, wavelength, and intensity of characteristic X-rays corresponding to elements. And an identification table in which information of already identified elements is registered, and a peak specified by referring to the wavelength table and the identification table when an element is identified by displaying an X-ray spectrum and designating a specific peak Display processing means for displaying the X-ray information for each element from the wavelength of, the display processing means displays the X-ray information of the element existing within the predetermined range from the wavelength of the designated peak, and the predetermined range. Among the X-ray information of the elements present inside, the X-ray information of the same element as the element present in the identification table is displayed in different colors using different colors.

[Action]

In the X-ray microanalyzer of the present invention, when an element identified by performing the identification process is registered in the identification table and a specific peak is designated to identify the element, the peak is identified from the wavelength table. The X-rays of the elements within the predetermined range are displayed, and the X-rays of the elements that are known in advance are displayed in different colors based on the identification table, so that information when performing identification can be accurately given. .

〔Example〕

 Hereinafter, embodiments will be described with reference to the drawings.

FIG. 1 is a diagram for explaining one embodiment of an X-ray microanalyzer according to the present invention, FIG. 2 is a diagram showing a configuration example of a wavelength table, and FIG. 3 is for explaining an X-ray peak determination range. FIG. 4, FIG. 4 is a diagram showing an example of a spectrum in which two elements are mixed, FIG. 5 is a diagram for explaining manual peak identification of observed X-rays, and FIG. 6 is a flow of X-ray identification processing. FIG.

In FIG. 1, 1 is an electron gun, 2 is a converging lens, 3 is an objective lens, 4 is a scanning coil, 5 is a sample, 6 is a sample stage, 7 is an electron beam, 8 is a characteristic X-ray, 9 is a dispersive crystal, 10 is a spectroscope drive motor, 11 is a detector, 12 is a spectroscope control circuit, 13
Is an arithmetic control circuit, 14 is a measurement circuit, 15 is a storage device, 16 is a wavelength table, 17 is an element table, and 18 is an output device.

In the X-ray microanalyzer system shown in FIG. 1,
An electron beam 7 generated by the electron gun 1 is narrowed down through a converging lens 2 and an objective lens 3 to irradiate the sample 5, and a characteristic X-ray 8 radiated from the electron beam irradiation section is detected by a detector 11.

Here, the wavelength table 16 is made up of information such as X-ray type, wavelength, and intensity for each element as shown in FIG. 2, and the element table 17 is determined as an element contained in the sample. It consists of things. Further, the spectroscope control circuit 12 controls the spectroscope drive motor 10 to move the dispersive crystal 9, and the detector 11 also moves in conjunction with the movement of the dispersive crystal 9, and the wavelength corresponding to the moving position. The characteristic X-ray of is detected by the detector 11. Then, the detected characteristic X-rays of each wavelength are stored in the storage device 15 through the measurement circuit 14,
The spectrum of the characteristic X-ray is output to the display device 18.

The arithmetic control circuit 13 is composed of, for example, a computer, and controls the operation of the spectroscope control circuit 12 and the measurement circuit 14, processes the data in the storage device 15, controls the display screen of the display device 18, and the like. In the manual peak identification of the line, the spectrum obtained from the sample 5 and stored in the storage device 15 is displayed on the display device 18, and at the same time, the specific X designated by the cursor is displayed.
With respect to the line peaks, the wavelength table 16 and the element table 17 are referred to, and a list display (listing up) of the X-rays and color-coded display are performed. As for the specific X-ray peak designated by the cursor, as shown in FIG.
The width at half intensity (half-value width, half-value width) is taken, and X-rays of elements contained in a certain width are slit as a function of this half-value width.

Next, the display control in the manual peak identification of the observation X-ray in the arithmetic control circuit 13 will be described with reference to FIGS.

The spectra shown in FIG. 4 are characteristic X-rays AX ₁ and AX _{2 of} element A.
And the characteristic X-rays BX ₁ and BX _{2 of the} element B exist, and among them, the characteristic X-rays AX ₂ and BX ₁ show the case where the peak positions are close to each other and separation is difficult. Therefore, in such a relationship, one element may not be contained at all in the actual sample, or both elements may be contained. is necessary.

Therefore, in the identification method of the elements contained in the sample, in order to check which characteristic X-ray of which element a specific X-ray peak is, first, as shown in FIG.
The line spectrum data is read and the X-ray spectrum is displayed on the screen of the display device 18. When the X-ray spectrum is displayed, the operator uses the mouse or the like to move the cursor to the target X-ray spectrum on the screen as shown in FIG. 5, and selects the X-ray peak designated by this cursor. (,).

On the other hand, referring to the X-ray wavelength table, the position of the X-ray spectrum and the wavelength table are sequentially compared, and the one close to the peak position is investigated and listed as shown in Fig. 5 BX ₁ , CX ₁ , AX ₁ , ... To do. At this time, the wavelength table uses the values corrected by the spectroscope position correction mechanism. This is for correcting the actual reading of the spectroscope and the theoretical X-ray position, and the correction amount is previously determined as a function of the X-ray position using a standard sample. In addition, since the observed X-ray peak has a certain width, whether or not the X-ray is suitable is
A certain width is given as a function of the half-value width, and if it is within that range, it is determined that there is a possibility (~
).

Then, the X-rays which may be within the predetermined range are displayed on the screen in the form of a table as shown in FIG. At this time, it is compared with the above-mentioned identification element table, and when it is an X-ray of the element in the table, it is color-coded and displayed (~
).

Further, as shown in FIG. 2, since the wavelength table has the information on the type and wavelength of the X-ray and the intensity for each element, the detected X-ray peak is compared with the KLM line of the element, and the wavelength is compared. The probability of the element is determined based on the comparison between the intensity of the table information and the displayed spectrum intensity and the like, and ranked in that order. For example, the A rank is an element which is almost certain to be contained in the sample, the B rank is an element which may be contained in the sample, and the C rank is an element which is not likely. Then, in identifying the elements contained in the sample, the most probable element is selected from these.

Thus, the present invention makes use of the fact that the information is useful when the element already contained in the sample is known by some method. It is not uncommon for the number of X-rays that may belong to a certain peak to be several tens, so it is practically very convenient to color-code the X-rays of elements that have already been determined.

The present invention is not limited to the above embodiment, and various modifications can be made. For example, in the above embodiment, the X-rays judged to be possible are displayed in different colors.
Color may be classified according to the ranks of B and C. Further, when any one of the possible X-ray tables is selected, all X-rays of the element may be displayed as a KLM marker in an overlapping manner with the X-ray spectrum. By doing so, the display can be made more understandable, and the X-ray spectrum can be analyzed in more detail.

〔The invention's effect〕

As mentioned above, any X-ray spectrum shows which X of which element
Whether or not it belongs to a line is determined by comparison with a wavelength table, but it is not rare that the number of possible X-rays reaches to several tens. As is clear from the above description, according to the present invention,
Even in such a case, since the X-rays of the elements that are known in advance are displayed in different colors, the possibility that the X-rays are erroneously identified can be reduced.

Further, in the X-ray microanalyzer, in order to scan the entire spectral range from the relationship of the spectral range of the dispersive crystal,
Several X-ray spectra (minimum 4) are required. Therefore, when only one spectrum is being viewed, a peak included in another spectrum may be missed and a judgment error may be made. However, according to the present invention, the judgment error can be reduced.

[Brief description of drawings]

FIG. 1 is a diagram for explaining one embodiment of an X-ray microanalyzer according to the present invention, FIG. 2 is a diagram showing a configuration example of a wavelength table, and FIG. 3 is for explaining an X-ray peak determination range. FIG. 4, FIG. 4 is a diagram showing an example of a spectrum in which two elements are mixed, FIG. 5 is a diagram for explaining manual peak identification of observed X-rays, and FIG. 6 is a flow of X-ray identification processing. FIG. 1 ... Electron gun, 2 ... Converging lens, 3 ... Objective lens,
4 ... Scanning coil, 5 ... Sample, 6 ... Sample stage,
7 ... electron beam, 8 ... characteristic X-ray, 9 ... dispersive crystal, 10 ...
… Spectroscope drive motor, 11 …… Detector, 12 …… Spectroscope control circuit, 13 …… Computation control circuit, 14 …… Measurement circuit, 15 …… Storage device, 16 …… Wavelength table, 17 …… Element table , 18
...... Output device.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Koji Yoshida 3-1-2 Musashino, Akishima-shi, Tokyo JEOL Ltd. (56) Reference JP-A-60-179641 (JP, A) JP-A-60 -135849 (JP, A)

Claims (1)

[Claims] 1. A characteristic X emitted from an electron beam irradiation portion of a sample.
In an X-ray microanalyzer for detecting X-rays, a wavelength table including information such as the type, wavelength, and intensity of characteristic X-rays corresponding to elements, an identification table in which information of already identified elements is registered, and X-rays A display processing unit for displaying X-ray information for each element from the wavelength of the designated peak with reference to the wavelength table and the identification table when the spectrum is displayed and a specific peak is designated to identify the element; The display processing means displays X-ray information of an element existing within a predetermined range from the wavelength of the designated peak, and is the same as the element existing in the identification table among the X-ray information of the element existing within the predetermined range. An X-ray microanalyzer, which displays X-ray information of an element in different colors using different colors.