JPH06231717A - Sample analyzing method x-ray microanalyzer - Google Patents

Abstract

PURPOSE:To display a graph correlatively showing the attitude of frequency distribution of the characteristic X-ray intensities taken by picture elements of two elements in a noticeable area in a color mapping image. CONSTITUTION:As elements to be correlatively displayed, elements theta1 and theta2 are designated by a keyboard 7. The data for picture elements contained in a designated area S of the stored data of an image memory area A1 and the data for picture elements contained in the area S of the stored data of an image memory area A2 are transmitted to a correlative graphic data forming part 17. In the correlative graphic data forming part 17, the date for the i-th picture element contained in the area S stored in the image memory area A2 is proportionally converted into the Y-coordinate yi of the i-th display point, which is then transmitted to a display control part 20.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample analysis method in an X-ray microanalyzer for acquiring characteristic X-ray intensity value data of each element in each pixel on a sample surface and analyzing the sample.

[0002]

2. Description of the Related Art In an X-ray microanalyzer,
The sample surface is divided into a number of pixels, and these pixels are sequentially irradiated with an electron beam to generate each element Θ generated from each pixel (x, y).
The characteristic X-rays of 1, Θ2, ..., Θn (n ≧ 2) are detected. In such an apparatus, the characteristic X relating to each of the detected elements Θ1, Θ2, ..., Θn
After the line intensity value data is temporarily stored in the storage device, the characteristic X-ray intensity value data of an arbitrary element Θi is read out based on the instruction of the operator and developed on the display device.

[0003]

When a characteristic X-ray intensity value of a certain element Θi is converted into an n-value and observed as a color mapping image with such an apparatus, it is possible to know the outline of the distribution state of the X-ray intensity value. it can. However, in such a mapping image, the X-ray intensity value signal is compared with a plurality of reference levels to be n-valued, and different colors are assigned to the values of different layers and displayed as a color mapping image. When the area displayed in the same color is seen in more detail, whether the X-ray intensity values of the pixels in this area are dispersed in a relatively wide range or concentrated in a narrow range, that is, this element It is not possible to know the degree of homogeneity of the sample in the region with respect to the concentration of. If the degree of uniformity of the sample in the region regarding the concentration of the element displayed as the mapping image can be known, the knowledge of the region can be deepened. In particular, if the uniformity of the concentrations of the two elements in the region can be known, the knowledge of that portion can be further deepened.

The present invention has been made in view of such a point, and its purpose is to correlate the frequency distribution of characteristic X-ray intensities taken by pixels of two elements in a region of interest in a color mapping image. An object of the present invention is to provide an analysis method in an X-ray microanalyzer capable of displaying a graph that is represented by a symbol.

[0005]

A sample analysis method for an X-ray microanalyzer of the present invention which achieves this object relates to each pixel (x, y) on a two-dimensional plane of a sample by irradiating the sample with an electron beam. Each element Θ1, Θ2, ..., Θn (n
≧ 2) characteristic X-ray intensity value data I1 (x, y), I2
(X, y), ..., In (x, y) are obtained, the obtained data is stored, and an arbitrary element Θi is selected from the stored data.
(I is 1, 2, ..., N) characteristic X-ray intensity value data Ii (x, y) is read, and a distribution image of the element Θi is displayed in a color according to the read data value. , An area S having an arbitrary size is designated at an arbitrary position of the distribution image, and for each two X-ray intensity values of pixels included in the designated area S for any two elements of the respective elements, It is characterized by displaying a graph that correlates the frequency distribution.

[0006]

The present invention will be described in detail below with reference to the drawings.
FIG. 1 is a view showing a main part of an apparatus for carrying out the present invention,
FIG. 2 is a system configuration diagram showing an entire apparatus for carrying out the present invention.

In FIG. 2, 1 is an X-ray microanalyzer (hereinafter abbreviated as XMA), 2 is a sample, EB is an electron beam, C1, C2 and C3 are dispersive crystals, D1, D2 and D.
3 is an X-ray detector, T1, T2 and T3 are X-ray counters, 3 is a CPU, 4 is a storage device, 5 is a color graphic display, 6 is a pointing device such as a digitizer or mouse, 7 is a keyboard, and 8 is a bus. It is a line. The dispersive crystals C1, C2 and C3 are the elements Θ1, Θ2 and Θ, respectively.
It is set so that the three characteristic X-rays can be selected. Further, the pointing device 6 is for pointing this area by drawing an area having an arbitrary position, size and shape on the screen of the color graphic display 5 by a bright line according to an instruction of the operator.

In FIG. 1, 9 is an X-ray intensity value data storage unit, 10 is a writing / reading control unit, 11 is a region designating unit, 12 is a mapping element designating unit, and 13 is an element for which a correlation graph to be described later is drawn. Target element designating section for designating, 14 is a function designating section, 15 is a function selecting section, 17 is a correlation graph data creating section, 18 is a level dividing processing section, 1
Reference numeral 9 is a color classification processing unit, and 20 is a display control unit. As shown in FIG. 1, the storage device 4 is provided with an X-ray intensity value data storage unit 9. The X-ray intensity value data storage unit further corresponds to each element Θ1, Θ2, Θ3. Screen image storage areas A1, A2, A3 are provided. Each one-screen image storage area has a storage area of a predetermined depth for each pixel (x, y) in the sample scanning area by the electron beam EB.

In such a structure, in the state where the sample is irradiated with the electron beam EB, the horizontal moving mechanism of the sample 2 is operated to move the sample 2 two-dimensionally. As a result, each pixel (x, y) of the sample 2 is sequentially irradiated with the electron beam EB. Of the characteristic X-rays generated from each pixel (x, y) of the sample 2 by the irradiation of this electron beam EB, the elements Θ1, Θ
The characteristic X-rays of 2 and Θ3 are the dispersive crystals C1, C2 and C, respectively.
3 is detected by X-ray detectors D1, D2, D3. Therefore, by the X-ray counters T1, T2, T3, each element Θ1, Θ2, Θ3 in each pixel (x, y) is
The count value signal of the characteristic X-ray is sent to the storage device 4 via the bus line 8. Each pixel (x,
The characteristic X-ray intensity value data regarding the element Θ1 of y) is stored in the storage region corresponding to each pixel (x, y) of the image storage region A1 of the X-ray intensity value data storage unit 9. Similarly, the characteristic X-ray intensity value data of the element Θ2 is stored in the image storage area A2,
The characteristic X-ray intensity value data of the element Θ3 is stored in the image storage area A3. Therefore, when the operator uses the keyboard 7 to instruct the color mapping display of the characteristic X-ray intensity distribution of the element Θ1, the mapping element designating section 12 sends a signal instructing the writing / reading control section 10 to select the element Θ1. The read control unit 10 sequentially reads all the data stored in A1 of the image storage area of the X-ray intensity value data storage unit 9 and sends them to the level classification processing unit 18.
The level classification processing unit 18 compares the transmitted X-ray intensity value data with a plurality of preset reference levels. The number and value of the reference levels can be set arbitrarily. In the case of this embodiment, assuming that four reference levels are set as the reference levels, the level division processing unit 18 classifies the transmitted X-ray intensity value data into the inside and outside of each of the reference levels. It is converted into five values by and sent to the color classification processing section 19. In the color-coding processing unit 19, hues corresponding to the hierarchical values are assigned to the 5-valued data sent from the level-dividing processing unit 18, and a signal for displaying each of the assigned hues is sent to the display control unit 20. . As a result, the color graphic display 5 is shown in FIG.
As shown in (a), a color mapping image showing the characteristic X-ray intensity distribution of the element Θ1 is displayed. Similarly, when the operator gives an instruction to display the characteristic X-ray intensity distribution image of the element Θ2, the data shown in FIG.
An image as shown in (b) is displayed on the display 5.
Among such X-ray intensity distribution images, for example, while observing the characteristic X-ray intensity distribution image of the element Θ2, a region of interest is found, and the element Θ2 taken by the pixels included in this region is found.
When the frequency distribution of the characteristic X-ray intensity value of the element Θ1 and the element Θ1 are to be known in a correlated manner, the following may be performed.

That is, first, the operator operates the pointing device 6, and under the control of the area designating section 11, the area S is surrounded by a bright line F as shown in FIG. Also,
The keyboard 7 is used to instruct execution of the correlation graph display.
As a result, the function designation unit 14 sends a control signal to the function selection unit 15, and sets the function selection unit 15 to send the data sent from the X-ray intensity value data storage unit 9 to the correlation graph data creation unit 17. . Therefore, when, for example, the elements Θ1 and Θ2 are designated by the keyboard 7 as the elements to be displayed in correlation, the target element designating unit 13 causes the writing / reading control unit 1 to operate.
0 is informed that the data in the image storage area A1 and the data in the image storage area A2 are selected for reading. Then, when the execution of the display is instructed, the data of the pixels included in the instructed area S in the storage data of the image storage area A1 is sent to the correlation graph data creation section 17 via the function selection section 15 and the image storage area The data of the pixels included in the area S of the stored data of A2 is similarly sent to the correlation graph data creation unit 17. In the correlation graph data creation unit 17, the data of the i-th pixel included in the area S stored in the image storage area A1 is set as the X-coordinate xi of the i-th point displayed on the screen of the display 5. , Data processing for proportionally converting the data of the i-th pixel included in the area S stored in the image storage area A2 into the Y coordinate yi of the i-th display point is performed. Since the data created by such processing is sent from the correlation graphic data creation unit 17 to the display control unit 20, the display control unit 20 displays a correlation graph as shown in FIG. By observing this correlation graph, the operator can know that the uniformity of the distribution of the element Θ2 is low when the spread of the distribution of the displayed points in the direction of the element Θ2 axis is large. It can be known that the concentration of the element Θ2 is uniform over the region S if the spread of the distributed points in the axial direction of the element Θ2 is narrow. Similarly, the degree of uniformity of the concentration of the element Θ1 can be known by observing the spread of the display point in the direction of the element Θ1 axis. It can be seen that the density has an inverse correlation in the area S.

The above-described embodiment is only one embodiment of the present invention, and the present invention can be modified and implemented.

For example, in the above-described embodiment, the pointing device unit is used to indicate an area having not only an arbitrary position and size but also an arbitrary shape. However, in FIG. As shown by K1, K2, and K3, a rectangle whose size is changed stepwise and its position is arbitrarily changed is displayed, and the region is designated by designating the position and size of this rectangle. Good.

Further, in the above-mentioned embodiment, the case of detecting characteristic X-rays of three kinds of elements has been shown for the sake of simplification of description, but the characteristic X-rays of more elements are not limited to three kinds. May be detected and stored in the storage device.

Further, in the above-mentioned embodiment, the characteristic X
Although the correlation graph is displayed by directly using the line intensity data, the correlation graph may be displayed after the characteristic X-ray intensity data is converted into the concentration value by using the calibration curve method or the like.

[0015]

EFFECTS OF THE INVENTION In the present invention, since a graph that correlatively represents the frequency distribution for each X-ray intensity value of two elements in a region of interest in a mapping image is displayed, the uniformity of the concentration of each element can be displayed. In addition to being able to know, the correlation of the concentrations of the two elements contained in the region can be known, and the knowledge of the region can be further deepened.

[Brief description of drawings]

FIG. 1 is a diagram showing a main part of an apparatus for carrying out the present invention.

FIG. 2 is a system configuration diagram of an apparatus for implementing the present invention.

FIG. 3 is a diagram for explaining an instruction of an arbitrary area in a screen displayed on a color graphic display.

FIG. 4 is a diagram for explaining a display example of a graphic display.

FIG. 5 is a diagram for explaining another embodiment of the present invention.

[Explanation of symbols]

 1 X-ray microanalyzer 2 Sample 3 CPU 4 Storage device 5 Color graphic display 6 Pointing device 7 Keyboard 8 Bus line 9 X-ray intensity value data storage unit 10 Writing / reading control unit 11 Area designation unit 12 Mapping element designation unit 13 Target element designation Part 14 Function designation part 15 Function selection part 17 Correlation graph data creation part 18 Level classification processing part 19 Color classification processing part 20 Display control part EB Electron beam C1, C2, C3 Spectroscopic crystal D1, D2, D3 X-ray detector T1, T2 , T3 X-ray counter

Claims (1)

[Claims] 1. A sample is irradiated with an electron beam, and each element Θ1, Θ2 relating to each pixel (x, y) on a two-dimensional plane of the sample.
, Θn (n ≧ 2) characteristic X-ray intensity value data I1
(X, y), I2 (x, y), ..., In (x, y) are obtained, the obtained data is stored, and an arbitrary element Θi (i is 1, 2) is stored in the stored data. , ..., n) of the characteristic X-ray intensity value data Ii (x, y) is read, and a distribution image of the element Θi is displayed in a color according to the read data value. A region S having an arbitrary size is designated at the position of, and the frequency distribution for each X-ray intensity value of each pixel included in the designated region S for any two elements of the respective elements is correlated. A method for analyzing a sample in an X-ray microanalyzer, characterized in that a graph shown is displayed.