JPH0646557B2 - Sample analysis method in X-ray microanalyzer - Google Patents

Description

TECHNICAL FIELD 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 the surface of a sample and analyzing the sample.

[Conventional technology]

In the X-ray microanalyzer, the sample surface is divided into a large number of pixels, and these pixels are sequentially irradiated with an electron beam to generate each element 1, 2, ..., N (n ≧ n) generated from each pixel (x, y).
The characteristic X-ray of 2) is detected. In such a device, these detected elements 1, 2,
.., n (n ≧ 2), the characteristic X-ray intensity value data is once stored in the storage device, and then the characteristic X-ray intensity value data of an arbitrary element i is read out based on the instruction of the operator and is developed on the display device. I am trying to do it.

[Problems to be Solved by the Invention] When a characteristic X-ray intensity value of a certain element i is converted into an n-value and observed as a color mapping image with such a device, the observation is performed at an arbitrary position on the observation screen. If the average weight concentration of the element j other than the element displayed as the color mapping image in the area of arbitrary size can be known,
It is extremely useful for deepening the knowledge about this part.

The present invention has been made in view of such a point, and an object thereof is in a region of interest in a color mapping image,
An object of the present invention is to provide a sample analysis method in an X-ray microanalyzer capable of obtaining and displaying weight concentration values of elements other than the elements displayed as a mapping image.

[Means for Solving the Problems] A sample analysis method in an X-ray microanalyzer of the present invention which achieves this object is to irradiate a sample with an electron beam to form each pixel (x, y) on a two-dimensional plane of the sample. Each element related to 1,
2, ..., N (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 i (i is 1, 2) is stored in the stored data. , N, or characteristic X-ray intensity value data Ii (x, y) is read, a distribution image of the element i is displayed in a color according to the read data value, and the distribution image is arbitrarily selected. Area S of arbitrary size at position
, The element j other than the element i (j is 1, 2, ...,
area S designated for any of n other than i)
To obtain the average characteristic X-ray intensity value M (j) s of each pixel, and convert the obtained average characteristic X-ray intensity value M (j) s into the weight concentration value W (i) s of the element j. It is characterized in that the obtained weight concentration value is displayed.

[Examples] Hereinafter, the present invention will be described in detail with reference to the drawings.

FIG. 1 is a diagram showing a main part of an apparatus for carrying out the present invention, and 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 micro analyzer (hereinafter X
(Abbreviated as MA), 2 is a sample, EB is an electron beam, C
1, C2, C3 are dispersive crystals, D1, D2, D3 are X-ray detectors, T1, T2, 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,
Reference numeral 7 is a keyboard, and 8 is a bus line. The dispersive crystals C1, C2 and C3 are set so that the characteristic X-rays of the elements 1, 2 and 3 can be selected. The pointing device 6 is for pointing an area having an arbitrary position, size and shape on the screen of the color graphic display 5 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 an average intensity value calculation unit, 13 is a concentration value conversion unit, and 14 is a display control unit. , 15 is a level division processing unit, 16 is a color division processing unit, 17 is a mapping element designation unit, and 18 is an average concentration value calculation element designation 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 includes elements 1, 2, 3
The one-screen image storage areas A1, A2, A3 are provided corresponding to. 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 configuration, the horizontal movement mechanism of the sample 2 is operated to move the sample 2 two-dimensionally in a state where the sample is irradiated with the electron beam EB. As a result, each pixel (x, y) of the sample 2 is sequentially irradiated with the electron beam EB. Among the characteristic X-rays generated from each pixel (x, y) of the sample 2 by the irradiation of the electron beam EB, the characteristic X-rays of the elements 1, 2 and 3 are X-rays via the dispersive crystals C1, C2 and C3, respectively. Line detector D
1, D2, D3 are detected. Therefore, from the X-ray counters T1, T2, T3, the count value signals of the characteristic X-rays of the elements 1, 2, 3 in each pixel (x, y) are transferred to the bus line 8.
Is sent to the storage device 4 via. The characteristic X-ray intensity value data relating to the element 1 of each pixel (x, y) sent to the storage device 4 is stored in the image storage area A of the X-ray intensity value data storage unit 9.
1 is stored in the storage area corresponding to each pixel (x, y). Similarly, the characteristic X-ray intensity value data of the element 2 is stored in the image storage area A2, and the characteristic X-ray intensity value data of the element 3 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 1, the mapping element designating unit 17 sends a signal instructing the writing / reading control unit 10 to select the element 1, 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 division processing unit 15. The level division processing unit 15 quantizes the transmitted X-ray intensity value data by comparing it with a plurality of reference levels. The number of reference levels can be arbitrarily selected, and the value of the reference level can also be arbitrarily set. In the case of this embodiment, assuming that four reference levels are set in advance, the level division processing unit 15 compares the received X-ray intensity value data with these reference levels to classify them into the inside and outside of each reference level. Then, it is binarized and sent to the color classification processing unit 16. In the color division processing unit 16, the level division processing unit 1
The hue corresponding to the hierarchical value is assigned to the five-valued data sent from No. 5, and a signal for displaying each with the assigned hue is sent to the display control unit 14. As a result, a color mapping image showing the characteristic X-ray intensity distribution of the element 1 is displayed on the color graphic display 5, as shown in FIG. Similarly, when the operator gives an instruction to display the characteristic X-ray intensity distribution image of the element 2, an image as shown in FIG. 3B is displayed on the display 5 based on the data stored in A2 of the image storage area. Then, when the operator gives an instruction to display the characteristic X-ray intensity distribution of the element 3, an image as shown in FIG. 3 (c) is displayed on the display 5. Of these X-ray intensity distribution images, for example, while observing the characteristic X-ray intensity distribution image of element 3, an interesting region was found,
When trying to know the average abundance concentration value of an arbitrary element in this region, the operator operates the pointing device 6 to move the region S to the third region under the control of the region designating unit 11.
It is surrounded by a bright line F as shown in FIG. After the designation of the area is completed in this way, when the display of the average weight concentration of, for example, the element 2 in the designated area is instructed by the keyboard 7, the average concentration calculation element designating section 18 causes the image storage area A to be displayed.
A signal for instructing selection of data No. 2 is sent to the write / read controller 10. At this time, a signal representing the designated area is sent from the area designating section 11 to the writing / reading control section reading 10. Therefore, the writing / reading control unit 10 reads only the X-ray intensity value data of each pixel (x, y) included in the area S from the data stored in the image storage area A2 and calculates the average intensity value calculation unit. Send to 12. The average intensity value calculation unit 12 calculates the average intensity value M (3) s of the element 2 relating to the designated area S given by the following formula from the sent data.

Thus, the average intensity value M of the element 2 with respect to the region S
When (2) s is obtained, the data representing M (2) s is sent to the density value conversion unit 13. The conversion unit 13 uses the calibration curve method to convert the sent data representing M (2) s into element 2
Of the density value data W (2) s. The density value data W (2) s from the conversion unit 13 is sent to the display control unit 14, and the display control unit 14 displays the density value data W (2) s in characters on the lower part of the display screen of the display 5 or the like. , Print to a printer, etc.

Therefore, next time the operator wants to know the average concentration value of the region S related to the element 1, if the user points to the element 1 by the keyboard 7, the average concentration value calculation element designating section 18 causes the element 1 to be calculated.
Since the signal for instructing is newly sent to the writing / reading control unit 10, the writing / reading control unit reads only the characteristic X-ray intensity value data of the pixels included in the area S of the image storage area A1 and calculates the average intensity value calculation unit 12 Send to. Therefore, in this case, the average concentration value of the element 1 existing in the region S can be displayed on the display 5.

As described above, according to the apparatus described above, the characteristic X of an arbitrary element is
When the region of interest is found by observing the line intensity distribution image and observing this image, pointing this region with the pointing device, the characteristic X-ray intensity value data of the element for which the average concentration value is to be calculated Only the data in the designated area is read out and the average intensity value is obtained, and this average intensity value is converted into the weight concentration value. The average density value in the selected area can be obtained and displayed.

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 is used to indicate an area having not only an arbitrary position and size but also an arbitrary shape. However, K1 and K2 in FIG. , K3, a rectangle whose size is changed stepwise and its position is arbitrarily changed may be displayed, and the region may be designated by instructing the position and size of this rectangle.

Further, in the above-described embodiment, the case where characteristic X-rays of three kinds of elements are detected has been shown for simplification of description, but the number of characteristic X-rays of more elements is not limited to three kinds. It may be stored in the storage device.

Further, in the above-described embodiment, the calibration curve method was used to convert the data from the average intensity calculation unit into the concentration value, but the conversion may be performed using the ZAF method or the B & A method of the quantitative analysis method. May be.

Further, the present invention can be similarly applied to an apparatus for acquiring characteristic X-ray intensity value data of each element by using a non-dispersive X-ray analyzer.

Furthermore, in the above-described embodiment, the element for which the average concentration value is calculated is designated, and only the average concentration value of the designated element is displayed, but the one-screen image storage areas A1, A2,
The average concentration value in the area S may be calculated and displayed for all the elements stored in A3 ....

EFFECTS OF THE INVENTION In the present invention, since the weight concentration values of the elements other than the elements displayed as the mapping image in the region of interest in the mapping image are displayed, the elements other than the elements displayed as the mapping image are displayed. It is possible to know the weight concentration value of, and it is possible to further deepen the knowledge in that area.

Further, in the present invention, for example, when the spatial variation of the distribution of the element j on the display screen is small, the color of the distribution image is almost the same over the entire display screen, so that the region of interest can be designated. Element j in the region of interest
It is possible to solve the problem that it is not possible to know the weight concentration value of. This is because a color distribution image of the element i having a large spatial change in the element distribution is displayed on the display screen, the image is observed, an area of interest is indicated, and the weight concentration value of the element j in the area is displayed. By doing so, the weight concentration value of the element j in the region of interest can be known.

[Brief description of drawings]

FIG. 1 is a view showing a main part of an apparatus for carrying out the present invention, FIG. 2 is a drawing for showing a system configuration of the apparatus for carrying out the present invention, and FIG. 3 is a color graphic display. FIG. 4 is a diagram for explaining an instruction of an arbitrary area in the displayed screen, and FIG. 4 is a diagram for showing another embodiment of the present invention. 1: X-ray microanalyzer 2: sample, EB: electron beam C1, C2, C3: dispersive crystal D1, D2, D3: X-ray detector T1, T2, T3: X-ray counter 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: Average intensity value calculation unit 13: To density value Conversion unit 14: Display control unit, 15: Level division processing unit 16: Color division processing unit 17: Mapping element designation unit 18: Average concentration value calculation element designation unit A1, A2, A3: 1 screen image storage area

Claims (1)

[Claims] 1. A sample is irradiated with an electron beam, and each element 1, 2, ..., N relating to each pixel (x, y) on a two-dimensional plane of the sample.
(N ≧ 2) intensity 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 i is stored in the stored data.
(I is one of 1, 2, ..., N) characteristic X-ray intensity value data Ii (x, y) is read, and a distribution image of the element i is displayed in a color according to the read data value. , An area S having an arbitrary size at an arbitrary position of the distribution image, and the area designated with respect to an element j other than the element i (j is any one of i of 1, 2, ..., N) The average characteristic X-ray intensity value M (j) s of each pixel included in S is obtained, and the obtained average characteristic X-ray intensity value M (j) s is converted into the weight concentration value W (i) s of the element j. And displaying the obtained weight concentration value, the sample analysis method in an X-ray microanalyzer.