JPS62167451A - X-ray spectrometer - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] B Industrial application field The present invention relates to an X-ray spectrometer.

Conventional techniques X-ray spectroscopy includes wavelength dispersive methods using spectroscopic crystals and energy dispersive methods typified by semiconductor detectors.

In the wavelength dispersion method, 11λ=2ds inθ<n: M number,
λ1 spectral wavelength, d・spectral crystal lattice spacing, θ・incident angle)
By setting θ that satisfies the flag conditions shown in , characteristic X-rays of a specific wavelength generated from an unknown sample are detected. However, as can be seen from this conditional expression, this condition only applies to diffraction orders n=1.2, 3. It includes...
Since higher-order X-rays with n other than 1 are also detected at the same time, it is necessary to measure whether the detected X-rays are influenced by the above-mentioned higher-order rays. FIG. 3 shows a relationship curve between the wavelength of X-rays emitted from a sample of multiple components (A and B components) measured using a wavelength dispersion method and the detected intensity. As shown in the figure,
When the position where the primary line of the characteristic X-ray of the A component appears and the position where the secondary line of the characteristic 2
The tail part of the peak of the next line affects the X-ray detection intensity,
The detection intensity 11 of only the A component is unknown, and in order to obtain the detection intensity 11 of only the A component, it is necessary to exclude the influence of the secondary line 2 by some method. With the Ikegata energy dispersive method, this problem does not occur because the analysis takes advantage of the fact that the peak value of the X-ray detection pulse differs depending on the wavelength. However, the wavelength dispersion method has better wavelength resolution and stability than the Tunnel-E dispersion method, so it is widely used. In order to perform measurements using the wavelength dispersion method, it is necessary to remove the effects of the above-mentioned higher order lines. Measurement is performed using a wavelength scan to determine whether there is a basic line of the element that shows a higher-order diffraction line, and the influence of the above-mentioned higher-order line is measured, and the basic measured value is corrected to obtain the measured value of the measured component. However, since it performs wavelength scanning, it lacks real-time performance, takes time to measure, and especially when using a fixed wavelength spectrometer, it cannot be corrected. 6 C. The invention solves the problem. Problems to be Solved by the Invention The present invention solves the problem that, in wavelength dispersive X-ray spectroscopy, conventional correction for the influence of high-order rays lacks real-time performance and is time-consuming for measurement, especially when using a spectrometer with a fixed wavelength. 2. Means for solving the problem In an X-ray spectrometer consisting of a wavelength dispersive spectrometer section and a detector section, the X-ray detector is replaced with an energy responsive counting system. An energy analyzer for analyzing the detection output of the detector into a designated energy band, and a means for counting the output of the energy analyzer were provided.

E. Effect According to the present invention, it has become possible to detect correction values for higher-order lines without performing wavelength scanning.

Embodiment FIG. 1 shows an embodiment of the present invention. In Figure 1, S
is the sample, 1 is the spectroscopic crystal, 2 is the proportional counting type X-ray detector, 3
is an amplifier, 4 is a multi-channel pulse peak value analyzer, which is a device that sorts the peak value of the output pulse of the X-ray detector 2 into multiple stages and counts the number of pulses at each stage; 5 is a C
The PU records a histogram of the peak values of each stage measured by the analyzer 4, and shows the relationship curve between energy and intensity of the separated X-rays on the display section 6, or the X-ray that is to be detected in the histogram. The height of the peak corresponding to the line wavelength is displayed as the intensity of the X-ray to be detected.

The measurement method will be explained. The spectrometer is set to the characteristic X-ray wavelength λ1 of the element to be measured, and the X-rays emitted from the sample S are separated by the spectroscopic crystal 1 by electron beam irradiation, and the separated X-rays are transferred to the X-ray detector. Detect with 2. The detection signal is amplified by an amplifier 3 and inputted to a multichannel pulse peak value analyzer 4. Analyzer 11
counts the X-ray detection pulses at each wave height level, and calculates the second
Form a histogram of pulse height values as shown in the figure. From the relationship between the pulse height value and the X-ray energy, it is clear that II' is the peak of the characteristic X-ray of the element we are trying to detect, and I2 is the peak of the second-order diffraction line of the characteristic X-ray of another element with wavelength λ2. It is. The CPU 5 takes in the data of the histogram formed by the peak value analyzer 4, performs the above-mentioned judgment, and calculates the T value corresponding to the X-ray of wavelength λ1.
The total count value for the 1'' peak is calculated and used as characteristic X-ray data of the element to be detected.

In this case, the histogram in Figure 2 is the distribution of pulse height values for X-rays that have already been wavelength-selected by a spectrometer, so the total area of the peak II' is formed only by the detected pulse of X-rays with wavelength λ1. Therefore, the surface quality of this peak provides the detected intensity of the element to be measured.

Effects According to the present invention, the primary line and the secondary line are distinguished without wavelength scanning, making it possible to perform quantitative measurements, improving analysis accuracy and providing measurement results in real time. The measurement efficiency has improved.

[Brief explanation of drawings]

121 is a block diagram of an embodiment of the present invention, FIG. 2 is a histogram of pulse peak values measured by a multi-channel pulse peak value analyzer, and FIG. FIG. 2 is a diagram showing a relationship curve between characteristic X-ray wavelength and intensity obtained by the method.

Claims (1)

[Claims] In an X-ray spectrometer consisting of a wavelength-dispersive spectrometer and a detector, the X-ray detector is an energy-responsive counting element, and an energy analyzer that analyzes the detection output of the detector into a specified energy band; An X-ray spectrometer characterized by comprising means for counting the output of the analyzer.