JPS6029896B2 - X-ray analyzer - Google Patents

Description

[Detailed Description of the Invention] The amount of retained austenite in carbon steel or high-speed steel depends on the austenitization temperature, that is, the quenching temperature, cooling conditions, or processing conditions such as straightening during processing. , chromium, nickel and other mineral components.

Therefore, by knowing the type and amount of elements contained therein and the retained austenite at any point on the sample, clues for estimating the treatment history can be obtained. Conventionally, for such observations, it was necessary to use an X-ray diffraction device to determine the amount of retained austenite, and an X-ray crab spectrometer to determine the components of the sample, so two types of equipment were required. Not only that, but observation operations were also complicated. Moreover, it is extremely difficult to observe retained austenite and components at precisely the same point on a sample, so accurate data could not be obtained. The present invention eliminates these drawbacks, makes it possible to simultaneously perform X-ray diffraction and optical analysis on a microscopic portion of a sample, and increases the intensity of the detected X-rays sufficiently to perform accurate measurements. The present invention provides a device for obtaining FIG. 1 is a side view of an embodiment of the present invention, FIG. 2 is a cross-sectional view taken along the line AA in FIG. 1, and FIG. 3 is a cross-sectional view taken along the line B-B in FIG.

In this way, the sample moving tables 2 and 3 are provided on the base 1, and the sample 4 is spread thereon. The movable table 2 moves along a guide groove 5 of the base, and the movable table 3 moves along a guide groove 6 of the movable table 2, and the guide grooves 5 and 6 are orthogonal to each other. The screw punches 7 and 8 are screwed onto the movable bases 2 and 3 respectively, and the screw punches 7 and 8 are driven by electric motors 9 and 10 mounted on the base 1 and the movable base 2, respectively.
are arranged to rotate respectively. Therefore, when the electric motor 9 is rotated, the sample 4 moves in the x direction in FIG. 2, and when the electric motor 10 is rotated, the sample 4 moves in the y direction. A vertical support 11 is provided on the base 1, and an X-ray tube 12 is attached to the upper end thereof.

The proximal end of a collimator 13 is placed opposite to the window of the X-ray tube 12 so that the thin parallel X-rays p passing through the collimator are incident on the sample 4 at right angles. In addition, a screw thread 16 connected to the electric motor 14 on the base 1 is arranged in parallel with the support column 11, and the holding stand 16 of the X-ray detector to which this screw hole is screwed can be freely slid into the guide groove 17 of the support support. It is combined with the Therefore, when the electric motor 14 is rotated, the holding table 16 moves in the z direction in FIG.
18, a slit 19, and filters 20 and 21 are attached. FIG. 4 is a bottom view of the x-ray detectors 17 and 18,
FIG. 5 is a cross-sectional view, and FIG. 6 is a cross-sectional view taken along line CC in FIG.

In this way, the X-ray detectors 17 and 18 are integrally formed by one circular metal airtight container 22,
The container has an annular X-ray entrance window 23 on one bottom surface and coaxial windows 24 and 25 formed inside the annular X-ray entrance window 23.
Core wires 26, 27, and 28 to which high voltage is applied are provided inside these windows, and are supported by insulator supports 30 and bushings 31 for drawing out the terminals of the core wires.
A partition wall 32 is provided between 6 and 27, 28, and a suitable ionized gas is sealed inside the container 22. In other words, core wire 2
6 and the space around it form one proportional counter tube 17, and the core wires 27, 28 and the space around them form another proportional counter tube 18, but in this embodiment, further The proportional counter tube 18 is separated into two parts, a core wire 27 part and a core wire part 28. The two X-ray detectors 17 and 18 arranged coaxially in this way are mounted on the holding table 16 so that their axes coincide with the X-rays passing through the collimator 13, as shown in FIG. Slit 19 on the front of
are arranged, and filters 20 and 21 are arranged in front of windows 24 and 25, respectively. FIG. 7 is a diagram showing the configuration of a device for detecting the output of the X-ray detector as described above, in which the output of the X-ray detector 17 is added to the rate meter 33 and the two core wires of the The outputs obtained from 27 and 28 are applied to rate meters 34 and 35, respectively.

The outputs of the rate meters 34 and 35 are added to a subtracter 36, and the outputs of the rate meter 33 and the subtracter 36 are added to a recorder 37. That is, the detector 17 is for detecting the X-rays d diffracted on the sample surface as shown in Fig. 1, and the detector 18 is for detecting the crab-like X-rays excited by the X-rays p and generated from the sample. , filters 20 and 21 constitute a balanced filter for the crab light X-rays to be detected. Figure 8 shows the absorption curve of this balanced filter, with the X-ray wavelength on the axis and the absorption rate B on the vertical axis.
has been set aside. For example, wavelength input. In order to detect copper crab light X-rays, nickel and cobalt foils are used as the filters 20 and 21, and these curves N,
and Co-like absorption properties. Therefore, when the outputs of the rate meters 34 and 35 are added to the subtracter 36, the outputs due to X-rays with smaller input wavelengths and the outputs due to X-rays with wavelengths larger than input 2 are almost canceled out, and the X-rays near wavelength ^6 rays, namely copper crab-light X-rays, are detected. However, the detection of crab light X-rays by this balanced filter is just one example, and the core wires 27 and 28 are connected to form a single X-ray detector, and the output thereof is applied to a pulse height analyzer. etc. are of course possible. In the above-described apparatus, when a thin parallel X-ray p is incident on the sample 4, the diffraction X-ray is projected so as to form a conical surface with the point of incidence as the apex.

Since the apex angle of this conically diffracted X-ray is determined by the crystal structure of the substance at the point of incidence,
6 is moved in the direction of arrow z, and the position of the holding table 16 is set so that the diffracted X-rays d from the substance with the desired crystal structure to be detected pass through the slit 19 and enter the detector 17. When X-rays p are incident on a sample, crab light x bran f is generated in all directions from the point of incidence, and the wavelength of this crab light X-ray is determined by the elements contained in the sample. Therefore, if the above-mentioned balanced filter is selected so that the crab light X-ray of the desired element is detected, the content of the substance with the desired crystal structure can be determined from the rate meter 33 and the subtractor 36. The corresponding output and the output corresponding to the content of the desired element are respectively sent out and recorded on the recorder 37. In other words, if the moving tables 2 and 3 are driven in this state to move the sample 4 in any direction, the incident point of the X-ray p changes, so for example, the sample is moved only in the x direction in Figure 1. year,
If the moving distance is x and the intensity of the detected X-ray is A, then the 9th
As shown by curves ◯ and F in the figure, changes in the intensity of the aforementioned diffraction X-rays and crab light X-rays are plotted. In the curves D and F, both a specific crystal structure and a specific element are present in a larger amount at position x than in other parts, so it is presumed that the above element contributes to the formation of the substance with the crystal structure. Furthermore, since only a specific crystal structure has increased in the cedar tree, it is presumed that this increase in crystal structure is due to other causes. As described above with respect to the embodiments, the apparatus of the present invention is capable of simultaneously performing elemental analysis and crystal structure analysis in a minute portion of a material.

Therefore, for example, test and research regarding retained austenite can be carried out extremely efficiently, and since diffraction X-rays and crab light X-rays can be detected exactly at the same point, accurate data can be obtained. Furthermore, the total diffraction X is projected onto a conical surface.
Since it is possible to detect X-rays and also detect crab-light X-rays through a wide-area annular window, precise measurements can be made.

[Brief explanation of drawings]

Fig. 1 is a side view of the embodiment of the present invention, and Fig. 2 is A-A in Fig. 1.
A sectional view, Figure 3 is a BB sectional view of Figure 1, Figure 4 is a bottom view of the X-ray detector in Figure 1, Figure 5 is a cross-sectional view, and Figure 6 is the same as Figure 5. 7 is a configuration diagram of a device for observing the output of an X-ray detector, FIG. 8 is a characteristic curve of the balanced filter in FIG. This is an example of a curve. In the figure, 1 is a base, 2, 3... moving table, 4 is a sample, 12 is an X-ray tube, 13 is a collimator, 17 and 18 are X-ray detectors, 19 is a slit, 20, 21... is a filter. It is evening. Two galleys outside the turtle phantom sled turtle sled easy to fly fly zoku crane sogu atsushi galley construction

Claims (1)

[Claims] 1. Means for coaxially arranging two X-ray detectors each having an annularly formed X-ray entrance window and moving the two X-ray detectors in their axial directions; means for projecting thin parallel X-rays onto a sample placed on the axis along the axis; and means for arbitrarily selecting the point of incidence of the X-rays by moving the sample in a plane perpendicular to the axis. and,
It is characterized by comprising means for simultaneously observing the diffracted X-ray intensity of the sample detected by one X-ray detector and the fluorescent X-ray intensity of the sample detected by the other X-ray detector. X-ray analyzer.