JPH04225152A - Automatic apparatus for x-ray analysis of crystal orientation - 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]

0001

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray crystal orientation analyzer for measuring grain orientation in single crystals and polycrystals.

0002

2. Description of the Related Art Conventionally, crystal orientation has been determined using the Laue camera method, in which a sample crystal is irradiated with continuous X-rays and diffracted X-rays from the sample are photographed. FIG. 4 is a diagram showing an example of an X-ray crystal orientation analysis apparatus using such a Laue camera method. In FIG. 4, reference numeral 21 denotes an X-ray generator, which is fixed to a column 23 provided at one end of the base 22. Reference numeral 24 denotes a cassette holder provided on a rail 25 on the base 22 so as to be slidable along the collimator axis, and a collimator 26 whose rear end is attached to the irradiation side of the X-ray generator 1 and faces toward the center of the sample. A film cassette 27 is attached to the holder 24 so as to receive diffracted X-rays from the sample and photograph Laue spots. Reference numeral 28 denotes a two-axis rotating sample stand that can rotate the sample crystal in the vertical axis Y and horizontal axis A ring 32 is attached to an in-plane rotation guide 31 mounted above and erected on the substrate 29, which rotates using the inner peripheral surface as a guide, and this ring 32 holds a sample crystal on the collimator axis. A sample holder is attached.

Next, a method of using this X-ray crystal orientation analyzer will be explained. First, the crystal of the sample is fixed on the sample stand 28, and the X-ray film cassette 27 is attached to the cassette holder 24. Then, the sample stand 28 is operated so that the sample surface to be measured faces the cassette 27, and the cassette holder 24 is Slide back and forth to adjust the distance between the two. When such preparations are completed, the X-ray generator 21 is energized to generate X-rays, and the X-rays are point-focused by the collimator 26 and irradiated onto the sample crystal. The incident X-ray beam is
Diffraction is performed based on the crystal orientation of the sample, and film cassette 2
It reflects back to 7. After a predetermined exposure time has elapsed, the X-ray generator 21 is turned off, the film cassette 27 is removed from the holder 24, and the film is developed. The rough orientation of the sample surface can be determined from the Laue spots on the photographed film in this manner.

0004

[Problems to be Solved by the Invention] Although the conventional X-ray crystal orientation analyzer is constructed as described above, the analysis of photographs obtained by this equipment is generally done manually.
This work not only requires a lot of labor and time, but also has the problem that the analysis accuracy is ±1 to 2 degrees or more in the peripheral areas of the stereo projection image. The present invention was devised to eliminate the drawbacks of the prior art as described above, and it is possible to shorten the analysis time of X-ray crystal orientation, and
It is an object of the present invention to provide an automatic X-ray crystal orientation analysis device that can achieve analysis accuracy of ±0.2 degrees or less.

[0005]

[Means for Solving the Problems] In order to achieve the above object, the automatic X-ray crystal orientation analyzer of the present invention has an X-ray generator, a sample stage for holding a sample, and rotates around the sample. The X-ray position detector detects diffracted X-rays from the sample.

[0006]

[Operation] The automatic X-ray crystal orientation analyzer of the present invention is constructed as described above, and irradiates the sample held on the sample stage with X-rays from the X-ray generator, and also uses the X-ray position detector to detect the sample. By rotating around the center, the diffraction from the sample
It is possible to accurately detect the position of the Laue spot based on the line and analyze the crystal orientation with high precision.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Examples of the present invention will be described below based on the drawings. FIG. 1 is a diagram showing one embodiment of the present invention, and FIG. 2 is a diagram showing an embodiment of the present invention.
This is a view of the example device shown in the figure, viewed from above. 1 is an X-ray generator using a tungsten filament, 2 is a collimator, and 3 is a position detection type proportional counter tube, and the distance to the sample crystal is adjustable. It has become. 4 is a sample crystal, 5 is a sample stage that can be moved in three dimensions, and 6 is a rotation device that uses a motor with a rotary encoder, gears, etc., and can rotate by about 0.3 to 0.5 degrees per step. It is possible. 7 is a control device, 8 is a data processing device, and 9 is a display device. Moreover, FIG. 3 is a detailed diagram of a position detection type proportional counter tube 3 which is an example of an X-ray position detector, and 10 is a detector container;
11 is a printed circuit board for a cathode, and 12 is a fixed resistor. The printed circuit board 11 for a cathode and the fixed resistor 12 constitute a cathode. By making the pattern of the printed circuit board radial, the angular resolution can be made constant. Furthermore, by changing the pattern shape of this printed circuit board, the required distance between the position detection type proportional counter 3 and the sample can be changed, and by selecting the value of the fixed resistor 12, a signal with a large S/N ratio can be obtained. I can do it. Reference numeral 13 indicates anode wires, and in this example, four anode wires are attached to the base 14. Reference numeral 15 denotes an X-ray entrance window, which is coated with a beryllium film to prevent excess X-rays from entering.

PR gas (90% Ar, 10% CH4) is flowing into the container 10 of the position detection type proportional counter 3, and a high voltage is applied to the anode wire 13. When X-rays enter the counter 3 through the window 15, a local electron avalanche occurs on the anode line 13, and at the same time an induced charge is generated on the cathode. This induced charge is
By detecting it via a preamplifier (not shown) connected to 2, the incident position and intensity of the X-ray can be measured.

Next, a method of using the automatic X-ray crystal orientation analyzer of this embodiment will be explained. After fixing the sample 4 to the sample stage 5 and adjusting the distance between the sample 4 and the position detection type proportional counter tube 3, when the X-ray generator 1 generates X-rays, the X-rays are point-focused by the collimator 2. The sample crystal 4 is irradiated with light, and the sample crystal 4 is diffracted as shown in FIG. Simultaneously with this X-ray irradiation, the rotating device 6 is driven by the control device 7, and the position detection type proportional counter tube 3 is rotated about the sample by a predetermined angle at regular intervals. This rotation range is 4
About 0 degrees is sufficient, but it is convenient if both sides can be rotated up to about 90 degrees.

On the other hand, while the position detection type proportional counter tube 3 is rotating, the X-ray incident angle and count rate data are transmitted from the position detection type proportional counter tube 3 via a preamplifier connected to a resistor 12 and a control device 7. The data is then input to the data processing device 8 together with the rotational position data of the counter tube 3. And data processing device 8
extracts at least three to more than ten pieces of data in descending order of the counting rate, determines the orientation index of the crystal plane from the angular relationship based on the index data in each crystal structure, and displays it on a display device 9 such as a CRT. .

[0011] Then, by driving the sample stage 5 by the control device 7 according to the determined index of the sample crystal plane,
After orienting the sample in a predetermined direction with respect to the X-ray generator 1,
By performing the measurement again, the orientation index of the crystal plane can be determined with high precision. In the above embodiment, a case has been described in which a position detection type proportional counter is used as the X-ray position detector, but a semiconductor type X-ray incident position detector may also be used as the X-ray position detector.

0012

[Effect of the invention] The automatic X-ray crystal orientation analysis device of the present invention has the following features:
With the above configuration, there is no need to manually analyze photographs as in the past, and the analysis can be performed directly by the data processing device, thereby significantly shortening the analysis time. In addition, since the diffracted X-rays from the sample are detected by an X-ray position detector, it is possible to accurately detect the position of the Laue spot due to the diffracted X-rays from the sample and determine the orientation index of the crystal plane with high precision. I can do it.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing an embodiment of an automatic X-ray crystal orientation analysis apparatus of the present invention.

FIG. 2 is a diagram of the automatic X-ray crystal orientation analyzer shown in FIG. 1 viewed from above.

FIG. 3 is a diagram showing details of a position detection type proportional counter, which is an example of an X-ray position detector used in the automatic X-ray crystal orientation analyzer of FIG. 1;

FIG. 4 is a diagram showing an example of an X-ray crystal orientation analysis apparatus using the conventional Laue camera method.

[Explanation of symbols]

1. X-ray generator 2 Collimator 3 Sample crystal 5 Position detection type proportional counter 7 Control device 8 Data processing device

Claims (1)

[Claims] Claim 1: An X-ray generator comprising an X-ray generator, a sample stage that holds a sample, and an X-ray position detector that is rotatable around the sample; An automatic X-ray crystal orientation analyzer characterized in that the X-ray position detector is rotated to detect X-rays diffracted from the sample while being irradiated with the X-rays.