JPS5977347A - X-ray diffraction apparatus - Google Patents

Abstract

PURPOSE:To carry out an X-ray diffraction measurement of a minute sample to be evaluated at high speed, by providing a two-dimensional moving mechanism which moves a sample mounting member on a plane including the sample surface such that an X-ray incident point is located at a position in a desired evaluation region. CONSTITUTION:Two-dimensional data detected by a two-dimensional optical detector 12 are passed through an A/D converter 17 and stored in a memory circuit 19. An arithmetic controller 20 detects deviations DELTAx, DELTAy of the position of the intersection of horizontal and vertical patterns, as an X-ray incident point, from the position of a minute region 23 to be evaluated, the positions having been stored in the circuit 19. The detected quantities DELTAx, DELTAy are respectively delivered from the controller 20 to a pulse motor 21 for driving a stage 10 in the X direction and a pulse motor 22 for driving the stage 10 in the Y direction in the form of pulses the numbers of which correspond to the movements of the stage 10 in the X and Y directions. Accordingly, it is possible to effect an X-ray diffraction measurement of a minute sample to be evaluated at high speed, and the diffraction data have high reliability.

Description

[Detailed Description of the Invention] Is the present invention applicable to reflected X-rays from a minute area? The present invention relates to an X-ray diffraction device that can perform reliable detection.

Conventional X-ray diffraction devices include an X-ray generator, a goniometer,
It consists of an X-ray detection device, but is it reflected X-rays from a minute area of the sample to be evaluated or from a minute evaluation sample? You may try to detect it. In this case, for the former, assuming that the uniform area of the sample to be evaluated is wide, the incident By the method, is the cross section of a small sample inserted into an incident X-ray flux?
After taking a complete bath, the reflected X-rays were detected.

In the current material processing industry and electronic materials industry, it is desirable to evaluate large-sized materials using iX-ray diffraction, especially for large-diameter substrate materials and thin films deposited on other large-diameter substrates. It is desired to evaluate the completeness of crystallinity, degree of heterogeneity, etc.

This irresponsibility? To evaluate, the incident Xfj! It is necessary to narrow down the beam to a very small size, have high reliability of reflected X-rays from a minute region to be evaluated, and perform evaluation without losing one correspondence.

As mentioned above, it is impossible to evaluate minute areas of large-sized materials using the method of simply narrowing down the incident X-rays with a slit or the like, or the complete bath method where the sample to be evaluated is destructively micro-processed and evaluated in a steady state. .

The purpose of the present invention is to improve the above-mentioned drawbacks and to enable the detection of the incident point r of X-rays in minute areas of the sample to be evaluated. An X-ray diffraction device that can be positioned reliably at the point of incidence of X-rays?
It is about providing.

The X-ray diffraction apparatus of the present invention includes a light source that forms a light beam output sound, an optical system that guides the light beam from this light source onto the incident X-ray axis of a sample to be irradiated with X-rays, and a light beam that irradiates the light beam from this optical system. a two-dimensional optical position detecting means for detecting a desired evaluation area on the sample from the YS (scattered from the sample surface), and a position detected by the optical position detecting means is stored as an X-ray incident point. a two-dimensional movement mechanism for moving the sample mounting member r on a surface including the sample surface so that the X-ray incident point stored in the memory means is located at the desired evaluation area; and? It consists of:

The following 5 inventions? drawing? This will be explained in detail using

FIG. 1 is a schematic diagram of an embodiment of the present invention. In the figure.

■Is it an X-ray? In this embodiment, six rotating anticathode type X-ray generators each having an output of 12 KW are used. 2, 7, and 8 are slits for narrowing down the incident XIW'. The optical system (3,4°5.6) is a light source #? Eggplant light source box 3. Aperture lens system 4. It is composed of an optical fiber 5 and a laser generator 6. In this example, a He-Ne laser (6) with an output of 5ITIW is used.
The laser beam r is guided onto the optical axis of the X-ray by an optical fiber 5. Due to the straightness of the X-rays and laser, they pass through the slit 2°7.8, and the incident point of the X-rays and the slit 7
．． It is clear that the incident point of the laser passing through 8 is the same. A laser beam narrowed by a slit 8 is incident on a minute region of a sample 11 placed on a stage 10 on a goniometer 9 . Reflection X from this sample 11
i is detected by the X-ray detector 16. Note that the slit 15 is a slit for preventing scattered X-rays.

In the present invention, since the incident point of the laser beam that has passed through Surin) 7.1 is the same as the incident point of the X-ray, the scattered light of the laser scattered from the sample surface is detected by the light detection device 12, and the Displayed on monitor 13. In this embodiment, a black and white video camera 11 is used as the photodetector.
j014 is an automatic position correction device.

FIG. 2 shows the two-dimensional photodetector and storage device shown in FIG. 1.

and automatic position correction device? FIG.

The two-dimensional information detected by the two-dimensional photodetector 12 is stored in the storage circuit 19 through 17 AD converters. This stored two-dimensional information is displayed on the two-dimensional display device 13 as an image. In this embodiment, a black and white video monitor television r is used as the two-dimensional display device 13. On this two-dimensional display device 13, horizontal and vertical patterns generated by the horizontal and vertical pattern generation circuit 18 are displayed so as to surround the X-ray incident point 2.

3(a) to 3(C) are schematic diagrams of two-dimensional information displayed as images on the two-dimensional display device 13 of FIG. 2. FIG. FIG. 3(a) shows the first ratio minute evaluation area 23 detected by the two-dimensional photodetector 12, and FIG. 3(b) shows the incident point of the X-rays detected and the distance between the incident point and the sound. Horizontal and vertical patterns displayed? It shows. In the steady state shown in FIG. 3(b), the deviation ΔX between the position of the t-small evaluation area 23 stored in the storage circuit 19 and the center of the horizontal and vertical patterns which are the incident points of X-rays.

ΔYk is detected by the arithmetic and control device 20, and the detected quantities, ΔX, and Δy are the pulses that drive the stage IO in the X direction 21. And drive in Y direction? The arithmetic and control unit 20 calculates the number of Hals corresponding to the amount of movement to the Hals motor 22.
Sent from. In this example, the l pulse is 2 μm of the movement amount.
It corresponds to

FIG. 3(C) is a diagram showing that the stage 10 has been moved by the automatic position correction device and the evaluation area 23 has been positioned in the horizontal and vertical patterns. Note that the image on the two-dimensional display device 13 used is divided into 512×512, and
9, and in this embodiment, the two-dimensional photodetector 1
2, the detectable area is 3 x 3 mm2. 5 X
5 mm2. It is possible to change the cutting angle in three steps: and 1, OX 10 mm2.

Therefore, the 4 resolutions are 6 x 6 μm, IQ x 10
μm, 20×20 μm2. Therefore, the number of pulses sent to the pulse motors 21 and 22 of the stage IO is 3 pulses, 5 pulses, and IO pulses, each of which is sent as 1 single f, corresponding to the above-mentioned three-stage detection area, resulting in high-speed operation. is possible. Also, the Y direction of stage io is the incident
It is perpendicular to the plane formed by the line and the reflection Xi. This stage 10 is placed on a 4-axis goniometer and can measure samples up to 75 mmφ in diameter.

Next, using the X-ray diffraction apparatus of this example, Cukα (e, length is 1.5418X) was used as the o and xi sources. 50×50μm2.1ooXloo11r on a quartz glass substrate using
An island-shaped silicon thin film formed with a dimension of n28 degrees (film thickness 0
．． When we measured the (400) reflection of 6 μm), we found that the automatic position correction time (Fig.
The transition time 9 to the state is performed within 2 seconds.

A great way to obtain highly reliable diffraction data.

By the way, is it a micro sample? When making measurements, the slit 8 used should be as close to the size of the minute sample as possible to reduce unnecessary scattering and obtain data with a high S/N ratio.

Note that the present invention is not limited to this embodiment, and other lasers and other high-intensity visible light sources may be used as the light source device, and a CCD (Charg
eCoupled 1) evi'ce) etc., the digital signal r may be directly transferred to a storage circuit and stored in advance.

As described above, the present invention provides a light source device that can guide the original beam onto the optical axis of X-rays, and a photodetection point equivalent to the incident point of X-rays. Two-dimensional light detection device for detection.

The X-ray diffractometer is equipped with an automatic position correction device that matches the position of a minute sample with the incident point of X-rays.

According to the present invention, the X
It is possible to perform linear diffraction measurements on gold, and the obtained diffraction data is highly reliable, making it an effective measurement method for testing and evaluating a single material in fields such as the material processing industry and electronic material industry. .

[Brief explanation of the drawing]

Fig. 1 is a schematic diagram of an embodiment of the present invention, Fig. 2 is a block diagram explaining a part of Fig. 1, and Figs. It is a schematic diagram. In the figure ■...X-ray generator, 2,7.8.15...
... Surin), 3. 4. 5. 6...
Light source device, 9...Goniometer, lO...
...Stage, 11...Sample, I2...
・Video camera, 13...Monitor TV, 14
... Automatic position correction device, 16 ... X-ray detector, 17 ... AI) converter, 18 ...
. . . horizontal and vertical pattern generation circuits, 19 . . . storage circuit, 20 . . . arithmetic control unit fu, 21.
22...Pulse motor, 23...Minute evaluation area. Figure Z Figure 1α 256- Figure 3

Claims (1)

[Scope of Claims] A light source for forming a light beam output, an optical system that guides the original beam from this light source onto the incident X-ray axis of a sample to be irradiated with iX-rays, and a Is the position of the desired evaluation area on the sample based on the scattered light from the sample surface?
A two-dimensional optical position detection means for detecting, and a storage means for storing the position detected by the optical position detection means as an X-ray incident point. a two-dimensional movement mechanism that moves the sample mounting member on a surface including the sample surface so that the X-ray incident point stored in the storage means is located at the desired evaluation area;
Line diffraction device.