JPS62106352A - Scanning type x-ray microscope - Google Patents

Abstract

PURPOSE:To make it possible to observe the various X-ray images of a metal or ceramics, by irradiating the minute part of a specimen with X-ray fine flux and scattering, diffracting and transmitting the irradiated fine flux to measure secondary X-ray intensities which are, in turn, displayed in synchronous relation to the movement of a measuring area. CONSTITUTION:All of X-ray scattered, diffracted or generated from a minute area are attenuated in the intensities thereof along with their distances by the diffusion thereof. In order to prevent this phenomenon, a light receiving side X-ray conduit of a long rotary parabolic surface type having an extremely small focus is used. As an X-ray detector 13, a solid detector having the resolving power of X-ray energy, for example, SSD is used in order to observe various X-ray images such as a scattered X-ray image, a diffracted X-ray image, a secondary X-ray image and a transmitted X-ray image etc. A computer 2 performs the storing of the position and measured value of each measuring point and the operational control of the XZ surface of a specimen and forms an image on the basis of the memory thereof to display the same on a cathode ray tube or an XY plotter or to display the same as a numerical value matrix.

Description

[Detailed description of the invention] Industrial applications The present invention is a scanning type X-ray! Regarding ffi.

Conventional technology Conventionally, there is no suitable lens for bending X-rays.

Therefore, it does not exist in X-rays @ mirrors, which have the same principle as optical microscopes. In order to observe internal defects in highly perfect crystals,
Although the method of ray topodaraf plays the role of a microscope, it has extremely low killing potential.

In addition, X-rays generated from a point-shaped X-ray generator are received by a thin plate-shaped sample, and a magnified possession image (shadow picture) is taken on the film behind it, or a thin biological specimen is placed on the film. After attaching the sample and exposing it to X-rays, removing the sample and developing it,
A radiographic method for observation using an optical microscope is also known. However, in all of these methods, the shape of the sample that can be observed is extremely limited and is not general.

Purpose of the Invention The present invention was made to solve the problems of conventional X-ray microscopes. The purpose of the present invention is to provide a scanning type X-ray microscope capable of observing and inspecting.

Structure of the Invention The scanning X-ray microscope of the present invention uses an X-ray conduit to inject a narrow bundle of high-intensity X-rays into a microscopic region of a sample, and then collects scattered, transmitted, and secondary X-rays generated from the microscopic region. as well as to measure and memorize their values and sample position parameters;
Sequentially move the sample to move the minute area to be measured, measure in the same way, and accumulate all these measured values and sample position parameters 771 > to create a scattered X-ray image! The present invention is characterized in that it is configured to form a diffraction X-ray image, a transmission X-ray image, a fluorescence jki-ray image, or a tomographic image thereof.

--''-'' Note that if a sample position is selected where the measurement point, that is, the intersection of the direction of the incident X-ray and the direction of the X-ray detector is inside the surface of the sample, a scanning X-ray tomographic microscope is obtained.

Part of the principle of the invention corresponds to a scanning electron microscope. In the history of the development of electron microscopes, transmission type and scanning type have developed in parallel. The former is an image magnification method similar to an optical microscope that uses an electron lens that takes advantage of the fact that electron beams are bent in a magnetic field.

On the other hand, the latter makes the electron beam as narrow as possible, and various interactions that occur in the sample (e.g., secondary electrons, fluorescent X-rays, etc.)
The intensity of backscattered electrons, etc.) is measured and displayed on a cathode ray tube as an image in synchronization with the movement of the electron beam. Therefore, the resolution of the former image is determined by the aberration of the electron lens, and the latter is determined by the thickness of the electron beam.

In the scanning X-ray microscope of the present invention, an X-ray conduit is used to create a fine bundle of X-rays, which is irradiated onto a minute part of the sample, and the scattered 9-diffraction and transmitted secondary X-ray intensity are measured. Display their intensity in synchronization with movement to create a magnified image. Therefore, in Oki, which synchronizes the measurement using a thin beam bundle with the movement of the measurement unit, it is the same as the image magnification mechanism of a scanning electron microscope, and the resolution limit is determined by the thickness of the thin X-ray beam. The same is true in terms of what can be done.

However, in the case of the present invention, the scanning mechanism moves the sample minutely, whereas in the case of a scanning electron microscope, a flux of incident electron beams is photographed. The present invention applies the outline of the imaging and image magnification mechanism used in scanning electron microscopes to X-rays, and also realizes a narrow beam of X-rays using an X-ray conduit that makes this application possible. be.

An example of an embodiment of the scanning X-ray microscope of the present invention will be described with reference to the drawings.

FIG. 1 is a plan view including a partially sectional view, and FIG. 2 is a side view including a partially sectional view. In the figure, 1 is a pulse generator and high voltage generator for generating pulsed or continuous X-rays, 2, 2 is a computer for measurement, sample movement 9, image processing, 3 is sample movement and detector position control 4 is a pulse height analyzer for a solid-state detector, 5 is a pulsed or continuous micro-focus high-intensity X-ray generator, 6 is an entrance side X-ray conduit attitude controller, 7 is an entrance side ray conduit, 8 is the receiving side X-ray conduit, 9 is the sample X direction (horizontal, perpendicular to the direction of the X-ray) minute movement mechanism, 10 is the sample rotation mechanism in the horizontal plane, 11 is the sample 2 direction (height) minute movement mechanism, 12 is a surface plate, 13 is an X-ray detector (solid state detector/5SD14 is a preamplifier for the X-ray detector, 15 is a light-receiving side X'M conduit attitude control mechanism, 16 is an X-ray detector horizontal plane rotation mechanism, 17 is the sample tilt control mechanism (parallel to the X-ray direction) -: ,
-18 represents the same (perpendicular to the direction of the X-ray).

The microfocus X#J generator 5 has a metal anticathode with a
This device is similar to a normal X-ray generator that collides with electron beams accelerated to 0~300 kV.

In order to obtain finely focused, high-intensity X-rays, the electron beam is focused onto the anticathode using an electronic coil 18, for example, as shown in the figure.

It is even more efficient if it is of a type that can generate pulsed X-rays by receiving a pulsed power supply from the pulse generator l. However, the generation of pulsed X-rays is synchronized with the movement of the sample position, the movement period is a rest period, and X-rays are generated only during measurement.

A computer 2 for synchronized Fi control of pulsed X-ray generation and sample movement is used.

The incident-side X-ray conduit 7 is used to efficiently guide the minute, high-intensity X-rays generated to a single point on the sample (the center of rotation of the sample and the measuring device). In the figure, it is shown as a rotating elliptical X-ray conduit. Instead of this, a long conical X-ray guide W1 cylindrical X-ray guide,
It may be a parabolic X-ray conduit or a hollow tube similar to this.

-Two! Examples of X-ray conduits include:
Ru゛.

1) A hollow tube whose inner wall shape is a shape obtained by cutting both ends of a long spheroid whose focal point is the point where X-rays are generated by electron beam irradiation and the two fixed measurement points; 2) A long cone. 3) A hollow tube whose inner wall surface has a shape in which both ends of the body are cut off or a cylindrical shape; 3) A hollow tube whose inner wall surface has a shape in which the tip of a long paraboloid of revolution with a small focus value is cut off; , the X-rays emitted from the X-ray generation point satisfy the critical angle for total X-ray reflection at the incident end of the hollow tube, and the inner wall surface of the hollow tube is smooth enough to cause total X-ray reflection.

The orientation of the incident side X-ray conduit 7 is adjusted using the incident side X@conduit attitude control device 6.

The centers of rotation of the sample horizontal plane rotation mechanism 10 and the X-ray detector horizontal plane rotation mechanism 16 are measurement points, and the position to be measured on or in the sample is minutely moved in the X direction of the sample around this rotation center. The mechanism 9, the I-sample two-direction fine movement mechanism 11, and the sample tilt control mechanism 17 and 18 are used to match the sample. In order to measure the X-rays generated or transmitted from the measurement point at any angle depending on the purpose, an X-ray detector horizontal rotation mechanism 16 is used.

Figure 1 shows the arrangement for measuring second-order scattered diffraction or secondary X-rays, and the detector is approximately 12
It is at position 00. Figure 2 is transparent x&! The detector is at 0° in the arrangement for measuring the quantity.

The intensity of the X-rays that are scattered or generated from a minute region is attenuated with distance due to their divergence.

In order to prevent this, the present apparatus uses an X-ray conduit 8 on the light receiving side. In FIGS. 1 and 2, X1lj! is a long paraboloid of revolution with an extremely small focal point. Shown as a conduit.

Alternatively, it may be of a rotating oblong shape, an oblong female shape, or a cylindrical shape.

The X-ray detector 13 can detect various XIs such as a scattered X-ray image, a diffraction X-ray image, a secondary X-ray (fluorescent X-ray) image, or a transmitted
In order to observe the s-image depending on the purpose, a solid-state detector (for example, SSD) with X-ray energy resolution is used. However, a scintillation counter can be used for detecting defects in metals or sintered ceramics that do not require high accuracy.

The measured value at one point on the sample and the position of the measurement point are stored in the computer, and the sample position is moved to the sample X direction fine movement mechanism 9.
Then, the sample is moved and measured using the two-direction sample movement mechanism 11, and this operation is successively repeated to measure each point in the entire area within XzrfJ.

The computer 2 stores the position and measured value of each measurement point,
The movement of the sample in the X2 plane is controlled, and an image is constructed based on the memory and displayed on a cathode ray tube, an XY plotter, or as a numerical matrix.

Effects of the Invention According to the scanning X-ray microscope of the present invention, the scattering of X-rays from metals and ceramics, which was impossible with conventional X-ray microscopes9, has been achieved.
Diffraction/absorption! Excellent effectiveness and redness can be achieved by allowing images created by secondary X-ray emission to be observed and inspected.

[Brief explanation of drawings]

The drawings are views showing an embodiment of the scanning type X#i1 microscope of the present invention, with FIG. 1 being a plan view and FIG. 2 being a side view. 1: Pulse generator and high voltage generator, 2: Computer, 3: Pulse motor controller for position control, 4: Wave height analyzer for solid state detector, 5: Microfocus high intensity X-ray generator, 6: Incident side X-ray conduit attitude controller, 7 two-person emission side X-ray conduit, 8: light-receiving side X-ray conduit, 9: sample minute movement mechanism, 10; sample horizontal plane rotation mechanism, 11: sample minute movement mechanism, 12: surface plate , 13: X-ray detector, 14: Preamplifier for X-ray detector, 15: X-ray conduit attitude control mechanism, 16: X-ray detector horizontal plane rotation mechanism, 17: Sample tilt control mechanism (parallel to the direction of X-rays) , 18:
Same as above (perpendicular to the direction of the X-rays). Patent applicant Goto, director of the Institute for Inorganic Materials, Science and Technology Agency
Excellent

Claims (1)

[Claims] 1) A fine beam of high-intensity X-rays is incident on a micro region of a sample using an X-ray conduit, and scattering, diffraction, transmission,
The secondary X-rays are measured, their values and sample position parameters are memorized, and the sample is successively moved to move the minute area to be measured, and all these measured values and sample position parameters are stored in the same manner. 1. A scanning X-ray microscope characterized in that it is configured to form a scattered X-ray image, a diffraction X-ray image, a transmitted X-ray image, a fluorescent X-ray image, or a tomographic image thereof. 2) The X-ray tube is a hollow tube whose inner wall is shaped like a long spheroid whose focal points are two points: the point where the X-rays are generated by electron beam irradiation and the fixed measurement point. The X-rays emitted from the generation point satisfy a critical angle for total X-ray reflection at the incident end of the hollow thin tube, and the inner wall surface is composed of a smooth surface capable of causing total X-ray reflection. The scanning X-ray microscope according to item 1. 3) The X-ray conduit is a hollow tube whose inner wall is shaped like a long cone with both ends cut off or a cylinder, and the X-rays emitted from the X-ray generation point undergo total X-ray reflection at the incident end of the hollow tube. 2. The scanning X-ray microscope according to claim 1, wherein the scanning X-ray microscope satisfies a critical angle and has an inner wall surface that is smooth and capable of causing total X-ray reflection. 4) The X-ray conduit is a hollow tube with a small focal point and whose inner wall shape is the shape of a long paraboloid of revolution with the tip cut off.
The X-rays emitted from the X-ray generation point are
2. A scanning X-ray microscope according to claim 1, which satisfies a critical angle for total linear reflection and is constructed of a smooth surface whose inner wall surface can cause total internal reflection of X-rays.