KR102170972B1 - Apparatus for measuring thickness of material using x-ray - Google Patents

Abstract

The apparatus for measuring material thickness using X-rays according to an embodiment of the present invention includes an X-ray unit for emitting X-rays for a predetermined time; A sample fixing part fixing the sample in the traveling direction of the emitted X-rays; A fluorescent ray collection unit fixed at a specific position to collect fluorescent rays emitted from the sample after the emitted X-rays are incident on the sample; And a controller configured to control the sample fixing unit to rotate the sample, and to detect a thickness of a material formed on the surface of the sample and a density of elements included in the formed material based on the collected fluorescent rays.

Description

Material thickness measurement device using X-ray {APPARATUS FOR MEASURING THICKNESS OF MATERIAL USING X-RAY}

The present invention relates to an apparatus for measuring material thickness using X-rays that precisely measures the thickness of a material formed on a surface of a sample while rotating a sample.

In general, the method of measuring the thickness of a material can be divided into a destructive method and a non-destructive method.The destructive method includes an electrolytic method and a method of making a specimen and observing it with an optical microscope or an electron microscope.The non-destructive method is magnetic induction method and ultrasonic wave A method, a method using eddy current, and a method using gamma rays or X-rays are mainly used.

Conventionally, an electrolytic material thickness measurement device that measures the thickness of a material from a change in potential difference caused by electrolyzing a metal material by using a reagent capable of causing an electrochemical reaction to a specific metal material, and A method for measuring the material thickness used has been disclosed.

However, in the case of a conventional electrolytic material thickness measuring apparatus, there is a problem that a sample (sample) cannot be preserved when measuring the material thickness.

In addition, the generally used non-destructive material thickness measurement method has a problem that only planar analysis is possible.

In order to solve these problems, it is necessary to develop a technique for preserving a sample as a non-destructive material thickness measurement method and measuring the thickness of a material formed on the surface of the sample, regardless of the shape of the sample.

KR 10-2002-0082801 A

The present invention relates to a material thickness measurement apparatus using X-rays for non-destructively measuring the thickness of a material by analyzing a fluorescence signal generated by X-rays and X-ray imaging while rotating a sample by 360°.

The apparatus for measuring material thickness using X-rays according to an embodiment of the present invention includes an X-ray unit for emitting X-rays for a predetermined time; A sample fixing part fixing the sample in the traveling direction of the emitted X-rays; A fluorescent ray collection unit fixed at a specific position to collect fluorescent rays emitted from the sample after the emitted X-rays are incident on the sample; The sample fixing part may be controlled to rotate the sample, and may include a controller configured to detect a thickness of a material formed on the surface of the sample and a density of elements included in the formed material based on the collected fluorescent rays. .

The control unit may control the sample fixing part so that the sample is rotated with respect to a central axis of the sample perpendicular to a normal line of an X-ray incident on the sample.

The control unit controls the sample fixing unit so that the sample is rotated about the z axis when the emitted X-ray is incident on the sample in the x-axis direction when the sample is located on the z-axis plane in the three-dimensional plane. can do.

When the sample has a cylindrical shape, the control unit may control the sample fixing part so that the sample is rotated about an axis of the sample.

The fluorescent ray collection unit may be fixed at a position spaced apart from the X-ray unit and the sample fixing unit, and may not block the progress of the emitted X-rays.

The x-ray unit may include a diaphragm for adjusting a diameter of the emitted x-ray.

The controller may adjust the degree of opening of the aperture based on the size of the fixed sample.

The preset time is a time during which the specimen fixing part rotates 360° at a constant angular speed.

The control unit may control the x-ray unit to emit the x-ray for the predetermined time.

The control unit extracts the fluorescent rays collected at regular time intervals among the collected fluorescent rays, measures a wavelength of each of the extracted fluorescent rays, and includes each of the extracted fluorescent rays based on the measured wavelengths of the fluorescent rays. You can detect the elements that emit

The control unit measures the intensity of the fluorescent ray emitted by each of the detected elements at each predetermined time interval, and calculates the density of each of the detected elements based on the intensity of the fluorescent ray emitted by each of the detected elements. Can be measured.

The control unit may measure the thickness of the formed material based on the measured density of each of the elements at each predetermined time interval.

It may further include a photographing unit positioned in the traveling direction of the emitted X-rays and photographing an image of the sample projected by the X-rays passing through the sample.

The control unit may additionally measure the thickness of the material formed on the surface of the sample from the captured image of the sample.

The photographing unit may include a scintillator through which X-rays passing through the sample are passed and converted into visible light; An optical lens to enlarge the converted visible light; A detection plate on which the enlarged visible light is projected; And a camera that photographs an image of visible light projected on the detection plate.

The scintillator, the optical lens, the detection plate, and the camera may have their centers arranged on the optical axis of the emitted X-ray.

According to an exemplary embodiment of the present invention, the apparatus for measuring material thickness using X-rays has the advantage of being able to measure the uniformity of elements included in the surface of one section of the sample and the thickness of the material formed on the surface while rotating the sample by 360°.

In addition, there is an advantage in that the degree of opening of the aperture can be adjusted to measure the uniformity of elements included in the surface of the sample and the thickness of the material formed on the surface.

In addition, when measuring the thickness of a material using the conventional electrolytic method, the problem that the sample of the sample cannot be preserved and the problem that only planar analysis is possible when measuring the thickness of the material using X-rays has been solved, so that the shape of the sample is restricted. Fluorescent ray analysis is possible without receiving, and there is an advantage in that a sample of the sample used for analysis is also preserved.

In addition, not only measuring the thickness of the material through fluorescence ray analysis, but also taking an image of the sample projected by X-ray and measuring the thickness of the material based on the captured image, the thickness of the material formed on the surface of the sample There is an advantage that can be measured twice.

BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are included as part of the detailed description to aid in understanding of the present invention, provide embodiments of the present invention, and together with the detailed description, the technical features of the present invention will be described.
1 is a block diagram schematically showing an apparatus for measuring material thickness using X-rays according to an embodiment of the present invention.
2 is a diagram illustrating an example of rotating a cylindrical sample in the apparatus for measuring material thickness using X-rays according to an embodiment of the present invention.
3 is a diagram showing X-ray fluorescence analysis measurement data using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.
4A and 4B are diagrams illustrating X-ray fluorescence analysis results of samples measured using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.
5A and 5B are diagrams showing X-ray images of samples taken using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.

In the present specification, terms such as first and/or second are used only for the purpose of distinguishing one component from another component. That is, it is not intended to limit the components by the terms.

Components, features, and steps referred to as'include' in this specification mean the existence of the corresponding components, features, and steps, and are intended to exclude one or more other components, features, steps, and equivalents thereof. This is not.

Unless otherwise specified and stated in the singular form in the specification, plural forms are included. That is, the components and the like mentioned in the present specification may mean the presence or addition of one or more other components.

Unless otherwise defined, all terms used in this specification, including technical or scientific terms, have the same meaning as commonly understood by a person of ordinary skill in the art to which the present invention belongs. to be.

That is, terms such as those defined in commonly used dictionaries should be interpreted as having meanings consistent with the meaning of the context of the related technology, and should be interpreted as ideal or excessively formal meanings unless explicitly defined in this specification. It doesn't work.

Hereinafter, an apparatus for measuring material thickness using X-rays according to an embodiment of the present invention will be described in detail with reference to the accompanying drawings.

1 is a block diagram schematically showing an apparatus for measuring material thickness using X-rays according to an embodiment of the present invention.

Referring to FIG. 1, the apparatus 100 for measuring material thickness using X-rays according to an embodiment of the present invention includes an X-ray unit 101, a sample fixing unit 103, a fluorescent ray collection unit 105, and a photographing unit 107. ) And a control unit 109.

The X-ray unit 101 may emit X-rays toward the sample fixed to the sample fixing unit 103 for a predetermined time. The preset time is a time required for the specimen fixing unit 103 rotating at a constant angular speed by the control unit 109 to rotate 360°, for example, may be set to 3 seconds.

The X-ray unit 101 includes a diaphragm and an X-ray lens for adjusting the size of the diameter of the emitted X-rays, and the degree of opening of the stop by the control unit 109 is adjusted.

The material thickness measurement apparatus 100 according to an exemplary embodiment of the present invention may adjust the size of the diameter of the emitted X-rays using an X-ray lens, an aperture stop, a focusing mirror, or a K-B mirror.

The sample fixing unit 103 may fix the sample in the traveling direction of the x-rays emitted from the x-ray unit 101. For example, the sample fixing part 103 may be positioned in the traveling direction of the emitted X-rays to fix the sample so that the emitted X-rays pass through the sample.

The specimen fixing unit 103 can be moved and rotated under the control of the control unit 109. The sample fixing unit 103 is a rotating stage that can rotate and a 3-axis stage that can be moved in three axes to be rotated and moved, and a sample is fixed to one side of the sample fixing unit 103 to fix the emitted X-rays. Passed through the sample.

For example, the specimen fixing unit 103 can be moved in the x-axis or y-axis under the control of the controller 109, and can adjust the height of the specimen fixed in the z-axis direction. In addition, the sample fixing unit 103 may rotate the sample by rotating under the control of the control unit 109.

The fluorescent ray collection unit 105 may be fixed at a specific position and collect fluorescent rays emitted from the sample after the emitted X-rays are incident on the sample. That is, the fluorescent ray collection unit 105 may be positioned to be spaced apart from the X-ray unit 101 and the sample fixing unit 103, and may be fixed at a position that does not block the progress of the emitted X-rays.

For example, when the sample is a cylindrical metal wire, the sample rotates around the axis of the cylinder, and the emitted X-rays are incident on the sample. The fluorescent ray collection unit 105 may collect fluorescent rays emitted from a portion where X-rays are incident while the sample is rotated in a fixed position.

Fluorescent rays collected by the fluorescent ray collection unit 105 are analyzed by the control unit 109 to detect the thickness of the material formed on the surface of the sample and the uniformity of elements included in the formed material.

The photographing unit 107 is located in the traveling direction of the emitted X-rays and may capture an image of a sample projected by the emitted X-rays independently of collecting the fluorescent rays emitted from the fluorescent ray collection unit 105. The controller 105 may measure the thickness of the material formed on the surface of the sample from the image of the sample captured by the photographing unit 107 separately from analyzing the collected fluorescent rays.

The photographing unit 107 includes a scintillator in which X-rays passing through the sample are passed and converted into visible light, an optical lens that enlarges the converted visible light, a detection plate on which the enlarged visible light is projected, and It may include a camera that photographs an image of visible light.

In order to improve the resolution of an image of a sample to be photographed, the scintillator, the optical lens, the detection plate, and the center of the camera may be arranged in parallel on the optical axis of the emitted X-ray.

The control unit 109 may control the x-ray unit 101 to emit X-rays for a predetermined time. For example, if the sample rotates 360° for 3 seconds, the controller 109 may control the x-ray unit 101 to emit X-rays for 3 seconds during which the sample rotates once.

That is, the control unit 109 may rotate the sample by 360° to detect the thickness of the material formed on the surface of one end face of the sample and the uniformity of the elements included in the formed material.

In addition, the control unit 109 may adjust the degree of opening of the aperture included in the x-ray unit 101 in order to adjust the size of the diameter of the x-ray emitted from the x-ray unit 101 according to the size of the sample.

For example, the control unit 109 can detect the thickness of a material formed on the surface of the wire rod by opening the diaphragm very finely and using a pin hole effect.

The control unit 109 may control the sample fixing unit 103 to rotate the sample. That is, the control unit 109 may control the sample fixing unit 103 to rotate the sample based on the central axis of the sample perpendicular to the normal line of the X-ray incident on the sample.

For example, if the sample is fixed to the sample fixing part 103 such that the emitted X-ray proceeds in the x-axis direction and the central axis of the sample is located on the z-axis (axis parallel to the vertical line), the controller 109 The sample fixing part 103 may be controlled to rotate the sample based on the z axis, that is, the central axis (z axis) of the sample perpendicular to the normal line of the X-ray.

In addition, the control unit 109 may precisely control the position of the sample by controlling the sample fixing unit 103 so that the emitted X-rays pass through the sample. For example, the control unit 109 may move the sample fixing unit 103 in the direction of one or more of the x-axis, y-axis, or z-axis by moving the sample fixing unit 103, and rotate the sample by rotating the sample fixing unit 103. I can.

Next, after rotating the sample, the control unit 109 may detect the thickness of the material formed on the surface of the sample and the density of elements included in the formed material based on the fluorescent rays collected by the fluorescent ray collection unit 105 .

The control unit 109 may control the sample fixing unit 103 to rotate the sample based on a central axis of the sample perpendicular to the normal of the X-ray incident on the sample.

For example, when the sample is in the shape of a cylinder, the control unit 109 may control the sample fixing part 103 to rotate the sample based on the axis of the sample (the axis of the cylinder). When the sample has a spherical shape, the controller 109 may control the sample fixing part 103 to rotate the sample based on an axis perpendicular to the optical axis of the X-ray incident on the sample.

The control unit 109 may detect a thickness of a material formed on the surface of the sample and a uniformity of elements included in the formed material from the fluorescent rays collected for a predetermined time by the fluorescent ray collection unit 105.

The control unit 109 extracts the fluorescent rays collected at regular time intervals among the collected fluorescent rays, measures the wavelength of each of the extracted fluorescent rays, and emits each of the extracted fluorescent rays based on the wavelength of the measured fluorescent rays. Elements can be detected.

For example, the control unit 109 may extract fluorescent rays from the collected fluorescent rays every 4° rotation time, and extract the fluorescent rays 90 times. The control unit 109 may detect elements emitting the fluorescent rays extracted at the first time by measuring wavelengths of the fluorescent rays extracted at the first time. In the same way, the controller 109 may detect elements that emit the fluorescent rays extracted at each time based on the wavelength of the fluorescent rays extracted at the second to 90th hours.

That is, when X-rays are incident on the sample, electrons in the inner shell of each element included in the sample are excited, and the excited electrons become quite excited, so electrons in the outer shell fill the inner shell to stabilize this. . At this time, energy corresponding to the binding energy of each shell is released, which is called a fluorescent ray, and each element has its own energy and wavelength. Accordingly, the control unit 109 may detect the elements emitting the fluorescent rays by measuring the wavelength of each of the extracted fluorescent rays at regular intervals.

In addition, the control unit 109 measures the intensity of the fluorescent rays emitted by each of the detected elements at regular time intervals, and measures the density of each of the detected elements based on the intensity of the fluorescent rays emitted by each of the detected elements. And, it is possible to measure the thickness of the formed material based on the measured density of the elements.

For example, the control unit 109 measures the intensity of the fluorescent rays emitted by each of the elements detected at the first time, extracts the density, that is, uniformity, of each element, and measures the thickness of the formed material based on the density of the elements. I can. The control unit 109 may measure the density of the elements detected in the second to 90th hours and the thickness of the formed material in the same way.

That is, the control unit 109 detects the uniformity of elements included in the surface of one section of the sample and the thickness of the formed material while the sample is rotated by 360°, so that the user can determine whether the surface of the sample is uniformly formed. have.

The controller 109 may additionally measure the thickness of the material formed on the surface of the sample by analyzing the X-ray image of the sample photographed by the photographing unit 107.

That is, the material thickness measurement apparatus 100 according to an embodiment of the present invention i) rotates the sample by 360° and analyzes the collected fluorescent rays, thereby reducing the thickness of the material formed on the surface of the sample and the elements included in the formed material. By detecting the uniformity and ii) analyzing the image of the sample projected by X-rays, the thickness of the material formed on the surface of the sample is measured, and the thickness of the material formed on the surface of the sample can be measured twice.

2 is a diagram illustrating an example of rotating a cylindrical sample in the apparatus for measuring material thickness using X-rays according to an embodiment of the present invention.

Referring to FIG. 2, when the sample 201 is fixed such that the axis of the sample 201 is positioned on the z-axis 207, the emitted X-rays are sampled in the x-axis 203 or y-axis 205 direction. When incident on 201), when the sample 201 is rotated based on the z-axis 207, the thickness of the material formed on the surface of one end face of the sample 201 may be measured.

The controller 109 rotates the sample fixing part 103 to rotate the sample 201 fixed to the sample fixing part 103 with respect to the z-axis 207, and included in the surface of one section of the sample 201 The uniformity of the formed elements and the thickness of the material formed on the surface can be measured.

3 is a diagram showing X-ray fluorescence analysis measurement data using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.

3, as a result of analyzing the fluorescent wire collected at a specific point in time, it was found that iron (Fe), copper (Cu), and zinc (Zn) were detected in a steel wire in which copper (Cu) and zinc (Zn) were formed. Able to know.

Each of the elements can be detected with the elements contained in the material formed on the surface of the sample by analyzing the collected type light because it has a wavelength unique fluorescent line (Cu _kα, Cu _kβ, Zn _kα and Zn _kβ) . In addition, it is possible to detect the density of each element, that is, how much each element is contained through the intensity of the fluorescent ray emitted from each element.

4A and 4B are diagrams illustrating X-ray fluorescence analysis results of samples measured using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.

4A and 4B, the control unit 109 determines the uniformity of the elements of the material formed on the surface of the sample and the thickness of the formed material from the fluorescent rays extracted at regular time intervals among the fluorescent rays collected while the sample is rotated 360°. Can be measured.

The x-ray used for fluorescence analysis is 10 keV monochromatic light, the diameter of the x-ray is 120 μm, and the measurement angle is 360° (displacement 4°).

When the control unit 109 analyzes the first sample 301, it can be seen that copper and zinc are uniformly included in one end surface of the first sample 301, and the thickness of the formed material is also uniform.

Looking at the results of the control unit 109 analyzing the second sample 303, copper is skewed in the lower right direction (60° to 180° direction) in one cross section of the second sample 303, and zinc is in the upper left direction. It is skewed in the direction (240° to 0° direction), so it can be seen that the elements included in the formed material are not uniformly distributed.

As such, the material thickness measurement apparatus 100 according to an embodiment of the present invention uses a conventional X-ray to measure the thickness of a material formed on a sample formed in a curved shape such as a wire rod due to the curvature of the sample using only a plane. By solving the problem of the formula material thickness measurement technology, there is an advantage of being able to measure the thickness of the material formed on the 360° surface of one cross section of the sample and the uniformity of the elements included in the formed material.

5A and 5B are diagrams showing X-ray images of samples taken using an X-ray material thickness measurement apparatus according to an embodiment of the present invention.

FIG. 5A is an image of the first sample 301 projected by X-rays, and FIG. 5B is an image of the second sample 303 projected by X-rays having the same diameter.

\*83 The size of the captured images of the first sample 301 and the second sample 303 is 20 μm, and the image resolution is 40 nm.

As described above, the material thickness measurement apparatus 100 according to an embodiment of the present invention analyzes the fluorescent rays emitted by the elements included in the sample to measure the thickness of the material formed on the surface of the sample and the uniformity of the elements included in the formed material. In addition, there is an advantage in that the thickness of the material formed on the surface of the sample can be measured by taking an image of the sample projected by X-rays.

Although the description in the present specification has been shown in several exemplary aspects, various modifications or changes may be made from the scope defined by the claims to be described later, and the technical protection scope of the present invention is in the following claims. Should be decided by

100: material thickness measuring device 201: sample
101: x-ray unit 203: x-axis
103: sample fixing part 205: y-axis
105: fluorescent ray collection unit 207: z-axis
107: photographing unit 301: first sample
109: control unit 303: second sample

Claims (14)

An x-ray unit emitting X-rays for a predetermined time;
A sample fixing part fixing the sample in the traveling direction of the emitted X-rays;
A fluorescent ray collection unit fixed at a specific position to collect fluorescent rays emitted from the sample after the emitted X-rays are incident on the sample;
A photographing unit positioned in the traveling direction of the emitted X-rays and photographing an image of the sample projected by the X-rays passing through the sample; And
Controlling the sample fixing unit to rotate the sample, extracting the fluorescent rays collected at regular time intervals among the collected fluorescent rays, measuring the wavelength of each of the extracted fluorescent rays, and Detecting elements emitting each of the extracted fluorescent rays based on the wavelength,
Each of the elements included in the material formed on the surface of the sample is measured based on the intensity of the fluorescence ray emitted by each of the detected elements at each predetermined time interval, and Measure the density of,
Measuring the thickness of the formed material based on the density of the detected elements,
Including a control unit for additionally measuring the thickness of the material formed on the surface of the sample in the image of the photographed sample,
The x-ray unit includes a diaphragm for adjusting a diameter of the emitted x-rays,
The control unit, based on the size of the fixed sample, adjusts the degree of opening of the aperture,
The X-ray unit emits X-rays for a predetermined time according to the rotational angular velocity of the sample fixed to the sample fixing unit,
A material thickness measurement device using X-rays.
The method of claim 1,
The control unit,
Controlling the sample fixing part so that the sample is rotated based on a central axis of the sample perpendicular to the normal line of the X-ray incident on the sample,
A material thickness measurement device using X-rays.
The method of claim 1,
The control unit,
When the sample is positioned on the z-axis plane in the three-dimensional plane, when the emitted X-ray is incident on the sample in the x-axis direction,
Controlling the sample fixing part so that the sample is rotated about the z-axis,
A material thickness measurement device using X-rays.
The method of claim 1,
The control unit,
When the sample is in the shape of a cylinder,
Controlling the sample fixing part so that the sample is rotated with respect to the axis of the sample,
A material thickness measurement device using X-rays.
The method of claim 1,
The fluorescent ray collection unit,
It is fixed at a position spaced apart from the X-ray unit and the sample fixing unit, and does not block the progress of the emitted X-ray,
A material thickness measurement device using X-rays.
delete The method of claim 1,
The preset time is,
It is the time that the sample fixing part rotates 360° at a constant angular speed,
The control unit,
Controlling the x-ray unit to emit the x-rays during the preset time,
A material thickness measurement device using X-rays.
delete delete The method of claim 1,
The control unit,
Measuring the thickness of the formed material based on the density of each of the measured elements at each predetermined time interval,
A material thickness measurement device using X-rays.
delete delete The method of claim 1,
The photographing unit,
A scintillator through which X-rays passing through the sample are passed and converted into visible light;
An optical lens to enlarge the converted visible light;
A detection plate on which the enlarged visible light is projected; And
Comprising a camera for photographing an image of visible light projected on the detection plate,
A material thickness measurement device using X-rays.
The method of claim 13,
The scintillator, optical lens, detection plate, and camera,
The center is arranged on the optical axis of the emitted x-rays,
A material thickness measurement device using X-rays.

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