KR20160049124A - Apparatus and Method for measuring thickness/composition of metal foil - Google Patents

Apparatus and Method for measuring thickness/composition of metal foil Download PDF

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KR20160049124A
KR20160049124A KR1020140145176A KR20140145176A KR20160049124A KR 20160049124 A KR20160049124 A KR 20160049124A KR 1020140145176 A KR1020140145176 A KR 1020140145176A KR 20140145176 A KR20140145176 A KR 20140145176A KR 20160049124 A KR20160049124 A KR 20160049124A
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thickness
metal foil
component
ray
sample
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KR1020140145176A
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Korean (ko)
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KR101639882B1 (en
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홍재화
정관호
이재곤
김홍준
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주식회사 포스코
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Abstract

An apparatus and method for measuring the thickness / component of a metal foil are presented. The apparatus for measuring a thickness / component of a metal foil is configured to generate X-rays on a metal foil sample positioned in a downward direction, and simultaneously detect transmitted X-rays transmitted through the metal foil sample and fluorescent X- Detecting module And an analysis module for analyzing the thickness and the component of the metal foil sample using the transmittance of the transmitted X-ray and the total spectral intensity of the fluorescent X-ray.

Description

Technical Field [0001] The present invention relates to an apparatus and a method for measuring a thickness / composition of a metal foil,

The present invention relates to an apparatus and a method for simultaneously measuring the thickness and component of a metal foil on-line.

Metal foils have been developed for various applications and are being used in industries. For example, aluminum foil is widely used for domestic and food cooking, and stainless foil is mainly used as a building interior material or exterior material. Special-purpose metal foils are also being produced. In the case of an invar alloy foil, the coefficient of thermal expansion is low and it is sometimes used as an FMM (Fine Metal Mask) of organic light emitting diodes.

Various methods can be used to measure the thickness of the foil. Normally, the measuring instrument has a micrometer, which can measure the thickness of the metal foil simply and nondestructively. However, in a conventional micrometer, measurement accuracy can not be precisely measured to about micrometer.

Also, when the surface roughness of the metal to be measured is large, the measurement error becomes larger. This method has a disadvantage in that it is impossible to measure in real time during production of the product.

On the other hand, in the case of an alloy foil, it is necessary to measure the thickness of the foil. However, since the composition of the foil affects the physical properties of the product, it must be measured and controlled.

In order to measure the composition of the alloy, it is possible to dissolve the foil and analyze the component by ICP (Inductively Coupled Plasma) method. However, this method requires time and effort because the sample has to be destroyed, and it is impossible to measure it online.

In order to measure the sample non-destructively, there is a method of using X-ray, which is a method in which an X-ray is incident on one side of a foil to be measured, and the intensity of X-rays transmitted through the opposite side of the foil is measured. Using the method of comparing with the intensity of the X-ray, it is possible to measure the thickness of the foil relatively non-destructively and the X-ray thickness measuring apparatus using this principle is commercialized and used.

However, these instruments are capable of measuring the thickness of single-component metal foils, but are not available if the alloy composition of the sample changes.

In addition, since such a device can measure thickness only, a separate measuring device must be installed in order to measure the component, so that the installation space of the measuring device becomes large and the total investment cost of the device increases. Fluorescence X-rays may be used to measure the composition of the alloy or metal foil.

However, since the intensity of the fluorescent X-ray changes according to the alloy component but also changes depending on the thickness of the foil, the fluorescent X-ray method of the conventional method can not accurately measure the alloy component.

Since a conventional fluorescence X-ray component measuring device can measure only when the thickness of the material is thicker than the transmission depth of fluorescent X-ray, there is a problem that the measurement accuracy of the metal foil with a thickness of several tens of micrometers is significantly lowered.

Korean Patent Publication No. 2004-0072780 (published on Aug. 19, 2004) (Name of the invention: Thin Film Thickness Measurement Method)

The present invention has been made in order to solve the problems of the prior art, and as described above, when the metal foil has a different composition and the thickness of the metal foil is thinner than the X-ray penetration depth, I do not.

Accordingly, in the present invention, an apparatus and a method for measuring the thickness / component of a metal foil capable of rapidly and precisely measuring the thickness and the composition of the metal foil composed of an alloy by using the integral intensity of the transmitted X-rays and the spectral intensity of the fluorescent X- And to provide the above objects.

According to an aspect of the present invention, there is provided an apparatus for measuring a thickness / component of a metal foil, which comprises: generating X-rays on a sample of a metal foil positioned in a downward direction; A detection module for simultaneously detecting fluorescent X-rays reflected on the metal foil sample; And an analysis module for analyzing the thickness and the component of the metal foil sample using the transmittance of the transmitted X-ray and the total spectral intensity of the fluorescent X-ray.

Wherein the detection module comprises: an upper module for generating X-rays having a predetermined voltage in the metal foil, and then detecting fluorescent X-rays reflected on the metal foil sample; And a lower module including a transmission X-ray detector for detecting the transmission X-ray, the lower module being spaced apart from a lower end of the upper module and spaced apart from the lower module.

The lower module further includes a metal foil filter for linearly adjusting a variation width of the transmitted X-ray according to the thickness of the metal foil sample.

The lower module further includes a temperature measuring unit for measuring a temperature in the spacing space.

According to another aspect of the present invention, there is provided a method of measuring a thickness / component of a metal foil, the method comprising: irradiating a metal foil sample with an X-ray from a detection module; A detection step of detecting, by the detection module, the amount of transmitted X-rays of the metal foil sample and the total spectral intensity of fluorescent X-rays; And a thickness and a component calculating step of calculating the thickness and the component of the metal foil sample by the analysis module using the transmission amount of the transmission X-ray and the total spectrum intensity of the fluorescent X-ray.

Wherein the thickness and the component calculating step include: a thickness calculating step of calculating a thickness of the metal foil sample using the transmission X-ray transmission amount; A component correction step of calculating the components of the metal foil sample using a fundamental variable method or a multivariate regression equation and then correcting the component to improve the accuracy of the calculated component; And a thickness and component recalculation step of recalculating the thickness of the metal foil sample using the corrected component and recalibrating the corrected component using the re-calculated thickness.

According to one embodiment of the present invention, the apparatus for measuring the thickness / component of a metal foil provides the advantage that the thickness and the component of the metal foil can be measured quickly and accurately on-line.

According to an embodiment of the present invention, the thickness / component measuring device for a metal foil can measure the thickness of a metal foil by using a component of the metal foil, thereby improving the accuracy of thickness even if the metal foil is an alloy component .

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an exemplary view showing an apparatus for measuring a thickness / component of a metal foil according to an embodiment of the present invention; FIG.
2 is a flowchart illustrating a method of measuring a thickness / component of a metal foil according to an embodiment of the present invention.
3 is a graph showing the transmission X-ray intensity according to the thickness of the metal foil sample.

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below. The shape and the size of the elements in the drawings may be exaggerated for clarity and the same elements are denoted by the same reference numerals in the drawings.

FIG. 1 is a schematic view showing an apparatus for measuring a thickness / component of a metal foil according to an embodiment of the present invention.

As shown in FIG. 1, an apparatus 100 for measuring a thickness / component of a metal foil according to an embodiment of the present invention includes a detection module 200 and an analysis module 300.

The detecting module 200 has a function of detecting X-rays transmitted through the metal foil sample and fluorescent X-rays reflected by the metal foil sample simultaneously after generating X-rays in the metal foil sample located in the lower direction .

More specifically, the detection module 200 includes an upper module 210 and a lower module 220.

The upper module 210 detects a fluorescent X-ray reflected on the metal foil sample due to an X-ray of a predetermined voltage generated in the metal foil sample.

The upper module 210 may include an X-ray generator 211 configured to generate an X-ray having a preset voltage, and an X-ray generator 211 configured to include a power supply unit. The X-ray generator 211 detects the fluorescent X- And a fluorescence X-ray detector 212 for measuring the fluorescence X-ray.

The fluorescent X-ray detector 212 is a semiconductor detector, and the X-ray energy may be at least 15 kV or more and 70 kV or less.

Here, the semiconductor detector is smaller than the other type detectors and has a high energy resolution, so that it is advantageous in that the components can be easily separated in the case of metal alloys of different components. The signals detected by the semiconductor detector are detected by a pulse height analyzer, Or a multiple signal analyzer to convert the intensity value into energy.

The reason why the X-ray energy uses a voltage of at least 15 kV to 70 kV is as follows.

When the voltage is 15 kV or less, the amount of transmitted X-ray decreases sharply and not only the precision of measuring the thickness of the metal foil sample is lowered, but also the intensity of the fluorescent X-ray emitted from the sample is lowered.

In addition, when the voltage of the X-ray energy is 70 kV or more, the rate of change of the transmitted X-ray varies with the thickness of the metal foil sample, and thus the thickness measurement accuracy becomes low.

Therefore, in the present invention, the X-ray energy is at least 15 kV to 70 kV.

Meanwhile, the lower module 220 is spaced apart from the lower end of the upper module 210 by a space and includes a transmission X-ray detector 221 for detecting the transmitted X-rays.

The transmission X-ray detecting unit 221 may be a proportional counter or a scintillation counter detector. This means that the X-ray generated from the X-ray generating unit passes through the metal foil sample and reaches the detector This is because it is advantageous to use a large-area detector because the path is relatively long.

Here, the lower module 220 may further include a metal foil filter (not shown) for linearly controlling the variation width of the transmitted X-rays according to the thickness of the metal foil sample.

The lower module 220 may further include a temperature measuring unit 223 for measuring a temperature in the spacing space.

In addition, the lower module 220 may further include a stand (not shown) for receiving and fixing the metal foil sample into the spacing space.

Next, the analysis module 300 calculates the thickness and the component of the metal foil sample using the transmission X-ray transmission amount and the total spectral intensity of the fluorescent X-ray.

More specifically, the analysis module 300 calculates a component of the metal foil sample using a thickness calculation process, a basic parameter method, or a multivariate regression formula for calculating the thickness of the metal foil sample using the transmission X- A component correction step of correcting the component so as to improve the accuracy of the calculated component, and a step of re-calculating the thickness of the metal foil sample using the corrected component, And corrects the thickness and the component of the metal foil sample, thereby performing the function of measuring the thickness and the component of the metal foil sample.

The thickness calculation process may be a process of calculating the thickness of the metal foil sample using Equation 1 below.

[Formula 1]

Figure pat00001

Where I is the transmitted X-ray intensity, t is the metal foil thickness, and a, b, and c are fitting constants.

The component correction process may be a process of calculating the components of the metal foil sample using a basic parameter method or a multivariate regression equation, and then correcting the component using Equation 2 described below to improve the accuracy of the calculated component.

[Formula 2]

Figure pat00002

Here, X is the post-correction foil component, X 'is the pre-correction foil component, Y is the foil thickness, and a, b, and c are fitting constants.

Finally, in order to improve the precision of the thickness of the metal foil calculated in [Formula 1], the thickness and the component recalculation process are applied to the following [Formula 3] Calibrating the component using the re-calculated thickness after reassembling the foil thickness.

[Formula 3]

Figure pat00003

Where X is the foil thickness after correction, X 'is the foil thickness before correction, Y is the alloy composition ratio, and a, b, and c are fitting constants.

2 is a flowchart illustrating a method of measuring a thickness / component of a metal foil according to an embodiment of the present invention.

2, a method S100 of measuring the thickness / component of a metal foil according to an embodiment of the present invention includes an X-ray irradiation step S110, a detecting step S120, a thickness and a component calculating step S130, .

The X-ray irradiation step (S110) may be a step of irradiating the metal foil sample with X-rays from the detection module (200).

The detecting step S120 may be a step of detecting the transmission amount of the transmitted X-ray of the metal foil sample and the entire spectrum intensity of the fluorescent X-ray by the detection module 200. [

The thickness and the component calculating step (S130) may be a step of calculating the thickness and the component of the metal foil sample in the analysis module using the transmission X-ray transmission amount and the whole spectral intensity of the fluorescent X-ray.

More specifically, the thickness and component calculation step S130 includes a thickness calculation step S131, a component correction step S132, and a thickness and component recalculation step S133.

The thickness calculation step S131 may be a step of calculating the thickness of the metal foil sample using the transmission X-ray transmission amount.

The component correction step (S132) may be a step of calculating the components of the metal foil sample using a basic variable method or a multivariate regression equation, and then correcting the components so as to improve the accuracy of the calculated components.

The thickness and component recalculation step (S133) may be a step of recalculating the thickness of the metal foil sample using the corrected component, and then recalibrating the corrected component using the re-calculated thickness.

More specifically, the thickness calculating step (S131) may be a step of calculating the thickness of the metal foil sample using the above-mentioned [Equation 1].

The component correction step (S132) may include calculating a component of the metal foil sample using a basic variable method or a multivariate regression equation, and then correcting the component using Equation 2 to improve the accuracy of the calculated component Lt; / RTI >

The thickness and component recalculation step (S133) may be performed by applying the component corrected in [Formula 2] to the [Formula 3] to improve the precision of the thickness of the metal foil calculated in the [Formula 1] And re-correcting the corrected component using the re-calculated thickness after recalculating the thickness.

Meanwhile, the present invention can be realized by storing computer-readable codes in a computer-readable storage medium. The computer-readable storage medium includes all kinds of storage devices in which data that can be read by a computer system is stored. The computer readable code is configured to perform the steps of implementing a method of measuring thickness and composition of a metal foil in accordance with the present invention when read and executed by a processor from the computer readable storage medium.

The computer readable code may be implemented in a variety of programming languages. And functional programs, codes, and code segments for implementing embodiments of the present invention may be readily programmed by those skilled in the art to which the present invention pertains.

Examples of the computer-readable storage medium include ROM, RAM, CD-ROM, magnetic tape, floppy disk, optical data storage device or SSD, Flash memory and the like in the form of a carrier wave .

In addition, the computer-readable storage medium may be distributed over a networked computer system so that computer readable code is stored and executed in a distributed fashion.

Hereinafter, the relationship between the thickness, the component, and the tube voltage (X-ray energy) of the metal foil sample will be described in more detail with reference to experimental examples using the apparatus for measuring thickness / component of the metal foil.

[Experimental Example]

In this experiment, X-rays were generated by applying a power of 20 kV, 30 kV, and 5 uA to an X-ray source.

The generated X-rays were made incident on a standard sample having various compositions and components, and the transmitted X-rays were measured by using a proportional counter type X-ray detector.

Table 1 below shows the intensity of transmitted X-rays at 20 kV and 30 kV.

[Table 1]

Figure pat00004

Referring to Table 1, in the present experiment, the thickness, component, and tube voltage (20 kV, 30 kV) of each of the ten metal foil samples were measured, and then the intensity of the transmitted X-ray was plotted against the thickness of the metal foil sample 3)

The points shown in FIG. 3 are data values, and the solid line is a value obtained by a regression equation according to [Equation 1].

The regression equation calculated in this experiment is as follows.

I (X-ray transmission intensity) = 7136392 + 68169exp (-0.040t)

In this experiment, the regression equation described above was calculated for t (thickness), and then the thickness was calculated by applying the intensity of the transmitted X-ray to the unknown sample.

Table 2 below shows the thickness values of the metal foil samples predicted using the energy of the transmitted X-rays measured at the incident X-ray energy of 20 kV and 30 kV, respectively. Referring to Table 2, when the X-ray energy is 30 kV It can be seen that there is less error in comparison with the actual thickness of the standard sample.

In addition, since the error increases when the intensity of the irradiated X-ray is 15 kV or less, the energy of the irradiated X-ray is limited to 15 kV or more.

[Table 2]

Figure pat00005

Table 3 shows the thickness of the metal foil samples before and after calibration using the component values of the metal foil samples.

In order to calibrate the components of the metal foil sample, the intensity of the transmitted X-rays is measured using other standard samples of various kinds of components, and the regression equation is made using [Equation 3] and the regression coefficient is derived.

Referring to Table 3, it can be seen that the thickness measurement error (1.6%) after correcting the components of the metal foil sample is smaller than the error before correction (2.6%).

Here, the components of the metal foil samples were firstly measured by the basic parameter method, and the components of the metal foil samples measured using 36% Ni-64% Fe alloy standard samples of various thicknesses were measured for the component values A difference appears.

[Table 3]

Figure pat00006

That is, it was found that the measurement error after the correction using the formula 2 proposed in the present invention greatly reduces the measurement error according to the foil thickness.

Table 4 shows the measurement error of the metal foil component before and after the thickness correction of the metal foil.

[Table 4]

Figure pat00007

Thus, according to an embodiment of the present invention, a device for measuring the thickness / component of a metal foil provides the advantage that the thickness and component of the metal foil can be measured quickly and accurately on-line.

Further, according to the embodiment of the present invention, when measuring the thickness of the metal foil, it is possible to measure the thickness / component of the metal foil by using the component of the metal foil, thereby improving the accuracy of thickness even if the metal foil is an alloy component. to provide.

The present invention is not limited to the above-described embodiments and the accompanying drawings. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. It will be self-evident.

100: Metal foil thickness / component measuring device
200: Detection module 210: Upper module
211: X-ray generator 212: fluorescent X-ray detector
220: lower module 221: transmission X-ray detector
300: Analysis module

Claims (15)

  1. A detecting module for generating X-rays in the metal foil sample located in the lower direction, and simultaneously detecting transmitted X-rays transmitted through the metal foil specimen and fluorescent X-rays reflected on the metal foil specimen; And
    And an analysis module for analyzing the thickness and the component of the metal foil sample using the transmission amount of the transmission X-ray and the total spectrum intensity of the fluorescent X-ray.
  2. The apparatus of claim 1,
    An upper module for generating X-rays having a predetermined voltage in the metal foil and detecting fluorescent X-rays reflected on the metal foil sample; And
    And a lower module that is spaced apart from a lower end of the upper module and is provided with a transmission X-ray detector for detecting the transmitted X-rays.
  3. [3] The apparatus of claim 2,
    Further comprising a metal foil filter for linearly controlling a variation width of transmission X-rays according to a thickness of the metal foil sample.
  4. 3. The apparatus of claim 2, wherein the lower module comprises:
    And a temperature measuring unit for measuring a temperature in the spacing space.
  5. [3] The apparatus of claim 2,
    An X-ray generating unit generating X-rays of a predetermined voltage; And
    And a fluorescent X-ray detector for detecting the fluorescent X-ray and then measuring the total spectral intensity of the fluorescent X-
    The fluorescence X-ray detector may comprise:
    Wherein the energy of the X-ray is 15 kV or more and 70 kV or less.
  6. The apparatus according to claim 2, wherein the transmission X-
    A device for measuring the thickness / component of a metal foil, which is a Proportional Counter or Scientilation Counter detector.
  7. The apparatus of claim 1,
    Wherein the thickness of the metal foil sample is calculated by using the following formula (1).
    [Formula 1]
    Figure pat00008

    Where I is the transmitted X-ray intensity, t is the metal foil thickness, and a, b, and c are fitting constants.
  8. 8. The system of claim 7,
    An apparatus for measuring the thickness / component of a metal foil, comprising the steps of: calculating a component of the metal foil sample using a basic variable method or a multivariate regression equation, and then correcting the calculated component using Equation 2 below to improve the accuracy of the calculated component;
    [Formula 2]
    Figure pat00009

    Here, X is the post-correction foil component, X 'is the pre-correction foil component, Y is the foil thickness, and a, b, and c are fitting constants.
  9. 9. The system of claim 8,
    In order to improve the precision of the thickness of the metal foil calculated in [Formula 1], the component corrected in [Formula 2] is applied to the following Formula 3 to determine the thickness of the metal foil, Component measuring device.
    [Formula 3]
    Figure pat00010

    Where X is the foil thickness after correction, X 'is the foil thickness before correction, Y is the alloy composition ratio, and a, b, and c are fitting constants.
  10. 3. The method of claim 2,
    Wherein the detection module comprises:
    And a stand capable of loading a standard sample on a side surface of the metal foil sample.
  11. An X-ray irradiation step of irradiating a sample of metal foil with an X-ray from a detection module;
    A detection step of detecting, by the detection module, the amount of transmitted X-rays of the metal foil sample and the total spectral intensity of fluorescent X-rays; And
    And a thickness and a component calculating step of calculating a thickness and a component of the metal foil sample using an analysis module, using the transmission amount of the transmission X-ray and the total spectral intensity of the fluorescent X-ray.
  12. 12. The method of claim 11,
    A thickness calculating step of calculating a thickness of the metal foil sample using the transmission X-ray transmission amount;
    A component correction step of calculating the components of the metal foil sample using a fundamental variable method or a multivariate regression equation and then correcting the component to improve the accuracy of the calculated component; And
    Calculating a thickness / component of the metal foil including a thickness and a component recalculation step of recalculating the thickness of the metal foil sample using the corrected component and then recalibrating the corrected component using the re-calculated thickness; .
  13. The method according to claim 12, wherein the thickness calculating step is a step of calculating a thickness of the metal foil sample using the following formula (1).
    [Formula 1]
    Figure pat00011

    Where I is the transmitted X-ray intensity, t is the metal foil thickness, and a, b, and c are fitting constants.
  14. 14. The method according to claim 13,
    A step of calculating the component of the metal foil sample using a basic variable method or a multivariate regression equation and then correcting the component using Equation 2 described below in order to improve the accuracy of the calculated component, Method of measuring components.
    [Formula 2]
    Figure pat00012

    Here, X is the post-correction foil component, X 'is the pre-correction foil component, Y is the foil thickness, and a, b, and c are fitting constants.
  15. 15. The method of claim 14,
    In order to improve the precision of the thickness of the metal foil calculated in the above-mentioned [formula 1], the component corrected in the above-mentioned [formula 2] is applied to the following [formula 3], the thickness of the metal foil is recalculated, And recalibrating the corrected component using a thickness of the metal foil.
    [Formula 3]
    Figure pat00013

    Where X is the foil thickness after correction, X 'is the foil thickness before correction, Y is the alloy composition ratio, and a, b, and c are fitting constants.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180073257A (en) 2016-12-22 2018-07-02 주식회사 포스코 Apparatus and method for measuring element of metal sample
KR20190131363A (en) * 2018-05-16 2019-11-26 한국원자력 통제기술원 X-ray analysis system and x-ray analysis method

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JPH11223523A (en) * 1998-02-09 1999-08-17 Toshiba Corp Radiation thickness-measuring apparatus
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JP3323042B2 (en) * 1995-10-24 2002-09-09 株式会社日立製作所 Method and apparatus for measuring three-dimensional element concentration distribution
KR20040072780A (en) 2003-02-11 2004-08-19 삼성전자주식회사 Method for measuring a thickness of a thin layer
JP2010512524A (en) * 2006-12-15 2010-04-22 フラウンホッファー−ゲゼルシャフト ツァ フェルダールング デァ アンゲヴァンテン フォアシュンク エー.ファオ Method and apparatus for thickness measurement

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JP3323042B2 (en) * 1995-10-24 2002-09-09 株式会社日立製作所 Method and apparatus for measuring three-dimensional element concentration distribution
JPH11223523A (en) * 1998-02-09 1999-08-17 Toshiba Corp Radiation thickness-measuring apparatus
JP2000258340A (en) * 1999-03-05 2000-09-22 Horiba Ltd Substance identification apparatus
KR20040072780A (en) 2003-02-11 2004-08-19 삼성전자주식회사 Method for measuring a thickness of a thin layer
JP2010512524A (en) * 2006-12-15 2010-04-22 フラウンホッファー−ゲゼルシャフト ツァ フェルダールング デァ アンゲヴァンテン フォアシュンク エー.ファオ Method and apparatus for thickness measurement

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180073257A (en) 2016-12-22 2018-07-02 주식회사 포스코 Apparatus and method for measuring element of metal sample
KR20190131363A (en) * 2018-05-16 2019-11-26 한국원자력 통제기술원 X-ray analysis system and x-ray analysis method

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