WO2007078088A1 - Method for processing and analyzing data of synchrotron grazing incidence x-ray scattering apparatus - Google Patents
Method for processing and analyzing data of synchrotron grazing incidence x-ray scattering apparatus Download PDFInfo
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- WO2007078088A1 WO2007078088A1 PCT/KR2006/005777 KR2006005777W WO2007078088A1 WO 2007078088 A1 WO2007078088 A1 WO 2007078088A1 KR 2006005777 W KR2006005777 W KR 2006005777W WO 2007078088 A1 WO2007078088 A1 WO 2007078088A1
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- sample
- synchrotron
- thin film
- ray beam
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
Definitions
- the present invention relates to a method for processing and analyzing data
- Synchrotron radiation sources especially an X-ray beam
- a strong scattering intensity may be obtained due to the large scattering volume in the case that the X-ray is incident on the thin film at the critical angle
- the present invention provides a method for processing and analyzing data
- the present invention provides a method for processing
- the present invention provides a method for processing and analyzing data
- the converting may include receiving the two-dimensional scattering data
- the acquiring may include receiving the one-dimensional scattering data
- the model sample by inputting quantitative information on the shape or structure of
- corrected data of the model sample is the same as the one-dimensional scattering data
- the assigning may be returned and repeated until the scattering intensity from the model sample is not the same as the scattering intensity from the sample.
- the scattering intensity from the model sample matches the scattering intensity from
- the variables may include coordinates of a synchrotron X-ray beam that
- the shape of the model sample may be selected from a sphere, a circular
- the structure of the model sample may be selected from a multi-layered
- the correcting may include obtaining a transmittance and a reflectance of
- Fig. 1 is a schematic diagram of a synchrotron grazing incidence X-ray scattering
- Fig. 2 is a perspective view showing an incident X-ray being scattered from the
- Fig. 3 is a flow chart showing procedures for processing and analyzing the data
- Fig. 4 is a flow chart schematically showing procedures for processing the data
- Fig. 5 is a flow chart schematically showing procedures for analyzing the data of
- sample mounting section 101 sample chamber
- sample 110 sample control section
- goniometer 112 goniometer drive
- goniometer controller 114 stepping motor 115 : stepping motor drive 116 : stepping motor controller
- liquid nitrogen injector 125 liquid nitrogen circulating tube
- main control section 140 signal detector
- stepping motor driving section 301 incident synchrotron X-ray beam
- Fig. 1 is a schematic diagram of a synchrotron grazing incidence X-ray
- apparatus includes a sample mounting section 100 where a thin film sample to be analyzed is located and the thin film reacts with incident synchrotron X-ray beams to
- a signal detector 140 that detects the
- processing/analyzing section 150 that is connected with the signal detector 140 and
- synchrotron X-ray beam is incident on a thin film sample at the critical angle thereof
- the synchrotron X-ray beam is generated by a synchrotron and is
- the sample mounting section 100 includes a sample chamber 101, a sample stage 102 that is placed inside the sample chamber 101 and where the sample is
- the sample chamber 101 is a device that generates scattering from the
- the sample chamber 101 is kept under vacuum.
- the window of the sample chamber 101 is preferably made of a
- synchrotron X-ray beam and the scattering signals are able to transmit to the sample
- the vacuum pump 103 is connected with the sample chamber 101 and
- the sample stage 102 is a place where the sample from which the incident
- synchrotron X-ray beam is scattered is located, and is placed inside the sample
- the sample stage 102 is preferably made of aluminum for its
- Fig. 2 is a perspective view showing that the incident X-ray is scattered from
- ray beam is divided into a horizontal scattering angle 303 and a vertical scattering
- the data processing/analyzing section 150 processes and analyzes the
- the accurate scattering signals 302 may be produced because the inclination
- the sample control section 110 includes a goniometer driving section 200
- the goniometer driving section 200 for precisely controlling the incident angle of the incident synchrotron X-ray beam 301 on the sample 104 includes the
- a goniometer drive 112 that drives the goniometer 111
- the goniometer 111 can be moved up and down (in the Z direction of the
- the goniometer driving section 200 adjusts the incident angle of the
- the goniometer controller 113 serves to deliver control commands to the
- goniometer 111 through the goniometer drive 112 and serves to display the control
- the stepping motor driving section 210 includes a stepping motor 114 that is
- a stepping motor drive 115 that drives the stepping motor 114, and a
- stepping motor controller 116 that imposes control signals on the stepping motor
- the stepping motor controller 116 serves to deliver control commands to the
- the temperature control section 120 includes a temperature adjuster 121 that
- liquid nitrogen circulating tube 125 that transports the liquid nitrogen to the sample
- the temperature control section 120 for controlling the temperature of the
- sample stage 102 is provided with the programmable temperature adjuster 121 and is
- the heating bar 123 is a conventional device, having an electrical resistance
- the heating bar 123 is embedded in the sample stage 102.
- the temperature adjuster 121 is connected to the temperature controller 122 via an RS232 port and
- the liquid nitrogen injector 124 serves to cool down the sample stage using
- liquid nitrogen The liquid nitrogen circulating tube extends into the inside of the
- sample stage 102 and circulates the liquid nitrogen through the sample stage 102,
- temperature control section 120 is able to control the temperature of the sample stage
- the data processing/analyzing section 150 is
- the data processing/analyzing procedure consists of a series of the
- sample includes converting two-dimensional scattering data from a thin film sample
- the synchrotron X-ray beam that passed through the beam line generates a
- the signals are captured as two-dimensional scattering data by the two-dimensional
- two-dimensional scattering data include a distortion phenomenon that results from
- processing/analyzing section 150 obtains the one-dimensional scattering data at a
- the data processing/analyzing section 150 obtains quantitative information
- Fig. 3 is a schematic flow chart showing procedures for processing the data
- the data processing procedure includes receiving the two-dimensional
- the data processing/analyzing section 150 reads the file of the two-
- the data acquired by the signal detector 140 are accepted as a multi-dimensional
- the scattering angle is calculated from the experimental variables by the
- a f ao ⁇ sir.( ⁇ Aar.(-FY+ CHJFIR (2)) ⁇ ⁇ D ; ⁇ hSize) 2 - J[PX - CEMER (I)) ] )) - a f
- the scattering intensity for a specific angle can be calculated by
- the data processing/analyzing section 150 obtains the
- the data processing/analyzing section 150 reads, loads, and displays the
- the shape of the model sample can be selected from the predetermined various models such as a sphere, a circular cylinder, a circular cone, a pyramid, a
- the structure of the model sample can be selected from the
- predetermined various models such as a multi-layered structure, a hexagonal
- perforated layer structure a hexagonal packed structure, etc.
- the scattering intensity (Ij) is calculated from the form factor (F(q)) and the
- the scattering intensity (I 1 ) does not consider the distortion in the
- the multi-layered thin film such as electron density, absorption coefficient, and thickness of the thin film and the substrate (S250).
- the scattering intensity obtained from the model sample is corrected by the
- Tj and Rj are the transmittance and the reflectance of the
- T f and R f are the
- q n and q z are the scattering vectors in which the wavelength of the
- the vector q z can be distinguished
- layered thin film can be represented by q 1>z , q 2 , z , q 3>z , and q 4jZ .
- IGIXS(independent) is always positive, but IGIXS(C ⁇ OSS) may be positive or negative,
- the sample the size of the structure, the divergence of the incident beam, etc.
- Equation (4) is in the following
- the data processing/analyzing section 150 displays the scattering intensity
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
In order to correct scattering data obtained from synchrotron grazing incidence X-ray scattering apparatus on a thin film sample and to accurately analyze them, the present invention provides a method for processing and analyzing data of a synchrotron grazing incidence X-ray scattering apparatus, the method including converting two-dimensional scattering data on a thin film sample, that are obtained from a signal detector of the synchrotron grazing incidence X-ray scattering apparatus, into one-dimensional scattering data for a specific scattering angle, and acquiring quantitative information on the internal structure of the thin film sample and the surface thereof with respect to a specific direction by comparing and analyzing the one-dimensional scattering data.
Description
TITLE OF THE INVENTION
Method for Processing and Analyzing Data of Synchrotron Grazing
Incidence X-ray Scattering Apparatus
Field of the invention
The present invention relates to a method for processing and analyzing data
of a synchrotron grazing incidence X-ray scattering apparatus, and more particularly,
to a method for properly processing and accurately analyzing data obtained
therefrom on a thin film sample.
Background art
Synchrotron radiation sources, especially an X-ray beam, provide
information on microstructure that is not obtained by visible light, so an X-ray
scattering method is one of the major tools for analysis on polymer structure.
However, for a thin film sample with a thickness of less than 1 μm, the
previous transmission X-ray scattering method is not suitable for structural analysis.
It is not possible to obtain strong scattering intensity due to the small
scattering volume of the thin film, and in addition, an X-ray having enough energy to
penetrate the substrate as well as the thin film is required due to the thin film formed
on the substrate that is opaque to the X-ray.
A strong scattering intensity may be obtained due to the large scattering
volume in the case that the X-ray is incident on the thin film at the critical angle,
however this method has a shortcoming in that the scattering signals may be distorted
by refraction and reflection of the incident X-ray beam.
DETAILED DESCRIPTION OF THE INVENTION
Technical objectives
The present invention provides a method for processing and analyzing data
from a synchrotron grazing incidence X-ray scattering apparatus that is capable of
correcting the distortion of the scattering data from a thin film sample.
In addition, the present invention provides a method for processing and
analyzing data from a synchrotron grazing incidence X-ray scattering apparatus that
is capable of accurately analyzing the scattering data on a thin film sample.
Technical solution
The present invention provides a method for processing and analyzing data
from a synchrotron grazing incidence X-ray scattering apparatus, the method
including converting two-dimensional scattering data from a thin film sample that are
obtained from a signal detector of the synchrotron grazing incidence X-ray scattering
apparatus into one-dimensional scattering data for a specific scattering angle, and
acquiring quantitative information on internal structure of the thin film sample and
the surface thereof with respect to a specific direction by comparing and analyzing
the one-dimensional scattering data.
The converting may include receiving the two-dimensional scattering data
from the signal detector, and converting the two-dimensional scattering data into the
one-dimensional scattering data by having experimental conditions for the sample as
variables.
The acquiring may include receiving the one-dimensional scattering data
obtained during the converting, assigning shapes or structures to a model sample that
is to be compared with the sample, calculating a form factor and a structure factor of
the model sample by inputting quantitative information on the shape or structure of
the model sample, calculating scattering intensity of the model sample from the form
factor and the structure factor, correcting the scattering intensity, and checking if the
corrected data of the model sample is the same as the one-dimensional scattering data
obtained during the converting, by comparing the two data.
If the scattering intensity from the model sample is the same as the scattering
intensity from the sample, the information on the shape and structure of the model
sample, characteristic information, and the calculated one-dimensional data as the
information on the sample may be saved.
If the scattering intensity from the model sample is not the same as the
scattering intensity from the sample, the assigning may be returned and repeated until
the scattering intensity from the model sample matches the scattering intensity from
the sample.
The variables may include coordinates of a synchrotron X-ray beam that
transmits through the sample and is detected by the signal detector, an incident angle
of the synchrotron X-ray beam, a distance between the sample and the signal detector,
pixel size of the signal detector, and coordinates of the scattering angle.
The shape of the model sample may be selected from a sphere, a circular
cylinder, a circular cone, a pyramid, and a prism.
The structure of the model sample may be selected from a multi-layered
structure, a hexagonal packed structure, and a hexagonal perforated layer structure.
The correcting may include obtaining a transmittance and a reflectance of
the synchrotron X-ray beam from information on electron density of a thin film and
of a substrate, absorption coefficient, and thickness of the thin film, and correcting a
refraction and a reflection of the incident synchrotron X-ray beam.
Effect of the invention
According to the present invention, it is possible to accurately analyze the
internal structural shape of a thin film sample and the surface thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a schematic diagram of a synchrotron grazing incidence X-ray scattering
apparatus according to the embodiment of the present invention.
Fig. 2 is a perspective view showing an incident X-ray being scattered from the
sample.
Fig. 3 is a flow chart showing procedures for processing and analyzing the data
of the synchrotron grazing incidence X-ray scattering apparatus according to the
embodiment of the present invention.
Fig. 4 is a flow chart schematically showing procedures for processing the data
of the synchrotron grazing incidence X-ray scattering apparatus according to the
embodiment of the present invention.
Fig. 5 is a flow chart schematically showing procedures for analyzing the data of
the synchrotron grazing incidence X-ray scattering apparatus according to the
embodiment of the present invention.
<Reference numerals for main components in the drawings >
100 : sample mounting section 101 : sample chamber
102 : sample stage 103 : vacuum pump
104 : sample 110 : sample control section
111 : goniometer 112 : goniometer drive
113 : goniometer controller 114 : stepping motor
115 : stepping motor drive 116 : stepping motor controller
120 : temperature control section 121 : temperature adjuster
122 : temperature controller 123 : heating bar
124 : liquid nitrogen injector 125 : liquid nitrogen circulating tube
130 : main control section 140 : signal detector
150 : data processing and analyzing section
200 : goniometer driving section
210 : stepping motor driving section 301 : incident synchrotron X-ray beam
302 : scattering signal 303 : horizontal scattering angle
304 : vertical scattering angle
DETAILED DESCRIPTION OF THE EMBODIMENTS
Hereinafter, with reference to appended drawings, the embodiments of the
present invention will be described in detail for enabling those skilled in the art.
However, the present invention may have different forms and is not limited to these
embodiments.
Fig. 1 is a schematic diagram of a synchrotron grazing incidence X-ray
scattering apparatus according to an embodiment of the present invention.
Referring to Fig. 1, the synchrotron grazing incidence X-ray scattering
apparatus includes a sample mounting section 100 where a thin film sample to be
analyzed is located and the thin film reacts with incident synchrotron X-ray beams to
be scattered so as to produce scattering signals; a sample control section 110 that
controls the incident angle of the synchrotron X-ray beam and the position of the
sample mounting section 100 with respect to the synchrotron X-ray beam so as to
control the scattering from the sample mounting section 100; a temperature control
section 120 that controls rise and drop in temperature of the sample mounting section
100; a main control section that conveys control commands to the sample control
section 110 and to the temperature control section 120, and restores and displays the
control commands and results thereof; a signal detector 140 that detects the
scattering signals from the sample mounting section 100; and a data
processing/analyzing section 150 that is connected with the signal detector 140 and
processes and analyzes the detected signals.
Hereinafter, the term "synchrotron grazing incidence" is defined such that a
synchrotron X-ray beam is incident on a thin film sample at the critical angle thereof
in order to graze the thin film sample.
Here, the synchrotron X-ray beam is generated by a synchrotron and is
preferably an X-ray that provides information on the molecular structure of the
sample by reacting with the sample and being scattered.
The sample mounting section 100 includes a sample chamber 101, a sample
stage 102 that is placed inside the sample chamber 101 and where the sample is
mounted, and a vacuum pump 103 that keeps the sample chamber 101 under vacuum.
The sample chamber 101 is a device that generates scattering from the
surface of the sample by the incident synchrotron X-ray beam thereon. However,
since the scattering signal of the synchrotron X-ray beam weakens in intensity due to
the scattering with the air, the sample chamber 101 is kept under vacuum.
In addition, the window of the sample chamber 101 is preferably made of a
polymer film such that the sample chamber 101 is maintained under vacuum and the
synchrotron X-ray beam and the scattering signals are able to transmit to the sample
chamber 101.
The vacuum pump 103 is connected with the sample chamber 101 and
maintains the vacuum state of the sample chamber 101.
The sample stage 102 is a place where the sample from which the incident
synchrotron X-ray beam is scattered is located, and is placed inside the sample
chamber 101. The sample stage 102 is preferably made of aluminum for its
excellent heat transfer characteristics and non-deformability at high and low
temperature.
Fig. 2 is a perspective view showing that the incident X-ray is scattered from
the sample.
Referring to Fig. 2, the incident synchrotron X-ray beam 301 that has passed
through the beam line enters the sample mounting section 100 and is scattered from
the surface of the sample 104. The scattering angle of the scattered synchrotron X-
ray beam is divided into a horizontal scattering angle 303 and a vertical scattering
angle 304.
The data processing/analyzing section 150 processes and analyzes the
scattering signals detected by the signal detector 140, and derives quantitative
information on the sample 104 such as the internal structure thereof.
The accurate scattering signals 302 may be produced because the inclination
(an inclining angle to the Y-Z plane of the drawing) of the sample stage 102 can be
corrected by operation of the sample control section 110 that is connected with the
sample mounting section 100.
The sample control section 110 includes a goniometer driving section 200
that adjusts an incident angle of the incident synchrotron X-ray beam 301 by
precisely rotating the sample mounting section 100 about the center axis (an axis
parallel to the Y direction of the drawing) of the goniometer 111, and a stepping
motor driving section 210 that moves the sample mounting section 100 up and down
(in the Z direction of the drawing).
The goniometer driving section 200 for precisely controlling the incident
angle of the incident synchrotron X-ray beam 301 on the sample 104 includes the
goniometer 111 that is connected with and rotates the sample mounting section 100,
a goniometer drive 112 that drives the goniometer 111, and a goniometer controller
113 that is connected with the goniometer drive 112 and imposes control commands
thereon.
The goniometer 111 can be moved up and down (in the Z direction of the
drawing) by a stepping motor 111 that is directly connected thereto.
Fulfilling the control command of the angle adjustment on a scale as small as
0.001 degrees, the goniometer driving section 200 adjusts the incident angle of the
incident synchrotron X-ray beam 301 by rotating the sample mounting section 100
about the center axis of the goniometer 111.
The goniometer controller 113 serves to deliver control commands to the
goniometer 111 through the goniometer drive 112 and serves to display the control
results.
The stepping motor driving section 210 includes a stepping motor 114 that is
connected with the goniometer 111 and moves the sample mounting section 100 up
and down, a stepping motor drive 115 that drives the stepping motor 114, and a
stepping motor controller 116 that imposes control signals on the stepping motor
drive 115.
The stepping motor controller 116 serves to deliver control commands to the
stepping motor 114 through the stepping motor drive 115 and serves to display the
control results.
The temperature control section 120 includes a temperature adjuster 121 that
adjusts the temperature of the sample stage 102, a temperature controller 122 that
controls the temperature adjuster 121, a heating bar 123 that supplies heat to the
sample stage 102 under the control of the temperature adjuster 121, a liquid nitrogen
injector 124 that supplies liquid nitrogen for cooling the sample stage 102, and a
liquid nitrogen circulating tube 125 that transports the liquid nitrogen to the sample
stage 102.
The temperature control section 120 for controlling the temperature of the
sample stage 102 is provided with the programmable temperature adjuster 121 and is
capable of maintaining the sample stage 102 at a constant temperature in the range of
room temperature to 450 °C or raising the temperature of the sample stage 102 at a
desired rate.
The heating bar 123 is a conventional device, having an electrical resistance
wire and an insulator, which is electrically connected to the temperature control
section 120 and is heated with a supplied electrical current.
The heating bar 123 is embedded in the sample stage 102. The temperature
adjuster 121 is connected to the temperature controller 122 via an RS232 port and
receives the control command.
The liquid nitrogen injector 124 serves to cool down the sample stage using
liquid nitrogen. The liquid nitrogen circulating tube extends into the inside of the
sample stage 102 and circulates the liquid nitrogen through the sample stage 102,
lowering the temperature of the sample stage 102 to below -80 °C. Thus, the
temperature control section 120 is able to control the temperature of the sample stage
102 in the range of -80 to 1000 °C and to provide a circumstance suitable for
observing the change of the structure of a temperature-dependent sample.
In the present embodiment, the data processing/analyzing section 150 is
realized with a program installed in a computer, and Figs. 3 to 5 exemplify the
procedures for processing and analyzing data through the data processing and
analyzing section.
Here, the data processing/analyzing procedure consists of a series of the
programs that are programmed with computer-readable codes or commands, and
enables the computer to function as the data processing/analyzing section.
According to the embodiment of the present program, the embodiment for
the analyzing process by the aforementioned data processing/analyzing section is
easily realized in a way in which the program is read by the computer from recording
media such as a ROM, CD-ROM, DVD-ROM, and hard disk, and is executed
thereby, or in which the program is executed after being down-loaded to the
computer through communicating means.
Referring to Fig. 3, the data processing/analyzing procedure for a thin film
sample includes converting two-dimensional scattering data from a thin film sample,
which are obtained from a signal detector of the synchrotron grazing incidence X-ray
scattering apparatus, into one-dimensional scattering data for a specific scattering
angle, and acquiring quantitative information on internal structure of the thin film
sample and the surface thereof with respect to a specific direction by comparing and
analyzing the one-dimensional scattering data.
The synchrotron X-ray beam that passed through the beam line generates a
specific scattering pattern by reacting with a thin film sample, the structure of which
is to be analyzed.
The signals are captured as two-dimensional scattering data by the two-
dimensional signal detector that is placed in the signal detecting section. Since the
two-dimensional scattering data include a distortion phenomenon that results from
the refraction and reflection of the incident synchrotron X-ray beam, the data
processing/analyzing section 150 obtains the one-dimensional scattering data at a
specific scattering angle by considering the scattering structure of the two-
dimensional scattering data from the signal detector (SlOO).
The data processing/analyzing section 150 obtains quantitative information
on the internal and surface structures of the thin film sample by comparing and
analyzing the scattering data of the assigned model sample to the calculated
scattering data (S200).
Fig. 3 is a schematic flow chart showing procedures for processing the data
by the data processing and analyzing section, and one-dimensional scattering data at
a specific scattering angle is obtained from two-dimensional scattering data obtained
by the signal detector.
The data processing procedure includes receiving the two-dimensional
scattering data from the signal detector of the synchrotron grazing incidence X-ray
scattering apparatus, and calculating the two-dimensional scattering data into the
one-dimensional scattering data by having experimental conditions for the sample for
the synchrotron X-ray beam scattering experiment, and outputting and storing the
calculated one-dimensional scattering data.
The data processing/analyzing section 150 reads the file of the two-
dimensional scattering data acquired by the two-dimensional signal detector 140.
The data acquired by the signal detector 140 are accepted as a multi-dimensional
matrix that matches the number of data pixels (Sl 10).
Next, a specific scattering angle at each coordinate is calculated from the
experimental variables for the thin film sample used in the scattering experiments,
and the scattering intensity at the specific angle is finally obtained (S 120).
The scattering angle is calculated from the experimental variables by the
following equations.
20, = atmι(sm(aicm(PX - CENTER)(I)) ÷ (SDDx PxSize)))
(i)
a f = aoπ{sir.(<Aar.(-FY+ CHJFIR (2)) ÷ φϋD ;< hSize)2 - J[PX - CEMER (I)) ] )) - af
(2)
In the above equations, SDD, CENTER(1, 2), Q, PxSize, PX, and PY are the
variables for the experimental conditions of the thin film sample to be inputted to the
above equation, and respectively represent a distance between the thin film sample
and the signal detector (SDD), coordinates of the transmitted incident synchrotron X-
ray beam that is detected by the signal detector (CENTER(1, 2)), incident angle of the
synchrotron X-ray beam (Cj), the size of the pixel in the signal detector (PxSize), and
coordinates of the data for a specific scattering angle (PX, PY).
Therefore, if the experimental variables including the coordinates (PX or
PY) of the data for a specific scattering angle to be analyzed are inputted into
Equations (1) and (2), one-dimensional scattering data at the coordinate for the
scattering angle (2Cj) along the X or Y direction (horizontal direction) and the
scattering angle (Q) along the Z direction (vertical direction) are obtained.
The one-dimensional scattering data obtained in the above procedure are
displayed on a computer screen and stored in the ASCII file format via the displaying
and storing, wherein X and Y coordinates of the stored file are the scattering angle
and the scattering intensity, respectively (S 130).
Thus, the scattering intensity for a specific angle can be calculated by
obtaining the one-dimensional scattering data for a specific angle from the two-
dimensional scattering data.
In the next procedure, the data processing/analyzing section 150 obtains the
quantitative information on the internal structure of the thin film sample and the
surface thereof by comparing and analyzing the scattering intensity obtained in the
data processing procedure (S200).
Referring to Fig. 5, the data analyzing procedure is explained as follows.
The data processing/analyzing section 150 reads, loads, and displays the
one-dimensional scattering data in the ASCII file format, which are obtained in the
data processing procedure (S210).
Further, the shape and structure of the model sample are assigned so as to be
compared with the thin film sample that is to be analyzed (S210).
The shape of the model sample can be selected from the predetermined
various models such as a sphere, a circular cylinder, a circular cone, a pyramid, a
prism, etc. The structure of the model sample can be selected from the
predetermined various models such as a multi-layered structure, a hexagonal
perforated layer structure, a hexagonal packed structure, etc.
Once a shape and a structure of the model sample are determined through the
above procedure, quantitative information on the selected shape or structure, such as
diameter, length of a side, and a distance between the layers, are inputted. The form
factor (F(q)) of the thin film sample is calculated using the information on the shape,
and the structure factor (S(q)) is calculated using the information on the structure.
Then, the scattering intensity (Ij) is calculated from the form factor (F(q)) and the
structure factor (S(q)) with the following Equation (3) (S230 ~ S240).
Ii(q) = S(q)-F(q) (3)
Here, the scattering intensity (I1) does not consider the distortion in the
scattering phenomenon due to the reflection and refraction of the synchrotron X-ray
beam in the multi-layered structure of the thin film and the substrate.
Therefore, there is a procedure for compensating for the refraction and
reflection of the synchrotron X-ray beam by the transmittance (T) and the reflectance
(R) of the synchrotron X-ray beam obtained using the characteristic information on
the multi-layered thin film such as electron density, absorption coefficient, and
thickness of the thin film and the substrate (S250).
The scattering intensity obtained from the model sample is corrected by the
following Equation (4).
incident synchrotron X-ray beam on the thin film, respectively, and Tf and Rf are the
transmittance and the reflectance of the synchrotron X-ray beam reflecting on the
substrate of the thin film, respectively.
Further, q n and qz are the scattering vectors in which the wavelength of the
incident synchrotron X-ray beam is considered. The vector qz can be distinguished
into four different scattering vectors with respect to the relative positions of the
incident synchrotron X-ray beam and the thin film and the substrate in the multi-
layered thin film, and can be represented by q1>z, q2,z, q3>z, and q4jZ.
When the squared term in the right-hand side of the equation (4) is arranged
properly, the squared term can be represented by the summation (iGixs(independent)) of
each of small squared terms and the summation (IGIXS(CΓOSS)) of each term multiplied
by other small terms.
iGixs(independent) is always positive, but IGIXS(CΓOSS) may be positive or negative,
depending on the incident angle, the thickness of the sample, the internal structure of
the sample, the size of the structure, the divergence of the incident beam, etc.
However, IGIXS(CΓOSS) is a negligible amount or zero in a statistical view. Therefore,
when the contribution of IGIXS(CTOSS) can be ignored, Equation (4) is in the following
mathematical form.
As stated above, when the scattering intensity of the model sample is
corrected, the data processing/analyzing section 150 displays the scattering intensity
obtained from Equations (3), (4), and (5), and checks by comparison if the scattering
intensity obtained in the data processing procedure for the thin film sample is the
same as the scattering intensity obtained in the data analyzing procedure for the
model sample (S270).
When the finally-obtained scattering intensity from the model sample
matches the scattering intensity from the thin film sample, it is determined that the
shape and structure of the model sample correspond to the shape and structure of the
thin film sample. Thus the information on the shape and structure of the model
sample, characteristic information, and the calculated one-dimensional scattering
data are stored as information on the thin film sample (S280).
In the case that the scattering intensity from the model sample is not the
same as the scattering intensity from the thin film sample in the comparing and
confirming procedure, the procedure where the model sample is assigned is returned
to and repeated until the scattering intensity from the model sample is the same as the
scattering intensity from the thin film sample.
Although an embodiment of the present invention has been described in
detail hereinabove, it should be clearly understood that many variations and/or
modifications of the basic inventive concepts herein taught which may appear to
those skilled in the present art will still fall within the spirit and scope of the present
invention, as defined in the appended claims.
Claims
1. A method for processing and analyzing data from a synchrotron grazing incidence
X-ray scattering apparatus, the method comprising:
converting two-dimensional scattering data from a thin film sample, that are
obtained from a signal detector of the synchrotron grazing incidence X-ray scattering
apparatus, into one-dimensional scattering data for a specific scattering angle; and
acquiring quantitative information on internal structure of the thin film
sample and the surface thereof with respect to a specific direction by comparing and
analyzing the one-dimensional scattering data.
2. The method of claim 1, wherein the converting includes:
receiving the two-dimensional scattering data from the signal detector; and
calculating the two-dimensional scattering data into the one-dimensional
scattering data by having experimental conditions for the sample as variables.
3. The method of claim 1, wherein the acquiring includes:
receiving the one-dimensional scattering data obtained during the
converting;
assigning shapes or structures to a model sample that is to be compared with the sample;
calculating a form factor and a structure factor of the model sample by
inputting quantitative information on the shape or structure of the model sample;
calculating scattering intensity of the model sample from the form factor and
the structure factor;
correcting the scattering intensity; and
checking if the corrected data of the model sample is the same as the one-
dimensional scattering data obtained during the converting, by comparing the two
data.
4. The method of claim 3, further comprising:
saving the information on the shape and structure of the model sample,
characteristic information, and the calculated one-dimensional data as the
information on the sample if the scattering intensity from the model sample is the
same as the scattering intensity from the sample; and
returning to and repeating the assigning until the scattering intensity from the
model sample matches the scattering intensity from the sample if the scattering
intensity from the model sample is not the same as the scattering intensity from the
sample.
5. The method of claim 2, wherein the variables include coordinates of a synchrotron
X-ray beam that transmits through the sample and is detected by the signal detector,
an incident angle of the synchrotron X-ray beam, a distance between the sample and
the signal detector, pixel size of the signal detector, and coordinates of the scattering
angle.
6. The method of claim 3, wherein the shape of the model sample is selected from a
sphere, a circular cylinder, a circular cone, a pyramid, and a prism.
7. The method of claim 3, wherein the structure of the model sample is selected from
a multi-layered structure, a hexagonal packed structure, and a hexagonal perforated
layer structure.
8. The method of claim 3, wherein the compensating includes obtaining a
transmittance and a refractive index of the synchrotron X-ray beam from information
on electron density of a thin film and of a substrate, absorption coefficient, and
thickness of the thin film, and compensating for a refraction and a reflection of the
incident synchrotron X-ray beam.
9. The method of claim 2, wherein the calculating is carried out by the following
Equations (1) and (2):
Wf = aiωι(sin(aian(PX - CIM1M)(I)) ÷ (SDDx PxSizejj)
(1)
ct f = am{sir.{<tar.(-W + CENTER (2))÷(λ/(5DDx ?xto)2 - J[PX - CEMER (I))3)) - αt (2)
wherein 2Q = scattering angle along X or Y direction,
Q- = scattering angle along Z direction,
SDD = distance between the thin film sample and the signal detector,
CENTER(1, 2) = coordinates of the transmitted synchrotron X-ray beam,
Q - incident angle of the synchrotron X-ray beam,
PxSize = pixel size of the signal detector, and
PX and PY = coordinates for a specific scattering angle.
10. The method of claim 3, wherein the compensating is carried out by the following
wherein Tj = transmittance of the incident synchrotron X-ray beam in the
thin film,
Ri = reflectance of the incident synchrotron X-ray beam in the thin film,
Tf = transmittance of the synchrotron X-ray beam that is reflected on the
substrate of the thin film,
Rf = reflectance of the synchrotron X-ray beam that is reflected on the
substrate of the thin film, and
q Ii and qz = scattering vectors, considering the wavelength of the incident
synchrotron X-ray beam, wherein
qi,z, q2,z> q3,z and q4jZ = four different scattering vectors that are
distinguishable according to the incident synchrotron X-ray beam and positional
relationship between the thin film and the substrate in the multi-layered thin film.
11. The method of claim 3, wherein the compensating is carried out by the following
Equation (5): Iaxsfrf&fϊ ≡
thin film,
Ri = reflectance of the incident synchrotron X-ray beam in the thin film,
Tf = transmittance of the synchrotron X-ray beam that is reflected on the
substrate of the thin film,
Rf = reflectance of the synchrotron X-ray beam that is reflected on the
substrate of the thin film, and
q ii and qz = scattering vectors, considering the wavelength of the incident
synchrotron X-ray beam, wherein
qi,z> q2,z, q3,z, and q4,z = four different scattering vectors that are
distinguishable according to the incident synchrotron X-ray beam and positional
relationship between the thin film and the substrate.
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Cited By (1)
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CN106769479A (en) * | 2017-02-09 | 2017-05-31 | 中国科学技术大学 | Supper-fast stretching device and its experimental technique associated with a kind of scattering of and X-ray |
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US5991035A (en) * | 1996-10-17 | 1999-11-23 | Tropel Corporation | Interferometric method of measuring toric surfaces at grazing incidence |
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CN106769479A (en) * | 2017-02-09 | 2017-05-31 | 中国科学技术大学 | Supper-fast stretching device and its experimental technique associated with a kind of scattering of and X-ray |
CN106769479B (en) * | 2017-02-09 | 2023-04-28 | 中国科学技术大学 | Ultra-fast stretching device combined with X-ray scattering and experimental method thereof |
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