WO2021029519A1 - Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur - Google Patents

Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur Download PDF

Info

Publication number
WO2021029519A1
WO2021029519A1 PCT/KR2020/006544 KR2020006544W WO2021029519A1 WO 2021029519 A1 WO2021029519 A1 WO 2021029519A1 KR 2020006544 W KR2020006544 W KR 2020006544W WO 2021029519 A1 WO2021029519 A1 WO 2021029519A1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
crystal structure
candidate group
interplanar
angle
Prior art date
Application number
PCT/KR2020/006544
Other languages
English (en)
Korean (ko)
Inventor
강성
허윤
홍기정
Original Assignee
재단법인 포항산업과학연구원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 재단법인 포항산업과학연구원 filed Critical 재단법인 포항산업과학연구원
Publication of WO2021029519A1 publication Critical patent/WO2021029519A1/fr

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/4788—Diffraction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • 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
    • G01N23/2055—Analysing diffraction patterns
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
    • G06T7/00—Image analysis
    • G06T7/70—Determining position or orientation of objects or cameras
    • G06T7/73—Determining position or orientation of objects or cameras using feature-based methods
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
    • G06T7/00—Image analysis
    • G06T7/70—Determining position or orientation of objects or cameras
    • G06T7/73—Determining position or orientation of objects or cameras using feature-based methods
    • G06T7/74—Determining position or orientation of objects or cameras using feature-based methods involving reference images or patches
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction

Definitions

  • the present application relates to an apparatus and method for analyzing a crystal structure of a sample, and a computer-readable recording medium.
  • the various properties of materials depend on the type and arrangement of the microstructured atoms, and the type and arrangement of these atoms can be observed with an electron microscope.
  • Electron microscopy can observe various defects and interfaces such as crystal shape and size, dislocation in crystal, stacking faults, etc. with much better resolution and magnification than optical microscopy, and X-ray diffraction (diffraction) ), it is possible to observe its crystallinity, lattice arrangement, and symmetry as electron diffraction in a much smaller nano-unit region than can be analyzed in ).
  • an apparatus a method for analyzing a crystal structure of a sample, and a computer-readable recording medium capable of analyzing an accurate crystal structure while reducing the time required for crystal structure analysis.
  • a measurement module for measuring an interplanar distance and an interplanar angle from a diffraction pattern (DP) image of a sample
  • a primary candidate group selection module for selecting a primary candidate group having crystal structures corresponding to the component information of the sample by referring to a database when component information of a sample is input
  • a second candidate group selection module configured to select, as a second candidate group, crystal structures having an interplanar distance matching the measured interplanar distance among crystal structures included in the selected first candidate group by referring to the database
  • a determination module configured to determine the crystal structure of the sample based on a surface index having an interplanar angle matching the measured interplanar angle among the crystal structures included in the selected secondary candidate group by referring to the database.
  • the first step of measuring the interplanar distance and the interplanar angle from the diffraction pattern (DP) image of the sample, and in the first candidate group selection module, the component information of the sample is When input, a second step of selecting a primary candidate group having crystal structures corresponding to the component information of the sample by referring to a database, and in a secondary candidate group selection module, the selected primary candidate group by referring to the database A third step of selecting crystal structures having an interplanar distance matching the measured interplanar distance among the included crystal structures as a second candidate group, and in a decision module, including in the selected second candidate group by referring to the database
  • a method for analyzing a crystal structure of a sample is provided, including a fourth step of determining a crystal structure of the sample based on a surface index having an interplanar angle matched with the measured interplanar angle among the determined crystal structures.
  • a computer-readable recording medium in which a program for executing the above-described sample crystal structure analysis method on a computer is recorded.
  • a sample by comparing the interplanar distance and the interplanar angle measured from the diffraction pattern image of the sample using the interplanar distance for each crystal structure stored in the database and a plane index that satisfies the interplanar distance.
  • FIG. 1 is a block diagram of an apparatus for analyzing a crystal structure of a sample according to an embodiment of the present invention.
  • FIG. 2 is a diagram illustrating a process of measuring an inter-planar distance and an inter-planar angle in a measurement module according to an embodiment of the present invention.
  • 3A to 3B are diagrams for explaining a process of correcting a diffraction pattern image according to an embodiment of the present invention.
  • FIG. 4 is a flowchart illustrating a method of analyzing a crystal structure of a sample according to an embodiment of the present invention.
  • FIG. 1 is a block diagram of an apparatus for analyzing a crystal structure of a sample according to an embodiment of the present invention.
  • FIG. 2 is a diagram illustrating a process of measuring an interplanar distance and an interplanar angle in a measurement module according to an embodiment of the present invention.
  • FIGS. 3A to 3B are diagrams for explaining a process of correcting a diffraction pattern image according to an embodiment of the present invention.
  • the apparatus 100 for analyzing a crystal structure of a sample includes a measurement module 110, a first candidate group selection module 120, a second candidate group selection module 130, a determination module 140, and It may be configured to include a database 150.
  • the measurement module 110 may measure an interplanar distance and an interplanar angle from a diffraction pattern (DP) image of the sample.
  • DP diffraction pattern
  • the diffraction pattern image of the sample can be obtained from an electron microscope, not shown.
  • the measured interplanar distance is the first interplanar distance between the two spots included in the vector in the first direction from an arbitrary origin in the diffraction pattern image to the first nearest spot, and the second closest from any origin in the diffraction pattern image.
  • the second interplanar distance between the two spots included in the vector in the second direction to the spot, and the third plane between the two spots included in the vector in the third direction, which is the sum of the vector in the first direction and the vector in the second direction. May include distance.
  • the measured interplanar angle may include a first interplanar angle between a vector in a first direction and a vector in a second direction, and a second interplanar angle between a vector in a second direction and a vector in a third direction.
  • FIG. 2 illustrates a process of measuring an interplanar distance and an interplanar angle in a measurement module according to an embodiment of the present invention.
  • the measurement module 110 includes two spots included in the vector in the first direction R1 from an arbitrary origin (O) in the input diffraction pattern image to the first nearest spot P1.
  • the distance between two spots included in the vector in the third direction R3 (passing through the spot P3), which is the sum of the vector in the first direction R1 and the vector in the second direction R2, may be included. have.
  • the first interplanar distance in the R1 direction measured in FIG. 2 is 0.4788 nm
  • the second interplanar distance in the R2 direction is 0.1455 nm
  • the third interplanar distance in the R3 direction is 0.138 nm.
  • the measurement module 110 includes a first interplanar angle between the vector in the first direction R1 and the vector in the second direction R2, and between the vector in the second direction R2 and the vector in the third direction R3. You can measure the angle between the second plane of
  • the measurement module 110 described above is, for each of the first direction, the second direction, and the third direction centering on an arbitrary origin (O) of the input diffraction pattern image.
  • a preprocessing process of correcting spots existing in the direction at equal intervals may be further performed.
  • the distance between spots in the diffraction pattern image when looked at, the distance between spots decreases from the center to the outside, so the value of the inter-planar distance varies according to the location to be measured.
  • the present invention by correcting the diffraction pattern image through the above-described pre-processing, even if the distance between any two spots existing in a specific direction is measured, there is an advantage that the distance between the planes in the corresponding direction can be set.
  • the average value between the spots is calculated by dividing the total distance including all spots in the R1 direction by the number of spots in the R1 direction (exactly the number of spots-1), and an arbitrary origin (O) is centered.
  • O an arbitrary origin
  • the diffraction pattern image may be corrected through a method as shown in FIG. 3A.
  • the diffraction pattern image may be corrected through a correction process as shown in FIG. 3B.
  • a straight line from an arbitrary reference spot to the center point coordinates of all spots is drawn (straight lines 1 to 5 are exemplarily shown) (the opposite side of the same straight line Spots are excluded).
  • spots included in a certain area range on a straight line are grouped (lattice dot grouping).
  • a regression line is derived through regression analysis for the grouped spots, and the coordinate points of the spots are moved by the derived regression line, and then rearranged. I can.
  • the primary candidate group selection module 120 may refer to the database 150 to select a primary candidate group having crystal structures corresponding to the component information of the sample.
  • the component information may include Fe and O.
  • the primary candidate group selection module 120 may select a crystal structure corresponding to the component ratio in addition to the component information as the primary candidate group.
  • the above-described component information and component ratio can be obtained from an EDS (Enegery Dispresive X-Ray Sepctrometer) component analyzer attached to an electron microscope (not shown). If the sample is Fe 2 O 3 , the component ratio may include 2 mol of Fe and 3 mol of O.
  • EDS Enegery Dispresive X-Ray Sepctrometer
  • the second candidate group selection module 130 refers to the database 150 and selects a crystal structure having an interplanar distance matching the measured interplanar distance among the crystal structures included in the selected first candidate group as the second candidate group. I can.
  • the second candidate group selection module 130 may determine that the difference between the measured interplanar distance and the interplanar distance of the crystal structure included in the selected first candidate group is less than ⁇ 5%. It should be noted that specific values for determining the degree of matching described above are for aiding understanding of the present invention, and the present invention is not limited to specific values.
  • the determination module 140 refers to the database 150 to determine a crystal structure having an interplanar angle matching the measured interplanar angle among the crystal structures included in the selected secondary candidate group as the crystal structure of the sample. I can.
  • the determination module 140 may determine that an error between the measured interplanar angle and the interplanar angle of the crystal structure included in the selected secondary candidate group is less than ⁇ 5%. It should be noted that specific values for determining the degree of matching described above are for aiding understanding of the present invention, and the present invention is not limited to specific values.
  • the determination module 140 calculates an inter-planar angle from the surface index used for calculating the inter-planar distance among the surface indices of the crystal structure included in the selected secondary candidate group, and compares the calculated inter-planar angle with the measured inter-planar angle. After that, a surface index matching the measured interplanar angle may be determined, and a crystal structure having the determined surface index may be determined as the crystal structure of the sample by referring to the database 150.
  • an inter-planar angle is further considered in addition to the inter-planar distance for crystal structure analysis. Since the inter-planar distance may be the same even when the crystal structure has different crystal structures, an accurate crystal structure is determined by considering the inter-planar angle. This is for analysis.
  • various crystal structures according to component information and component ratios, and crystal structure information including lattice constants, plane indices, and inter-planar distances for each crystal structure may be stored in advance.
  • the interplanar distance and the interplanar angle measured from the diffraction pattern image of the sample are obtained by using the interplanar distance for each crystal structure stored in the database and a plane index that satisfies the interplanar distance.
  • FIG. 4 is a flowchart illustrating a method of analyzing a crystal structure of a sample according to an embodiment of the present invention.
  • FIGS. 1 to 4 a method of analyzing a crystal structure of a sample according to an embodiment of the present invention will be described in detail with reference to FIGS. 1 to 4. However, for the sake of simplicity of the invention, descriptions of the details that have already been described in FIGS. 1 to 3B will be omitted.
  • the method for analyzing the crystal structure of a sample may be initiated by measuring an inter-planar distance and an inter-planar angle from a diffraction pattern (DP) image of the sample in the measurement module 110 (S401). ).
  • DP diffraction pattern
  • the primary candidate group selection module 120 may refer to the database 150 to select a primary candidate group having crystal structures corresponding to the component information of the sample (S402).
  • the second candidate group selection module 130 refers to the database 150 and selects a crystal structure having an interplanar distance matching the measured interplanar distance among the crystal structures included in the selected first candidate group as a second candidate group. It can be selected (S403).
  • the second candidate group selection module 130 may determine that the difference between the measured interplanar distance and the interplanar distance of the crystal structure included in the selected first candidate group is less than ⁇ 5%.
  • the determination module 140 refers to the database 150 to determine a crystal structure having an interplanar angle matching the measured interplanar angle among the crystal structures included in the selected secondary candidate group as the crystal structure of the sample.
  • the determination module 140 may determine that an error between the measured interplanar angle and the interplanar angle of the crystal structure included in the selected secondary candidate group is less than ⁇ 5%. It should be noted that specific values for determining the degree of matching described above are for aiding understanding of the present invention, and the present invention is not limited to specific values.
  • the determination module 140 calculates an inter-planar angle from the surface index used for calculating the inter-planar distance among the surface indices of the crystal structure included in the selected secondary candidate group, and compares the calculated inter-planar angle with the measured inter-planar angle. After that, a surface index matching the measured interplanar angle may be determined, and a crystal structure having the determined surface index may be determined as the crystal structure of the sample by referring to the database 150.
  • the interplanar distance and the interplanar angle measured from the diffraction pattern image of the sample are obtained by using the interplanar distance for each crystal structure stored in the database and a plane index that satisfies the interplanar distance.
  • the above-described method for analyzing a crystal structure of a sample according to an embodiment of the present invention may be produced as a program for execution in a computer and stored in a computer-readable recording medium.
  • Examples of computer-readable recording media include ROM, RAM, CD-ROM, magnetic tape, floppy disk, optical data storage device, and the like.
  • the computer-readable recording medium is distributed over a computer system connected through a network, so that computer-readable codes can be stored and executed in a distributed manner.
  • functional programs, codes, and code segments for implementing the method can be easily inferred by programmers in the art to which the present invention belongs.
  • ' ⁇ module' refers to various methods, for example, a processor, program instructions executed by a processor, a software module, a microcode, a computer program product, a logic circuit, an application-only integrated circuit, and a firmware. It can be implemented by

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Computer Vision & Pattern Recognition (AREA)
  • Theoretical Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

Un appareil d'analyse de la structure cristalline d'un échantillon selon un mode de réalisation de la présente invention peut comprendre : un module de mesure pour mesurer la distance interplanaire et l'angle interplanaire à partir d'une image de motif de diffraction d'un échantillon ; un module de sélection de premier groupe candidat destiné à se référer à une base de données et à sélectionner un premier groupe candidat ayant des structures cristallines correspondant à des informations de composant de l'échantillon, si les informations de composant de l'échantillon sont entrées ; un module de sélection de second groupe candidat destiné à se référer à la base de données et à sélectionner, en tant que second groupe candidat, des structures cristallines ayant une distance interplanaire correspondant à la distance interplanaire mesurée, parmi les structures cristallines comprises dans le premier groupe candidat sélectionné ; et un module de détermination destiné à se référer à la base de données et à déterminer, sur la base d'un indice de plan ayant un angle interplanaire correspondant à l'angle interplanaire mesuré, la structure cristalline de l'échantillon parmi les structures cristallines incluses dans le second groupe candidat.
PCT/KR2020/006544 2019-08-09 2020-05-19 Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur WO2021029519A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2019-0097306 2019-08-09
KR1020190097306A KR102251068B1 (ko) 2019-08-09 2019-08-09 시료의 결정 구조 분석 장치, 방법 및 컴퓨터로 독출 가능한 기록 매체

Publications (1)

Publication Number Publication Date
WO2021029519A1 true WO2021029519A1 (fr) 2021-02-18

Family

ID=74569602

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2020/006544 WO2021029519A1 (fr) 2019-08-09 2020-05-19 Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur

Country Status (2)

Country Link
KR (1) KR102251068B1 (fr)
WO (1) WO2021029519A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0587746A (ja) * 1991-04-05 1993-04-06 Nippon Steel Corp 電子回折パターンの解析方法
JP2004264260A (ja) * 2003-03-04 2004-09-24 Kyocera Corp 電子回折パターンの解析方法及び解析装置
WO2008060237A1 (fr) * 2006-11-15 2008-05-22 Hovmoeller Sven Appareil électronique de prise de vues par rotation
KR20170076263A (ko) * 2015-12-24 2017-07-04 주식회사 포스코 알루미나 분체의 불순물 측정 장치 및 이의 측정 방법
JP2018197657A (ja) * 2017-05-23 2018-12-13 住友電気工業株式会社 面間隔の評価方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101308949B1 (ko) 2011-07-12 2013-09-24 백종원 창틀용 우수 배수 장치의 시공방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0587746A (ja) * 1991-04-05 1993-04-06 Nippon Steel Corp 電子回折パターンの解析方法
JP2004264260A (ja) * 2003-03-04 2004-09-24 Kyocera Corp 電子回折パターンの解析方法及び解析装置
WO2008060237A1 (fr) * 2006-11-15 2008-05-22 Hovmoeller Sven Appareil électronique de prise de vues par rotation
KR20170076263A (ko) * 2015-12-24 2017-07-04 주식회사 포스코 알루미나 분체의 불순물 측정 장치 및 이의 측정 방법
JP2018197657A (ja) * 2017-05-23 2018-12-13 住友電気工業株式会社 面間隔の評価方法

Also Published As

Publication number Publication date
KR20210017673A (ko) 2021-02-17
KR102251068B1 (ko) 2021-05-13

Similar Documents

Publication Publication Date Title
US8068662B2 (en) Method and system for determining a defect during charged particle beam inspection of a sample
CN106767402B (zh) 一种盾构法隧道表观质量检测方法及系统
TWI521475B (zh) Pattern inspection and testing devices and programs
JP4771714B2 (ja) パターン検査装置および方法
US20010055416A1 (en) Defect inspection method and defect inspection apparatus
Rhines et al. Measurement of average grain volume and certain topological parameters by serial section analysis
JPS6379058A (ja) 熱交換器の管の渦電流試験データの機械分析方法及び装置
CN112825190B (zh) 一种精度评估方法、系统、电子设备和存储介质
JP4943616B2 (ja) 直線の欠陥検出
Ojha et al. A multicolor survey of absolute proper motions: galactic structure and kinematics in the direction of galactic centre at intermediate latitude
WO2021029519A1 (fr) Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur
TW471016B (en) Defect detection using gray level signatures
WO2015046668A1 (fr) Procédé de mesure de rapport volumique de chaque milieu constitutif existant dans une unité minimale d'image de tomodensitométrie à rayons x pour un échantillon formé de milieux complexes
US4745296A (en) Process for optically testing circuit boards to detect incorrect circuit patterns
Müller et al. Utilization of single point uncertainties for geometry element regression analysis in dimensional X-ray computed tomography
CN111563532B (zh) 一种基于属性权重融合的未知目标识别方法
JP4597509B2 (ja) パターン検査装置およびパターン検査方法
WO2015053480A1 (fr) Système et procédé d'analyse d'échantillons biologiques
US20040234133A1 (en) Computer-assisted detection method for diaphragm edges caused in an image by a diaphragm
CN114299406B (zh) 基于无人机航拍的光纤电缆线路巡检方法
CN114567771A (zh) 一种在棋盘格测试图上进行sfr测试的方法、装置及可读存储介质
WO2017043942A1 (fr) Procédé d'analyse d'échantillon tridimensionnel
KR20210149435A (ko) 자가면역질환 진단을 위한 항핵항체 역가측정 방법
WO2024144296A1 (fr) Procédé et dispositif de mesure de dimension de faisceau ethernet
Schuecker The Muenster Redshift Project: improved methods for automated galaxy redshift measurements from very low-dispersion objective-prism spectra

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20853073

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20853073

Country of ref document: EP

Kind code of ref document: A1