Instrument Configuration for Powder Diffraction
|
|
- George Jerome Hicks
- 6 years ago
- Views:
Transcription
1 Instrument Configuration for Powder Diffraction Advanced X-ray Workshop S.N. Bose National Centre for Basic Sciences, 14-15/12/2011 Innovation with Integrity
2 Overview What is the application? What are the requirements of your application? Early Decisions Sample Instrument Data Collection Early decisions: What are the sample properties? What data quality is necessary? What instrument and measurement parameters to use? Advanced X-ray Workshop 2
3 Overview "Although the physical nature of a specimen from which the X-ray powder-diffraction data are collected is seemingly simple, sample preparation and data collection are generally the source of most of the serious problems with accurate X-ray diffraction analysis" Too small number of scattering particles / coarse grains (spotiness) Preferred orientation Inappropriate instrument geometry / sample presentation Unsuited step size / measurement time Advanced X-ray Workshop 3
4 The Sample Advanced X-ray Workshop 4
5 The Sample What is the form of the sample? "Powder Diffraction" is more aptly named "Polycrystalline Diffraction" Samples can be powder, sintered pellets, coatings on substrates, engine blocks, What is in your sample? Inorganics often better collected in reflection, organics often better collected in transmission Organics are poor scatterers at high angles Fluorescence can cause problems in data quality How much sample is there? Small quantities suggest capillary geometry (but absorption needs to be considered) Advanced X-ray Workshop 5
6 The Sample Minimize systematic sample related effects! This is as important as the optimization minimization of the instrument configuration! Avoid persisting with poor data (if possible) Find a better sample Re-prepare or remake the sample Change instrument or instrument setup Improve data collection parameters Don t rely on any software corrections! Variable slits conversion Preferred orientation corrections Microabsorption corrections (worst!)... Advanced X-ray Workshop 6
7 The Sample The grains in a powder should be randomly oriented: Front loading Sample prone to preferred orientation Back loading Better, but not effective on preferred orientation in all cases; consider using sandpaper to create a rough sample surface Use of capillary techniques Most effective but potential absorption issues No automation (sample preparation) Sample motion Motion should be 90 to the diffraction vector No effect on preferred orientation in reflection geometry! May slightly improve particle statistics; no improvements if large grains are present Advanced X-ray Workshop 7
8 The Sample Rotation parallel to the scattering vector does not reduce preferred orientation effects! Bragg-Brentano Reflection Debye-Scherrer Capillary Advanced X-ray Workshop 8
9 The Sample Debye cone of diffracted beam Ideally some crystallites in the beam Ideally completely random orientation Incident beam Adapted from S. Misture, 2002 Advanced X-ray Workshop 9
10 The Sample Phase Grain size ( crystallite size!) (C)orundum 28.0µm (M)agnetite 36.2µm (Z)ircon 21.1µm M Z C ZM Advanced X-ray Workshop 10
11 The Sample Spotiness effects cannot be corrected! Advanced X-ray Workshop 11
12 The Sample Need to get sample to a fine powder (preferably in the micron size range) without destroying or detrimentally affecting the sample The higher energy the grinding, the more likely the sample could undergo a phase transition Need to check different methods / grinding times to see which gets the job done effectively with the minimum of effort Peak broadening, apparent increase of background? Overgrinding? Crystallite size already too small? Samples gets amorphous? Variable relative intensities? New or disappearing peaks? Spotiness effect? Preferred orientation? Phase transformation? Try to grind materials with soft phases in liquid nitrogen Advanced X-ray Workshop 12
13 The Instrument Advanced X-ray Workshop 13
14 The Instrument The choice of the optimum instrument configuration must consider the aim of the experiment as well as specific sample properties Advanced X-ray Workshop 14
15 The Instrument Bragg-Brentano geometry with secondary monochromator (K α1+2 ) Advanced X-ray Workshop 15
16 The Instrument Bragg-Brentano geometry with incident beam monochromator (pure K α1 ), reflection geometry Focusing monochromator Asymmetric Ge(111) for λ Cu, asymmetric Ge(220) for λ Mo Advanced X-ray Workshop 16
17 The Instrument Bragg-Brentano geometry with incident beam monochromator, transmission geometry Foil transmission - capillary transmission Advanced X-ray Workshop 17
18 The Instrument ~ 1990: Introduction of parabolic graded multilayers Basic idea: Convert a divergent beam into a parallel beam Nowadays also eliptical graded multilayers for focussing beam Göbel Mirror X-ray Tube Advanced X-ray Workshop 18
19 The Instrument Parallel Beam Geometry Reflection Foil Transmission Capillary Transmission Advanced X-ray Workshop 19
20 The Instrument Bragg-Brentano Geometry - Properties Excellent resolution / line profile shapes ++ Up to 90% intensity loss with monochromators Large footprint of the beam (up to several cm) Good crystallite statistics Possibility of beam overflow at low angles 2θ Flat specimen error Sample displacement error Sample transparency error Advanced X-ray Workshop 20
21 Bragg-Brentano Geometry Flat Specimen Error 2Θ Sample is tangent to the variable focussing circle leading to peak shifts and asymmetric broadening Small divergence slits help at the expense of intensity Sample Advanced X-ray Workshop 21
22 Bragg-Brentano Geometry Sample Displacement Error 2Θ The sample must be tangent to the focussing circle Any deviations lead to peak shifts and asymmetric broadening Note: The sample displacement error is typically the largest error found in Bragg-Brentano geometry Sample Advanced X-ray Workshop 22
23 Bragg-Brentano Geometry Sample Transparency Error 2Θ In low absorbing samples the average diffracting surface lies below the physical sample surface leading to peak shifts and asymmetric broadening Note: The sample transparency error is equivalent to the sample displacement error Use transmission geometry Sample Advanced X-ray Workshop 23
24 The Instrument Parallel beam geometry - Properties Offers new possibilites for lab X-ray powder diffraction by overcoming significant limitations of the Bragg-Brentano geometry Ill-shaped samples may be used Minimized sample displacement, sample transparency, and beam overflow errors Easy change between reflection and transmission geometry - with foil transmission even without touching the instrument Intensity gain of a factor of up to 10??? Advanced X-ray Workshop 24
25 Parallel Beam Geometry Intensity Gain? An intensity gain of a factor of up to 10 may be obtained, if collimators / pinholes / slits are replaced by a Göbel mirror Thin film analysis (high resolution, grazing incidence, reflectometry) SAXS... This is NOT the case for standard powder diffraction applications, intensity may be even less! Advanced X-ray Workshop 25
26 The Instrument Parallel beam geometry - Properties Poor to medium resolution Not enough scattering particles ("Spotiness" effect) Parallel beam conditions Small footprint of the beam (few mm at maximum) Can deal with sample surface roughness, but... Advanced X-ray Workshop 26
27 Parallel Beam Geometry "Spotiness" effect Bragg-Brentano geometry Horizontal beam divergence significantly increases the number of diffracting crystallites Parallel beam geometry Significant reduction of the number of diffracting particles due to low beam divergence Advanced X-ray Workshop 27
28 Parallel Beam Geometry Surface Roughness With decreasing 2q diffracted intensity may not reach the detector due to "self-absorption" leading to severe intensity errors Note: Surface roughness will normally prevent reliable quantitative analysis and structure analysis Advanced X-ray Workshop 28
29 The Instrument The Bragg-Brentano is the preferred geometry for most powder diffraction applications, including non-ambient measurements The parallel beam geometry is required for ill-shaped samples and micro-diffraction. Applications are normally limited to phase ID. Advanced X-ray Workshop 29
30 Data Collection Advanced X-ray Workshop 30
31 Data Collection Need of accurate profile parameters: Phase ID Quantitative Analysis 2θ Intensity Resolution Indexing Structure Analysis Advanced X-ray Workshop 31
32 Data Collection Phase ID has the least stringent requirements on both sample prep and data collection Highly tolerant to large peak position and intensity errors Highly tolerant to sample preparation and presentation, unless there are issues related to complex samples (peak overlap) and lower limits of detection Size-strain analysis, quantitative phase analysis, and structure analysis require careful sample preparation and presentation! Advanced X-ray Workshop 32
33 Data Collection Phase ID Make sure to get enough peaks for confident phase identification. Using Cu X-rays: 2 to 90 degrees 2θ; most PDF entries dont go beyond Count time depends on whether only interested in major phases, minor or trace phases Consider VCT All search / match results given can only be a list of suggestions. It is up to the user to pick the correct suggestions or to recognise that there are no reasonable hits The best match does not necessarily give you the correct / best crystal structure! Advanced X-ray Workshop 33
34 Data Collection Indexing Data collection range to get 20 to 40 peaks For low absorbing samples (organics), floating onto a low background plate can be desirable (reflection geometry) Accurate peak positions are important with indexing, not intensities Use the Fundamental Parameters Approach to obtain the best peak positions possible XRD optimized for maximum resolution Monochromatic radiation desirable! Small peaks shouldn't be obscured by Kα 2 peaks! Advanced X-ray Workshop 34
35 Data Collection Size-Strain Analysis Measure the maximum accessible 2θ-range to be able to distinguish between crystallite size and strain XRD optimized for line profile shape Bragg-Brentano geometry gives best defined line profile shapes Fundamental Parameters Approach XRD optimized for line profile shape if crystallite size is large and / or strain is small Advanced X-ray Workshop 35
36 Data Collection Structure Analysis Optimize sample preparation and presentation to minimize any sample related effects Preferred orientation, spotiness, absorption Inorganics: Measure in reflection or transmission; for transmission Mo radiation is strongly recommended Organics: Measure in transmission Consider Mo + capillary rather than Vario-1 with Cu, specifically if there are preferred orientation and absorption issues! XRD rather optimized for high intensity rather than maximum resolution High intensity using Kα 1,2 may be more important than getting rid of Kα 2 High angle data are particularily important, VCT is crucial Measure the maximum accessible 2θ-range Advanced X-ray Workshop 36
37 Data Collection Quantitative Analysis Similar to structure analysis Optimize sample preparation and presentation to minimize any sample related effects Preferred orientation, spotiness, absorption XRD rather optimized for high intensity rather than maximum resolution High intensity using Kα 1,2 may be more important than getting rid of Kα 2 High angle data are particularily important, VCT is crucial Measure the maximum accessible 2θ-range For well characterized mixtures a smaller 2θ-range maybe sufficient Advanced X-ray Workshop 37
38 Innovation with Integrity Copyright 2011 Bruker Bruker Corporation. Corporation. All rights reserved. All rights reserved.
OPTIMIZING XRD DATA. By: Matthew Rayner
OPTIMIZING XRD DATA By: Matthew Rayner 1 XRD Applications PANalytical classifies XRD applications in 4 groups 1. Powders 2. Nanomaterials 3. Solid objects 4. Thin films Many day-to-day samples cross these
More informationLesson 1 Good Diffraction Data
Lesson 1 Good Diffraction Data Nicola Döbelin RMS Foundation, Bettlach, Switzerland Digital Diffractometers Transmission Geometry Debye-Scherrer Geometry Reflective Geometry Bragg-Brentano Geometry Glass
More informationLesson 3 Sample Preparation
Lesson 3 Sample Preparation Nicola Döbelin RMS Foundation, Bettlach, Switzerland January 14 16, 2015, Bern, Switzerland Repetition: Bragg-Brentano Diffractometer Typical Configuration (with Kβ filter)
More informationFundamentals of X-ray diffraction and scattering
Fundamentals of X-ray diffraction and scattering Don Savage dsavage@wisc.edu 1231 Engineering Research Building (608) 263-0831 X-ray diffraction and X-ray scattering Involves the elastic scattering of
More informationLECTURE 7. Dr. Teresa D. Golden University of North Texas Department of Chemistry
LECTURE 7 Dr. Teresa D. Golden University of North Texas Department of Chemistry Diffraction Methods Powder Method For powders, the crystal is reduced to a very fine powder or microscopic grains. The sample,
More informationEarth & Planetary Science Applications of X-Ray Diffraction: Advances Available for Research with our New Systems
Earth & Planetary Science Applications of X-Ray Diffraction: Advances Available for Research with our New Systems James R. Connolly Dept. of Earth & Planetary Sciences University of New Mexico 401/501
More informationX-ray diffraction
2.2.3.- X-ray diffraction 2.2.3.1.- Origins and fundamentals of the technique The first experimental evidence concerning x-ray diffraction was given by Max von Laue who in 1912 demonstrated that x-rays
More informationIntroduction to Powder Diffraction/Practical Data Collection
Durham University Chemistry Department Introduction to Powder Diffraction/Practical Data Collection Dr Ivana Evans Durham, January 2007 Durham Outline Information in a powder pattern What is diffraction
More informationTravaux Pratiques de Matériaux de Construction. Etude de Matériaux Cimentaires par Diffraction des Rayons X sur Poudre
Travaux Pratiques de Matériaux de Construction Section Matériaux 6 ème semestre 2015 Etude de Matériaux Cimentaires par Diffraction des Rayons X sur Poudre Study Cementitious Materials by X-ray diffraction
More informationWhat if your diffractometer aligned itself?
Ultima IV Perhaps the greatest challenge facing X-ray diffractometer users today is how to minimize time and effort spent on reconfiguring of the system for different applications. Wade Adams, Ph.D., Director,
More informationATTACHMENTES FOR EXPLORER DIFFRACTOMETER. Monochromators
Monochromators Secondary flat and curved graphite monochromators suitable for Ag, Cr, Fe, Cu, Co and Mo radiations This attachment is installed in the X-ray detection unit. It is designed to remove continuous
More informationX-RAY DIFFRACTION IN SEMICONDUCTOR INDUSTRY AND RESEARCH
X-RAY DIFFRACTION IN SEMICONDUCTOR INDUSTRY AND RESEARCH M. Leszczyński High Pressure Research Center UNIPRESS, Sokolowska 29/37, 01 142 Warsaw, Poland, e-mail: mike@unipress.waw.pl ABSTRACT The paper
More informationThis lecture is part of the Basic XRD Course.
This lecture is part of the Basic XRD Course. Basic XRD Course 1 A perfect polycrystalline sample should contain a large number of crystallites. Ideally, we should always be able to find a set of crystallites
More informationATTACHMENTES FOR APD 2000 PRO POWDER X-RAY DIFFRACTOMETER. Monochromators
Monochromators Secondary graphite monochromator Johansson Ka 1 monochromator Parabolic monochromator Secondary flat and curved graphite monochromators suitable for Ag, Cr, Fe, Cu, Co and Mo radiations
More informationSmithsonian Museum Conservation Institute
Smithsonian Museum Conservation Institute XRD Analysis of the Corrosion Products from a Tlingit Copper Rattle MCI#6241 Object: Tlingit Stikine Rattle Owner/Custodian: National Museum of the American Indian
More informationThermo Scientific ARL EQUINOX X-ray Diffractometers
Thermo Scientific ARL EQUINOX 1000 X-ray Diffractometers High performance in a compact size Thermo Scientific ARL EQUINOX 1000 X-ray diffractometer (XRD) is designed to meet structural and phase analysis
More informationLesson 1 X-rays & Diffraction
Lesson 1 X-rays & Diffraction Nicola Döbelin RMS Foundation, Bettlach, Switzerland February 11 14, 2013, Riga, Latvia Electromagnetic Spectrum X rays: Wavelength λ: 0.01 10 nm Energy: 100 ev 100 kev Interatomic
More informationThermo Scientific ARL EQUINOX 100. X-ray Diffractometers
Thermo Scientific ARL EQUINOX 100 X-ray Diffractometers High performance in a compact size Thermo Scientific ARL EQUINOX 100 X-ray diffractometer (XRD) is designed to meet structural and phase analysis
More informationX-ray Powder Diffraction in Catalysis
X-ray Powder Diffraction in Catalysis 0/63 Introduction Introduction: scope of this lecture This lecture is designed as a practically oriented guide to powder XRD in catalysis, not as an introduction into
More informationTravaux Pratiques de Matériaux de Construction
Travaux Pratiques de Matériaux de Construction Section Matériaux 6 ème semestre 2009 Etude de Matériaux Cimentaire Par Diffraction des Rayons X Responsable: Silke Ruffing E-Mail: silke.ruffing@epfl.ch
More informationPrecision Without Compromise
D1 EVOLUTION Precision Without Compromise Versatile and user-friendly high resolution and multipurpose X-ray diffractometer for the characterization of advanced materials www.jvsemi.com D1 Overview Introduction
More informationCHARACTERISATION OF CRYSTALLINE AND PARTIALLY CRYSTALLINE SOLIDS BY X-RAY POWDER DIFFRACTION (XRPD)
2.9.33. Characterisation of crystalline solids by XRPD EUROPEAN PHARMACOPOEIA 6.0 with its standard deviation. The mean values for x 10 and x 90 must not deviate by more than 5 per cent from the certified
More informationDiffraction Basics. The qualitative basics:
The qualitative basics: Diffraction Basics Coherent scattering around atomic scattering centers occurs when x-rays interact with material In materials with a crystalline structure, x-rays scattered in
More informationX-Ray Analytical Methods
X-Ray Analytical Methods X-rays were discovered by W.C. Röentgen in 1895, and led to three major uses: X-ray radiography is used for creating images of light-opaque materials relies on the relationship
More informationTechnical articles Micro-area X-ray diffraction measurement by SmartLab μ
Technical articles Micro-area X-ray diffraction measurement by SmartLab μhr diffractometer system with ultra-high brilliance microfocus X-ray optics and two-dimensional detector HyPix-3000 Yuji Shiramata*
More informationBasics of XRD part IV
Basics of XRD part IV Dr. Peter G. Weidler Institute of Functional Interfaces IFG 1 10/31/17 KIT The Research University in the Helmholtz Association Name of Institute, Faculty, Department www.kit.edu
More informationSingle crystal X-ray diffraction. Zsolt Kovács
Single crystal X-ray diffraction Zsolt Kovács based on the Hungarian version of the Laue lab description which was written by Levente Balogh, Jenő Gubicza and Lehel Zsoldos INTRODUCTION X-ray diffraction
More informationDiffraction: Powder Method
Diffraction: Powder Method Diffraction Methods Diffraction can occur whenever Bragg s law λ = d sin θ is satisfied. With monochromatic x-rays and arbitrary setting of a single crystal in a beam generally
More informationBasics of X-Ray Diffraction
Basics of X-Ray Diffraction Crystalline materials are characterized by the orderly periodic arrangements of atoms. The (200) planes of atoms in NaCl The (220) planes of atoms in NaCl The unit cell is the
More informationSYSTEMATIC ERRORS IN LINEAR PSD BASED HTXRD SYSTEMS
Copyright(c)JCPDS-International Centre for Diffraction Data 2,Advances in X-ray Analysis,Vol.43 267 SYSTEMATIC ERRORS IN LINEAR PSD BASED HTXRD SYSTEMS E.A. Payzant and W.S. Harrison, III * Metals and
More informationPhilips Analytical, Lelyweg 1, 7602 EA Almelo, The Netherlands
Copyright(c)JCPDS-International Centre for Diffraction Data 2001,Advances in X-ray Analysis,Vol.44 284 MICRO-DIFFRACTION WITH MONO-CAPILLARIES M.J. Fransen, J.H.A. Vasterink and J. te Nijenhuis Philips
More informationMiniFlex. Analysis of materials by X-ray diffraction. Benchtop XRD diffractometer
MiniFlex Analysis of materials by X-ray diffraction Benchtop XRD diffractometer More power More flexibility More results The new MiniFlex is available in two models. The MiniFlex 600 is the most powerful
More informationBenchtop XRD diffractometer. MiniFlex. Analysis of materials by X-ray diffraction
Benchtop XRD diffractometer MiniFlex Analysis of materials by X-ray diffraction More power More flexibility More results The new MiniFlex is available in two models. The MiniFlex 600 is the most powerful
More informationX-Ray Diffraction. Nicola Pinna
X-Ray Diffraction Nicola Pinna Department of Chemistry, CICECO, University of Aveiro, 3810-193 Aveiro, Portugal. School of Chemical and Biological Engineering, College of Engineering, Seoul National University
More informationPhysics 6180: Graduate Physics Laboratory. Experiment CM5: X-ray diffraction and crystal structures
Physics 6180: Graduate Physics Laboratory Experiment CM5: X-ray diffraction and crystal structures References: Preston and Dietz, Expt. 10 pp. 180-197 Eisberg and Resnick, Quantum Physics, Sec. 9 Kittel,
More informationCopyright JCPDS - International Centre for Diffraction Data 2004, Advances in X-ray Analysis, Volume
Copyright JCPDS - International Centre for Diffraction Data 2004, Advances in X-ray Analysis, Volume 47. 240 SIMULTANEOUS MEASUREMENTS OF X-RAY DIFFRACTION (XRD) AND DIFFERENTIAL SCANNING CALORIMETRY (DSC)
More informationSystematic Errors and Sample Preparation for X-Ray Powder Diffraction. Jim Connolly EPS , Spring 2010
Systematic Errors and Sample Preparation for X-Ray Powder Diffraction Jim Connolly EPS400-001, Spring 2010 Introduction Most systematic errors in diffraction experiments are related to the characteristics,
More informationHIGH-RESOLUTION PARALLEL-BEAM POWDER DIFFRACTION MEASUREMENT OF SUB-SURFACE DAMAGE IN ALUMINA-SILICON CARBIDE NANOCOMPOSITE
169 HIGH-RESOLUTION PARALLEL-BEAM POWDER DIFFRACTION MEASUREMENT OF SUB-SURFACE DAMAGE IN ALUMINA-SILICON CARBIDE NANOCOMPOSITE B K Tanner, H Z Wu + and S G Roberts * Department of Physics, University
More informationA. KISHI AND H. TORAYA
THE RIGAKU JOURNAL VOL. 21 / NO. 1 / 2004, 25 30 SIMULTANEOUS MEASUREMENTS OF X-RAY DIFFRACTION (XRD) AND DIFFERENTIAL SCANNING CALORIMETRY (DSC) DATA UNDER CONTROLLED HUMIDITY CONDITION: INSTRUMENTATION
More informationMaterials Lab 1(MT344) X-ray Diffractometer Operation and Data Analysis. Instructor: Dr. Xueyan Wu ( 吴雪艳 )
Materials Lab 1(MT344) X-ray Diffractometer Operation and Data Analysis Instructor: Dr. Xueyan Wu ( 吴雪艳 ) Goals To give students a practical introduction into the use of X-ray diffractometer and data collection.
More informationAn Introduction to X-Ray Powder Diffraction. credits to: Scott A Speakman, Patrick McArdle Edited by Di Cicco 2014
An Introduction to X-Ray Powder Diffraction credits to: Scott A Speakman, Patrick McArdle Edited by Di Cicco 2014 LATTICE ARRAYS AND BRAVAIS LATTICES Crystalline materials differ from amorphous materials
More informationStrain. Two types of stresses: Usually:
Stress and Texture Strain Two types of stresses: microstresses vary from one grain to another on a microscopic scale. macrostresses stress is uniform over large distances. Usually: macrostrain is uniform
More informationIdentification of Crystal Structure and Lattice Parameter. for Metal Powders Using X-ray Diffraction. Eman Mousa Alhajji
Identification of Crystal Structure and Lattice Parameter for Metal Powders Using X-ray Diffraction Eman Mousa Alhajji North Carolina State University Department of Materials Science and Engineering MSE
More informationThin Film Scattering: Epitaxial Layers
Thin Film Scattering: Epitaxial Layers 6th Annual SSRL Workshop on Synchrotron X-ray Scattering Techniques in Materials and Environmental Sciences: Theory and Application May 29-31, 2012 Thin films. Epitaxial
More informationBasic X-ray Powder Diffraction (XRPD)
Basic X-ray Powder Diffraction (XRPD) Solid-State, Material Science Crystalline (Scattering : diffraction) Non-crystalline (Scattering) Analytical Tool Qualitative and Quantitative Analysis Quantitative
More informationHigh Resolution X-ray Diffraction
High Resolution X-ray Diffraction Nina Heinig with data from Dr. Zhihao Donovan Chen, Panalytical and slides from Colorado State University Outline Watlab s new tool: Panalytical MRD system Techniques:
More informationX-ray fluorescence (XRF)
X-ray fluorescence (XRF) Laboratory: n.4 3D microtomographic systems, n.2 portable XRF systems Various X-ray detectors: HpGe, SI-PIN, SDD, NaI. n. 6 X-Ray tubes Four samples of mineral of different colors
More informationX-ray Diffraction (XRD)
هب انم خدا X-ray Diffraction (XRD) 1.0 What is X-ray Diffraction 2.0 Basics of Crystallography 3.0 Production of X-rays 4.0 Applications of XRD 5.0 Instrumental Sources of Error 6.0 Conclusions Bragg s
More informationSmall-angle X-ray scattering (SAXS) with synchrotron radiation
Small-angle X-ray scattering (SAXS) with synchrotron radiation Martin Müller Institut für Experimentelle und Angewandte Physik der Christian-Albrechts-Universität zu Kiel Introduction to small-angle scattering
More informationDedication in X-ray powder diffraction
X PERT 3 POWDER Dedication in X-ray powder diffraction The Analytical X-ray Company x-ray diffraction Let materials work for you Advancing materials research From geological exploration, through processing
More informationLECTURE 8. Dr. Teresa D. Golden University of North Texas Department of Chemistry
LECTURE 8 Dr. Teresa D. Golden University of North Texas Department of Chemistry Practical applications for lattice parameter measurements: -determine composition (stoichiometry) of the sample -determine
More informationWorkshop RIETVELD REFINEMENT OF DIFFRACTION PATTERNS Program Monday June 1st, Introduction to Rietveld refinement S.
Workshop RIETVELD REFINEMENT OF DIFFRACTION PATTERNS Program Monday June 1st, 2009 9.00 13.00 Introduction to Rietveld refinement S.Enzo Università di Sassari X-ray diffraction for bulk samples and thin
More informationBruker AXS D8 FABLINE. X-Ray Metrology Solutions. think forward
Bruker AXS D8 FABLINE X-Ray Metrology Solutions think forward XRD & µxrf D8 FABLINE Metrology for Semiconductor Manufacturing The functional units of semiconductor and compound semiconductor devices shrink
More informationBackground Statement for SEMI Draft Document 5945 New Standard: Test Method for Determining Orientation of A Sapphire Single Crystal
Background Statement for SEMI Draft Document 5945 New Standard: Test Method for Determining Orientation of A Sapphire Single Crystal Notice: This background statement is not part of the balloted item.
More informationARL X TRA Powder X-ray Diffraction System. Uncompromised Intensity and Resolution
e l e m e n t a l a n a l y s i s ARL X TRA Powder X-ray Diffraction System Uncompromised Intensity and Resolution Analyze Detect Measure Control ARL X TRA Powder X-ray Diffraction System ARL X TRA High
More informationX-Ray Diffraction Analysis
162402 Instrumental Methods of Analysis Unit III X-Ray Diffraction Analysis Dr. M. Subramanian Associate Professor Department of Chemical Engineering Sri Sivasubramaniya Nadar College of Engineering Kalavakkam
More informationNEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES
NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES Jeff Shield Department of Mechanical & Materials Engineering Nebraska Center for Materials and Nanoscience National Nanotechnology Coordinated Infrastructure
More informationPractical X-Ray Diffraction
Typical Example Practical X-Ray Diffraction White powder sample of NaCl,KCl,KNO 3 (trace of H 2 O) Département de chimie Université Laval Prof. Josée BRISSON Dr. Wenhua BI 2014-03-20 Powder X-Ray Diffraction
More informationAN INNOVATED LABORATORY XAFS APPARATUS
Copyright (c)jcpds-international Centre for Diffraction Data 2002, Advances in X-ray Analysis, Volume 45. 397 AN INNOVATED LABORATORY XAFS APPARATUS TAGUCHI Takeyoshi XRD Division, Rigaku Corporation HARADA
More informationThin Film Scattering: Epitaxial Layers
Thin Film Scattering: Epitaxial Layers Arturas Vailionis First Annual SSRL Workshop on Synchrotron X-ray Scattering Techniques in Materials and Environmental Sciences: Theory and Application Tuesday, May
More informationCarnegie Mellon MRSEC
Carnegie Mellon MRSEC Texture, Microstructure & Anisotropy, Fall 2009 A.D. Rollett, P. Kalu 1 ELECTRONS SEM-based TEM-based Koseel ECP EBSD SADP Kikuchi Different types of microtexture techniques for obtaining
More informationRECONSTRUCTION OF ORIGINAL INTENSITY FROM COVERED SAMPLES
RECONSTRUCTION OF ORIGINAL INTENSITY FROM COVERED SAMPLES 163 R.I. Barabash, T.R. Watkins, R.A. Meisner, T.D. Burchell, T.M. Rosseel Oak Ridge National Laboratory, Oak Ridge TN 37831, USA ABSTRACT The
More informationAdvanced Methods for Materials Research. Materials Structure Investigations Materials Properties Investigations
Advanced Methods for Materials Research Materials Structure Investigations Materials Properties Investigations Advanced Methods for Materials Research 1. The structure and property of sample and methods
More informationChapter 3 Basic Crystallography and Electron Diffraction from Crystals. Lecture 9. Chapter 3 CHEM Fall, L. Ma
Chapter 3 Basic Crystallography and Electron Diffraction from Crystals Lecture 9 Outline The geometry of electron diffraction Crystallography Kinetic Theory of Electron diffraction Diffraction from crystals
More informationSpatially resolved crystal domain identification: Implementing Laue-mapping technique on the M4 TORNADO spectrometer
Spatially resolved crystal domain identification: Implementing Laue-mapping technique on the M4 TORNADO spectrometer Bruker Nano Analytics, Berlin, Germany Webinar, July 14 th, 2016 Innovation with Integrity
More informationMICROSTRUCTURAL CHARACTERIZATION OF NANOCRYSTALLINE POWDERS AND THIN FILMS BY X-RAY POWDER DIFFRACTION
MICROSTRUCTURAL CHARACTERIZATION OF NANOCRYSTALLINE POWDERS AND THIN FILMS BY X-RAY POWDER DIFFRACTION Zdeněk MATĚJ a, Lea NICHTOVÁ a, Radomír KUŽEL a a Faculty of Mathematics and Physics, Charles University
More informationMicroanalysis with high spectral resolution: the power of QUANTAX WDS for SEM
Microanalysis with high spectral resolution: the power of QUANTAX WDS for SEM Bruker Nano Analytics, Berlin, Germany Webinar, September 14, 2017 Innovation with Integrity Presenters Dr. Jörg Silbermann
More informationATTACHMENT D3 University of British Columbia X-Ray Diffraction Report and Scanning Electron Microscopy Images
Appendix D Laboratory Geotechnical Data and Interpretation ATTACHMENT D3 University of British Columbia X-Ray Diffraction Report and QUANTITATIVE PHASE ANALYSIS OF ONE POWDER SAMPLE USING THE RIETVELD
More information9/28/2013 9:26 PM. Chapter 3. The structure of crystalline solids. Dr. Mohammad Abuhaiba, PE
Chapter 3 The structure of crystalline solids 1 2 Why study the structure of crystalline solids? Properties of some materials are directly related to their crystal structure. Significant property differences
More informationEurope. Benchtop X-Ray Diffractometer.
Europe Benchtop X-Ray Diffractometer www.gnr.it benchtop x-ray diffractometer Europe, High Performance in a compact configuration GNR is a worldwide market leader supplying advanced X-Ray (XRD, XRF) and
More informationStress Mitigation of X-ray Beamline Monochromators using a Topography Test Unit
128 Stress Mitigation of X-ray Beamline Monochromators using a Topography Test Unit J. Maj 1, G. Waldschmidt 1 and A. Macrander 1, I. Koshelev 2, R. Huang 2, L. Maj 3, A. Maj 4 1 Argonne National Laboratory,
More informationThermo Scientific ARL X TRA Powder X-ray Diffraction System Uncompromised Intensity and Resolution
e l e m e n t a l a n a l y s i s Thermo Scientific ARL X TRA Powder X-ray Diffraction System Uncompromised Intensity and Resolution Part of Thermo Fisher Scientific ARL X TRA Powder X-ray Diffraction
More informationBasics of X-Ray Powder Diffraction
Basics of X-Ray Powder Diffraction Scott A. Speakman, Ph.D. For assistance in the X-ray lab, please contact Charles Settens settens@mit.edu Scott A. Speakman, Ph.D. http://prism.mit.edu/xray Training Required
More informationINGE Engineering Materials. Chapter 3 (cont.)
Some techniques used: Chapter 3 (cont.) This section will address the question how do we determine the crystal structure of a solid sample? Electron microscopy (by direct and indirect observations) Scanning
More informationNEMI Sn Whisker Modeling Group Part 2:Future Work
NEMI Sn Whisker Modeling Group Part 2:Future Work IPC/NEMI Meeting Maureen Williams, NIST Irina Boguslavsky, NEMI Consultant November 7, 2002 New Orleans, LA Capabilities of NEMI Modeling Group NEMI Fundamental
More informationThe first measurement will be performed with a sample temperature of 35 by executing the following steps:
Work Instructions The experimental procedure of this practical is subdivided into two parts. In one part, a phase diagram of DEPE lipids is scanned through different temperatures, where a phase transition
More informationAtomic Densities. Linear Density. Planar Density. Linear Density. Outline: Planar Density
Atomic Densities Outline: Atomic Densities - Linear Density - Planar Density Single- vs poly- crystalline materials X-ray Diffraction Example Polymorphism and Allotropy Linear Density Number of atoms per
More informationThe object of this experiment is to test the de Broglie relationship for matter waves,
Experiment #58 Electron Diffraction References Most first year texts discuss optical diffraction from gratings, Bragg s law for x-rays and electrons and the de Broglie relation. There are many appropriate
More informationThe Empyrean Tube. Advanced eco-friendly design, powerful performance
The Empyrean Tube Advanced eco-friendly design, powerful performance The Empyrean Tube The industrial benchmark, redefined PANalytical s Empyrean Tubes set the standard, both for X-ray diffraction (XRD)
More information9/16/ :30 PM. Chapter 3. The structure of crystalline solids. Mohammad Suliman Abuhaiba, Ph.D., PE
Chapter 3 The structure of crystalline solids 1 Mohammad Suliman Abuhaiba, Ph.D., PE 2 Home Work Assignments HW 1 2, 7, 12, 17, 22, 29, 34, 39, 44, 48, 53, 58, 63 Due Sunday 17/9/2015 3 Why study the structure
More informationA Brief History of XRD 1895: Röntgen discovers X-Rays received the first Nobel prize in physics in 1901
X-ray Diffraction A Brief History of XRD 1895: Röntgen discovers X-Rays received the first Nobel prize in physics in 1901 1912: Laue diffracts X-Rays from single crystal 1914 Nobel prize in Physics 1912:
More informationCharacterization of Surfaces and Thin Films Using a High Performance Grazing Incidence X-ray Diffractometer
Copyright(c)JCPDS-International Centre for Diffraction Data 2000,Advances in X-ray Analysis,Vol.43 177 Characterization of Surfaces and Thin Films Using a High Performance Grazing Incidence X-ray Diffractometer
More informationX-RAY DIFFRACTION. X- Ray Sources Diffraction: Bragg s Law Crystal Structure Determination
X-RAY DIFFRACTION X- Ray Sources Diffraction: Bragg s Law Crystal Structure Determination Part of MATERIALS SCIENCE & ENGINEERING A Learner s Guide AN INTRODUCTORY E-BOOK Anandh Subramaniam & Kantesh Balani
More informationPowder X-ray Diffraction. Brendan J. Kennedy School of Chemistry The University of Sydney
Powder X-ray Diffraction Brendan J. Kennedy School of Chemistry The University of Sydney State of the Art on Earth1912 Bragg s X-ray tube Laue X-ray Diffractometer State of the Art on Mars 2012 Prototype
More informationX-Ray Diffraction by Macromolecules
N. Kasai M. Kakudo X-Ray Diffraction by Macromolecules With 351 Figures and 56 Tables Kodansha ~Springer ... Contents Preface v Part I Fundamental 1. Essential Properties of X-Rays................. 3 1.1
More informationChapter 4 Collection of EXAFS data from oxidised and reduced Plastocyanin
36 Chapter 4 Collection of EXAFS data from oxidised and reduced Plastocyanin 4.1 Preferred crystal orientations for collecting polarised EXAFS from poplar Pc Poplar Pc crystallises in the orthorhombic
More information9/29/2014 8:52 PM. Chapter 3. The structure of crystalline solids. Dr. Mohammad Abuhaiba, PE
1 Chapter 3 The structure of crystalline solids 2 Home Work Assignments HW 1 2, 7, 12, 17, 22, 29, 34, 39, 44, 48, 53, 58, 63 Due Sunday 12/10/2014 Quiz # 1 will be held on Monday 13/10/2014 at 11:00 am
More informationA - Transformation of anatase into rutile
Exercise-Course-XRD.doc 1/12 04/06/2012 A - Transformation of anatase into rutile Anatase and rutile are two distinct phases of titanium dioxide TiO 2. The stable phase is rutile. 1. Structural study Anatase:
More informationTHE EVALUATION OF QUARTZ RESONATORS VIA X-RAY DIFFRACTION TOPOGRAPHY
THE EVALUATION OF QUARTZ RESONATORS VIA X-RAY DIFFRACTION TOPOGRAPHY INTRODUCTION K. G. Lipetzky and R. E. Green, Jr. Center for Nondestructive Evaluation The Johns Hopkins University Baltimore, MD 21218
More informationLecture C4b Microscopic to Macroscopic, Part 4: X-Ray Diffraction and Crystal Packing
Lecture C4b Microscopic to Macroscopic, Part 4: X-Ray Diffraction and Crystal Packing X-ray Diffraction Max von Laue won the 1914 Nobel Prize for his discovery of the diffraction of x-rays by crystals.
More informationX-RAY DIFFRACTION CHARACTERIZATION OF MOVPE ZnSe FILMS DEPOSITED ON (100) GaAs USING CONVENTIONAL AND HIGH- RESOLUTION DIFFRACTOMETERS
77 X-RAY DIFFRACTION CHARACTERIZATION OF MOVPE ZnSe FILMS DEPOSITED ON (100) GaAs USING CONVENTIONAL AND HIGH- RESOLUTION DIFFRACTOMETERS T.N. Blanton 1), C.L. Barnes 1), M. Holland 1), K.B. Kahen 1),
More informationHow to Analyze Polymers Using X-ray Diffraction
How to Analyze Polymers Using X-ray Diffraction Polymers An Introduction This tutorial will cover the following topics How to recognize different types of polymers Crystalline, semi-crystalline and amorphous
More informationInfluence of Bulk Graphite Thickness on the Accuracy of X-Ray Diffraction Measurement. I. Introduction
Influence of Bulk Graphite Thickness on the Accuracy of X-Ray Diffraction Measurement Jane Y. Howe 1*, Burl O. Cavin 1, Amy E. Drakeford 2, Roberta A. Peascoe 1, Tracy L. Zontek 2, and Douglas J. Miller
More informationDIFFRACTION METHODS IN MATERIAL SCIENCE. PD Dr. Nikolay Zotov Tel Room 3N16.
DIFFRACTION METHODS IN MATERIAL SCIENCE PD Dr. Nikolay Zotov Tel. 0711 689 3325 Email: zotov@imw.uni-stuttgart.de Room 3N16 Lecture 7 OUTLINE OF THE COURSE 0. Introduction 1. Classification of Materials
More informationDefect depth profiling of CdZnTe using high-energy diffraction measurements
Defect depth profiling of CdZnTe using high-energy diffraction measurements M.S. Goorsky, a H. Yoon, a M. Ohler, b K. Liss b a Department of Materials Science and Engineering University of California,
More informationAGING OF EXPLOSIVE CRYSTALS (RDX) INVESTIGATED BY X-RAY DIFFRACTION
1 AGING OF EXPLOSIVE CRYSTALS (RDX) INVESTIGATED BY X-RAY DIFFRACTION Michael Herrmann, Manfred A. Bohn Fraunhofer Institut für Chemische Technologie ICT, Pfinztal, Germany ABSTRACT Coarse and fine particles
More informationAtomic Densities. Linear Density Number of atoms per length whose centers lie on the direction vector for a specific crystallographic direction.
Atomic Densities Linear Density Number of atoms per length whose centers lie on the direction vector for a specific crystallographic direction. Planar Density Number of atoms per unit area that are centered
More informationAn Investigation of Non-Crystalline Materials Using X-ray Powder Diffraction. PPXRD 12 Beijing May 2013 Simon Bates: Triclinic Labs
An Investigation of Non-Crystalline Materials Using X-ray Powder Diffraction PPXRD 12 Beijing May 2013 Simon Bates: Triclinic Labs 1 This document was presented at PPXRD - Pharmaceutical Powder X-ray Diffraction
More informationPossibilities and limitations of X-ray diffraction using high-energy X-rays on a laboratory system
Z. Kristallogr. Suppl. 30 (2009) 163-169 / DOI 10.1524/zksu.2009.0023 163 by Oldenbourg Wissenschaftsverlag, München Possibilities and limitations of X-ray diffraction using high-energy X-rays on a laboratory
More informationCHAPTER 7 MICRO STRUCTURAL PROPERTIES OF CONCRETE WITH MANUFACTURED SAND
99 CHAPTER 7 MICRO STRUCTURAL PROPERTIES OF CONCRETE WITH MANUFACTURED SAND 7.1 GENERAL Characterizing the mineralogy of the samples can be done in several ways. The SEM identifies the morphology of the
More information