ArabLab 2018 Chemical and Structural Analysis of Materials using XRF and XRD Didier Bonvin, Nazih Ziade, Dr.Simon Welzmiller and Dr. Ravi Yellepeddi Thermo Fisher Scientific Switzerland The world leader in serving science Proprietary & Confidential
Advanced materials in our lives Nanomaterials Composites Biomaterials Energy Polymers Materials Ceramic & Metals & Alloys Glass Electronics & Photonics Proprietary & Confidential 2
A variety of complementary techniques used for Chemical and Structural analysis of Materials SEM TEM IR Multi-Modal RAMAN XRD XRF FT-IR XPS EDS WDS CT Proprietary & Confidential 3
Enabling the Materials Development Cycle CHARACTERIZE Structure Composition Properties • Electron Microscopy • MS; quantitative, destructive • Particle size • SPM • EDS , XRF (Elemental) ; XPS (surface) • Thermal • XRD • Raman; molecular, hard samples • Rheological • FTIR • Multimodal Techniques: - Rheo-Raman, XPS-Raman Proprietary & Confidential 4
Materials Science Multi-Modal, Multi-Scale Workflow Chemical Analysis Selection of Area of Interest TEM prep Atomic Structure Meter Millimeter Micrometer Nanometer Atomic UltraDry EDS Detector ARL QUANT'X EDXRF Spectrometer DXR 2Xi Raman Imaging ARL Microscope FEI Helios G4 CX Thermo Scientific PERFORM’X K-Alpha+ XPS XRF Nicolet iN5 iXR Raman Spectrometer Microscope FEI Themis Z TEM ARL EQUINOX XRD Proprietary & Confidential 5
WDXRF, EDXRF and XRD: Elemental and Phase analysis of a variety of materials • Cement and building materials • Metals, Slags • Petroleum, Polymers, Oils • Ores and raw materials • Chemicals/Pharmaceuticals • Geology • Environmental • Food products • Mining extraction • Universities, central labs • Thin films, magnetic media, paints • Etc.. Proprietary & Confidential 6
Wave – Matter Interaction Diffusion X-rays Production : classically by excitation of Reflection external electronic level with electron beam XRD Imaging Diffraction XRF Fluorescence Proprietary & Confidential 7
Thermo Scientific XRF and XRD Product Portfolio Integrated XRF EDXRF WDXRF Powder XRD and XRD ARL QUANT’X - Top performance EDXRF ARL PERFORM’X Equinox 6000: High ARL 9900 Series High Performance performance Powder XRD sequential XRF Integrated XRF-XRD Equinox 100 & 1000 Benchtop XRD ARL OPTIM’X: Surprising XRD: Analysis of Portable Niton performance in WDXRF Structure-crystallography XRF: Elemental analysis Phase or compound Proprietary & Confidential 8
Geology/Mining/Core drilling: Laboratory and Field XRD Calcite, Quartz, Dolomite,Bauxite.. The problem The analysis The solution • Complete Mineralogical/Phase Geological exploration, mineral Use a Powder XRD to analysis in Bauxite, Alumina and other processing and raw material characterize the mineral content aluminum bearing minerals in few screening for industrial of any ore body and total seconds to minutes using Position production require identification geochemical analysis including Sensitive Detector and quantification of specific other techniques such as XRF • Qualitative and Quantitative Phase phases of economic interest in and FTIR. analysis using Rietveld programs addition to their chemistry EQUINOX 100 bench-top • High throughput with large 30-position (transportable) for field sample loader and unattended batch applications and EQUINOX operation 1000/3000 for Geochemical labs Proprietary & Confidential 9
Feldspar example: Elemental Mapping using XRF Proprietary & Confidential 10
Feldspar: XRF Data to represent the distribution of elements within the mineral sample Proprietary & Confidential 11
Crystallinity, Polymorphism and Structural finger printing of Pharmaceutical Products by XRD 250 s 0 s Indication of a Problem Analyze the Problem Solve the Problem Study and obtain the following Crystal structure of the active Very fast identification and information in few seconds to molecule in pharmaceutical screening of pharma products minutes: products is an important using EQUINOX 100 XRD can be • information for the synthesis done to establish various Time-dependent crystallization and application of new structural parameters and • %Crystallinity vs Amorphous formulations. Rapid screening characteristics in real time. • Polymorphism and their stability for polymorphism, crystallinity, Depending on the nature of the • Crystallite size and bio-availability stability and reproducibility of sample and quantity, both the formulations are routinely transmission and reflection mode • Reactivity to temperature and carried out by XRD. XRD can be done. environment Proprietary & Confidential 12
Dynamic studies of materials: Real-time structural changes captured by XRD Phase transition at high temperature 5s per pattern with multilayer mirror Equinox 3000 + HTK16 (Anton Paar) Indication of a Problem Analyze the Problem Solve the Problem Materials undergo structural Whether it is the crystallization of EQUINOX XRD technology is based changes as they are heated, pharmaceutical products or on real-time simultaneous detection of treated and/or stressed. Their transformation of an amorphous full pattern in few seconds to minutes reactivity and stability in controlled material into crystalline or vice and this enables dynamic studies of environment are also important for versa, real-time dynamic materials most efficiently. Even the their manufacturability and scaling- monitoring of their specific phases bench-top EQUINOX 100/1000 can be up from research to production. is required and XRD can be used used with different options to study to track such reactions and reactivity and kinetics of such Real-time changes need to be dynamics. materials in real time. captured for optimization and efficiency of the process Proprietary & Confidential 13
Structural simulations, molecular modeling and XRD pattern Indication of a Problem Analyze the Problem Solve the Problem Material Research Scientists From the initial chemical XRD is the fastest and most need to simulate and model the composition and atomic reliable technique for studying appropriate molecular structure coordinates, scientists need to structure-property relationship and to ensure the expected build a crystallographic model elucidate materials as a function of properties when the material is and iterate or refine the their final state. Rietveld programs synthesized. Structure structure until it matches (quantitative structural refinement of new or applied closely with the expected determination) are used in materials is a pre-requisite for molecular bonding/structure. conjunction with XRD and their optimization. EQUINOX XRD + MAUD programs are designed for such scientists. Proprietary & Confidential 14
Materials Science Research – Batteries & Fuel Cells - Spectroscopy The problem The analysis The solution Graphite, Lithium Ion and other Use the X-ray Diffraction system to Use XRD to determine • battery manufacturers need to check for the appropriate crystal % Crystallinity versus Amorphous ensure highest conductivity or structure, amorphous versus content of the active material to charge density of the materials crystallinity, specific orientation optimize the process • used. These properties are characteristics with diffraction pattern Identify and Quantify specific structure or orientation dependent (linewidth, intensity ratio of different polymorphic structures of interest and a consistent crystal structure or reflections) and thickness/homogeneity to increase the yield • alignment of conducting lattices is and density of thin films or layers Structural stability and repeatability essential to increase yield and in real-time to enhance lifetime • efficiency. Thickness, surface roughness and density of layers or coatings Proprietary & Confidential 15
XRF-XRD APPLICATIONS IN CEMENT INDUSTRY 1 Clay Iron ores 3 4 Kiln Minerals Aluminum Feed Quartz oxides 7 Additives: 2 Limestone Gypsum Dolomite phases Slag Fly ash Pozzolan Limestone Free lime 6 8 5 Cements Hot meal Clinker phases Langbeinite Periclase Proprietary & Confidential 16
XRF and XRD Applications in Mining and Mineral Extraction processes 1 FeTiO 3 3 Minerals in Ti0 2 ZrSiO 4 tailings Fe 2 O3 Fe 3 O 4 FeO etc. 2 ZrSiO 4 TiO 2 17
IRON and STEEL Process: Chemical and Phase Analysis by XRF and XRD Cast iron 3 4 Slags Fe 3 C CaO (free lime in slags) Fe-metallic Sinters Fe 2 O 3 1 Fe 3 O 4 FeO 2 CaCO 3 5 Fe-metallic FeO Fe total Raw Materials 1 2 3 4 Steel Making Hot Rolling Mill Processing 5 Cold Rolling Mill Steel Processing 18
INTEGRATED XRF-XRD Instruments for Process Control and Industrial Materials X-Ray X-Ray Fluorescence Diffractometry Proprietary & Confidential 19
Example of combined analysis: XRF results first XRF data Proprietary & Confidential 20
Example of combined analysis for process control: Chemistry and Mineralogy XRF data XRD data Proprietary & Confidential 21
Recommend
More recommend
