Instrumentation and Measurements (XRD) Dr. Christophe Fontugne R&D Instrument manager MAUD 2018 November 26, 2018 The world leader in serving science Proprietary & Confidential
Sum m ary Presentation of ThermoFisher X-ray part (very quick) Interaction X-ray and matter (no maths, good for digestion) XRD basics Powder Thin Layer Stress Texture XRD setup : Some important parameters defining an instrument Some real XRD examples : Dynamic studies on Equinox 100 Combined XRD/XRF on Equinox 100 Phase transition at (not very) high temperature on Equinox 3000 Texture/Stress Combination on Equinox 6000 Proprietary & Confidential 2
70,000 5,000 $1B $24B employees R&D scientists/engineers invested in R&D in revenues The world leader in serving science Proprietary & Confidential 3
Our leading scientific products, services and workflow solutions The world leader in serving science Analytical precision and Inspiring meaningful Accelerating discovery One-stop access for Instrument and diagnostic excellence genetic analysis research scientific products enterprise services Proprietary & Confidential 4
We take pride in our Mission We enable our customers to make the world healthier, cleaner and safer Proprietary & Confidential 5
Our customer value proposition Technology Digital science based capabilities partnership Production R&D Companion outsourcing optimization diagnostics development We help our customers accelerate Laboratory Supply chain Customer flow and management innovation and enhance efficiency productivity , underpinned by quality . Clinical trial Exclusive & manufacturing tools and applications services Compliance Outsourced to defined enterprise standards services Assurance of supply quality and resilience Proprietary & Confidential 6
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Thermo Scientific XRF and XRD Product Portfolio : Strong And Complementary Technologies (>4000 customers ) Stand-alone Integrated XRF EDXRF WDXRF Powder XRD and XRD ARL QUANT’X Top performance ARL PERFORM’X bench-top EDXRF High performance ARL 9900 Series sequential XRF Integrated XRF-XRD ARL EQUINOX Series from benchtop XRD to advanced research XRD ARL OPTIM’X: Surprising performance in WDXRF XRD: Analysis of structure, XRF: Elemental analysis crystallography phases or compounds Proprietary & Confidential 8
Therm o Fisher Scientific – I nel Brand Therm o Fisher Scientific – XRD research Z.A. C.D. 405 45410 ARTENAY , France T + 33 (0)2 3880 4545 F + 33 (0)2 3880 0814 Key figures Creation : 1974 of INEL SAS INEL integrates Thermo Fisher in Feb. 2016 Staff 2015 : 20 employees 80% technically qualified (PhD, Engineers and technicians) Staff seniority average: 10 years Resources All technical and human resources are situated in our headquarter in France : • Research & Development, technical assistance • Informatics tools development & assistance • Mechanical parts design & metrology • X-Ray diffraction systems assembling • Installation & After Sales Services for instrumentation • Components and electronic cards design & integration Proprietary & Confidential 9 9
Wave-matter interaction e - λ When a photon does encounter an atomic particle, it transfers energy to the particle. The energy may be reemitted back the way it came (reflected), scattered in a different direction or transmitted forward into the material. Proprietary & Confidential 10
I nteraction w ave-m atter The energy of photons used for optical spectroscopic measurements of various quanta EHz : exahertz (10 18 ) - ZHz : zettahertz (10 21 ) - YHz : yottahertz (10 24 ) Proprietary & Confidential 11 11
W ave-m atter interaction X-rays Production : classically by excitation of external electronic level with electron beam Bragg's law λ = d sin 2 θ θ θ d Proprietary & Confidential 12 12
X-Ray Diffraction basics (1/3) • Planes of atoms act like a diffraction grating • Constructive & destructive interference lead to peaks in scattered intensity • Values of λ & d determines 2 θ Bragg’s law : n λ = 2d sin θ • Where • n = order of radiation • λ = wavelength of radiation • 2d = latice spacing of crystallites in the powder sample for XRD • θ = Bragg angle Proprietary & Confidential 13
X-Ray Diffraction basics (2/3) Peak position d-spacings Peak intensity nature and atomic positions in planes With XRD we measure distances... … nothing more Chemical composition Phases Structure ….. Proprietary & Confidential 14
X-Ray Diffraction basics (3/3) Without a Database we can DATABASE not do much... Pattern DATABASE Source : wikimedia Halite (NaCl)... ... should give this pattern Proprietary & Confidential 15
One important issue with XRD : isomorphism This is one real issue with XRD Pattern AgS 2 Sb has the same structure as NaCl !!! A complementary technique sensitive to chemistry is helpful (XRF…) Proprietary & Confidential 16
THIN LAYER (GiXRD) Proprietary & Confidential 17
What is called thin layer Issue 1 GiXRD (or thin layer) is used to see Issue 3 the first few nm to µm of sample surface…. To control Often quality of penetration signal is poor depth of X-Rays due to a lack of cristallinity Layer Substrate Issue 4 Issue 2 Sometimes detector Speed : if layer dynamic … Therefore at least motorized is really thin required is omega and Z are required (thin (few nm) really high layer attachement or Equinox 5000 (epitaxial or 6000) layers) Proprietary & Confidential 18
Information obtained 1/2 • XRR (X-Ray Reflectometry) X-Ray Reflectivity curve X-Ray Reflectivity curve 5nm Nb layer 10nm Ni layer • Bump spacing : information on thickness • Bump decay : information on roughness (angstrom scale) • Thin is easy (less than 300 nm) thick is very difficult. Unique feature for a desktop instrument Proprietary & Confidential 19
Information obtained 1 / 2 … continued Stack of 128 W/Si layers on Silicon substrate W = 1.1nm Si = 2.2nm Proprietary & Confidential 20
Information 2/2… Diffraction of course 4µm Ni layer on Iron Ω increases Proprietary & Confidential 21
What is Epitaxie? Thin layer but with nearly same structure as a single crystal. Au on TbPC2 Proprietary & Confidential 22
STRESS Proprietary & Confidential 23
What is (residual) stress • A simple cubic structure 2 θ d Is always Is always d the same the same d d Proprietary & Confidential 24
Some violence…… Sample larger than before DEFORMATION Sample smaller than before Proprietary & Confidential 25
…. At atomic level d d1 d d d2 d3 d1 < d < d2 & d3 d2 = d3 in case of uniaxial stress d changes implies that 2 theta changes Proprietary & Confidential 26
Just for fun Texture measurement Using Precix robotic system Proprietary & Confidential 27
TEXTURE Proprietary & Confidential 28
What is called texture? Powder or random texture Preferred orientation / texture Texture means classically deviation from random texture Proprietary & Confidential 29
Why do we have texture sometime Extrusion Cold rolling And many other things…. Geology Proprietary & Confidential 30
Instrument Instrument is designed to retrieve the information we are looking for. It allows to measure and quantify physical parameters (length, weight, power, energy, time…) Proprietary & Confidential 31
X-ray diffraction setup Elastic coherent interaction : reflectometrie : investigation on thin film for measuring thickness, roughness and density diffraction : investigation on phases absorption : imaging and radiography. Incoherent elastic interaction : diffusion by a rough surface or cristalline defects. => instrumental configuration adapted according to: Grazing - type of measurement Diffraction measurements - type of sample Powder, - accuracy of the result bulk 2D fibres, bulk Powder, 2D or 3D fibres, bulk Small angle measurements 2D Instrument Environment X-ray optic sample Detection Source Performances depends on the instrumental function Proprietary & Confidential 32
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