The ID27 beamline at the European Synchrotron Radiation Facility ...

The ID27 beamline at the European Synchrotron Radiation Facility:High Pressure Diffraction and High Pressure TomographyMSc. Michelle Jenice Alvarez Murga 1,21. ID27, Dynamics and Extreme Conditions Group, European Synchrotron Radiation Facility, Grenoble, France2. Institut Néel CNRS-UJF, Structure et Propriétés des Matériaux – Conditions Extrêmes, Grenoble, FranceFirst Mexican Synchrotron Radiation User’s Meeting

Science at Extreme Conditions: multidisciplinary researchIn the last 5 years of operation ID27 has produced:•168 peer reviewed publications in different areas of research of which 15% appeared in “highprofile journals” with “Impact Factors” greater or equal than Physical Review Letters•1 publication/experiment in average (1/3 of them from in-house research or strongcollaborations)First Mexican Synchrotron Radiation User’s Meeting

ID27 staff: High Pressure Diffraction expertsM. MezouarBeamline responsibleG. GarbarinoBeamline scientistLow TemperaturesP.BouvierCollaborator scientistRamanS.BauchauBeamline TechnicianA. SalamatPostdoctoral fellowChemistry and LaserHeating in DACS. PetitgirardPostdoctoral fellowResistive Heating andLarge Volume PressM. Alvarez-MurgaPhD studentTomography and LargeVolume PressFirst Mexican Synchrotron Radiation User’s Meeting

ID27 advanced sample environment•Diamond anvil cell :P>300 GPa, 5

ID27 Low T sample environment•Commercial He flow cryostat by OxfordInstalled since September 2007T ≥ 4K•In-house made He flow cryostatInstalled since September 2010T ≥ 3K, (20 min to 5K, 0.35l/h@15K)Both cryostats are completely automatedpermanent facilities @ ID27 and offerpossible Raman measurements and othertechniques (transport & magnetic)Specially designed for single crystalhigh pressure experiments at low T(sphere of confusion

ID27 detectorsA good detector for high pressure must fulfill the following criteria:- a large input surface (>150 mm diameter)- high spatial resolution- high dynamic range (14 bits or more)- good sensitivity, even at high X-ray energies (60-80 keV)- fast reading (a few seconds or less)MAR CCD: 165 mm diameter14 bits dynamic range; readout time 4sLow sensitivity at high X-ray energiesMar345 on-line image plate: 345 mm diameter14 bits dynamic range; readout time 60 sHigh sensitivity at high X-ray energiesFirst Mexican Synchrotron Radiation User’s Meeting

The ID27 beamline experimental setups•Infrastructure:2 dedicated hutchesEH1: Paris-Edinburgh press, Low T and resistively heated diamond anvil cellsEH2: YAG and CO2 laser heating (extra-space for complementary equipments)2 dedicated laboratories (DAC/Paris-Edinburgh cell)First Mexican Synchrotron Radiation User’s Meeting

Paris-Edinburgh SetupFirst Mexican Synchrotron Radiation User’s Meeting

Low T diamond anvil cell setupFirst Mexican Synchrotron Radiation User’s Meeting

Double-sided laser hetaing systemFirst Mexican Synchrotron Radiation User’s Meeting

Strong collaboration with the ESRF sample environment unit:J. Jacobs and P. VanderlindenState-of-the-art offline equipments to perform the mostchallenging cell loadings on-siteHigh Pressure LabLaser Drilling MachinesGas Loading SystemFirst Mexican Synchrotron Radiation User’s Meeting

Summary of ID27 capabilites40002500Temperature vs. Pressure diagram – HP/HT technologiesavailable at ID27Laser heating1200T (K)600300100PE-cellresistive heating (external)He cooling0.2 3P (MBar)+ Time resolutionFirst Mexican Synchrotron Radiation User’s Meeting

Some examples of daily science at ID27• Physics,Chemistry,Biology …• Powder and single crystal structural characterization• Phase transitions• Melting curves• New material synthesis• Effect of pressure on chemical bonds: neighborsdistances, coordination number, angles...• Structural relations between polymorphs in the solidand liquid states at high pressure are poorlyunderstood.P=138 GPaMetallic O 2• Geophysics• Determination of planets cores structures• Effect of light elements• Water in the Earth’s upper mantle• Magmas...First Mexican Synchrotron Radiation User’s Meeting

Future of the beamline•Keep a high level of user and in-house research support•Install a new faster, more efficient, high energy planar detector(pixel or flat panel detector)•Develop new type of experiments−In situ micro and nano-XRF in the double laser heated DAC−In situ micro XRD tomography in the rotative PE press⇒Transform ID27 into a long beamline (3 rd experimental hutch at~100 meters from the source)First Mexican Synchrotron Radiation User’s Meeting

In situ micro XRD tomography (XRD-CT) in the rotative Paris-Edinburgh pressSince the end of 2009, ID27 team has engaged important efforts to developin situ diffraction tomography (XRD-CT) studies under high pressure.The work of Michelle Alvarez thesis project is to develop the ID27-EH1tomography setupPRINCIPLE: tomography uses penetrating X-rays to exploit a specific contrast(absorption, fluorescence, diffraction ) and reconstruct an image from high resolution2D angular projections.HOW TO COUPLE THIS WITH HIGH PRESSURE?To achieve this, a new rotating tomography ParisEdinburgh cell with an angular acess of 180°hasbeen constructed and will be tested in June 2011.First Mexican Synchrotron Radiation User’s Meeting

‘Ambient conditions’ experimental setupXRD-CT uses X-raymicrobeams to maplocal crystallineproperties like phase,texture (orientation),lattice strain and defectdensity in threedimensions (3D)FluorescenceImagingωyBeamzX-ray focusing opticsStructural ImagingyxAbsorption ImagingP. Bleuet, et al. Nature Materials, 7:468-472, June 2008.First Mexican Synchrotron Radiation User’s Meeting

What do we get as result?...example on C602D pattern recovery (by projection)The demonstration, carried out on a high pressure quenchedC60 sample, reveals a new ill-ordered carbon phase with shortinterlayer distance (3.11 Å) and evidences concentric spatialdistribution of diamond, sp3 amorphous diamond and sp2graphite-like carbon.3D Structural phase map(A)The scanned dimensions are 1320 m length and 184 mthickness. The voxel size is (2.3×2.3×1.6 µm3).(B) The scattered intensity is rendered as a function of the realsample coordinates (x, y, z)M. Alvarez-Murga et al., Submitted (2011).Phase-Spatial selective scattering analysis. (A) experimental(black) and calculated (red) selectively recovered scatteringpatterns and 2D (x, y, zi) reconstructions of(1) full sample cross-section(2) glass capillary amorphous signal(3) amorphous sp3-like carbon phase(4) cubic diamond “D” Fd-3m a=3.565(1)Ǻ(5) new ill-ordered carbon phase “S” with short interlayer distance3.114(1)Ǻ(6) sp2-like carbon “G” with interlayer distance 3.420(1)Ǻ

Lattice d-spacing mapsM. Alvarez-Murga et al., Submitted (2011).Here, we report the development of scattering resolved tomography by including the Bragg angle (2θ) as fourth dimension of aX-ray diffraction computed tomography experiment (x,y,z). This extension enables the 3D mapping of strain (lattice spacingcontrast) . In this case lattice d-spacing maps allow discrimination of different strained diamond crystallites in the core of thesample with a high accuracy.2D (x, y) lattice d-spacing maps of diamond phase(a) 2D reconstructions obtained at three different 2positions on the (311) cubic diamond reflection: lowfwhm (yellow), center-fwhm (orange), high-fwhm (red).The squares indicate the zones of the sample thatwere used to extract 1D scattering patterns.Inset: The scattered intensity is rendered as a functionof real sample coordinates (x, y, z) for different (i =1n)Bragg angles.(b) 2D lattice d-spacingmaps using (111), (220), (311),(400) and (331) diamond reflections.(c) Calculated lattice d-spacing, of selected areas(same as in a).(d) Histogram of lattice d-spacingdistribution of theseanalyzed areas.First Mexican Synchrotron Radiation User’s Meeting

Rotative Paris-Edinburgh pressHP-HT spatially resolved structural studies will help to clarify long-standing issues ofinhomogeneous phase transformation, local grain growth and elastic anisotropy, until nowinvestigated by classical HP-HT XRD and ultrasound velocities.[1]« New generation of large volume cells for research under extremeconditions» High Pressures network Project CNRS 2009 – MRCT 2010-11.[2] Proposal MI-1086 Insitu X-ray Micro-Diffraction Computed Tomography(XRD-CT) under extreme conditions using a new rotation tomography Paris-Edinburgh cellSpecial thanks to Yann Le Godec and Julien Phillipe from IMPMCFirst Mexican Synchrotron Radiation User’s Meeting

Future in situ XRD-CT experiments on ID27…This technological development willprovide new scientific opportunities fororiginal and unique studies of phasetransitions, density, crystallization anddeformation in extreme environments.in situ diffraction tomographyin situ absorption tomographyMeasure glassdensities underpressurein situ deformation and radiographyCEA Tours : energetic materials subjected topressure and shear stress.¨We wish to characterize our materials in poredistribution and crystal structure according tothe different stresses applied…¨First Mexican Synchrotron Radiation User’s Meeting

Thank you for your attentionContact information: michelle.alvarez@esrf.frMichelle AlvarezM.Sc. Materials Science and EngineeringPhD Student, Dynamics and Extreme Conditions GroupID27 - High Pressure BeamlineEuropean Synchrotron Radiation Facility - ESRF6 rue Jules Horowitz, B.P. 220, F-38043 Grenoble Cedex, FranceTel: +33 (0)4 76 88 23 17Institut Néel CNRS-UJFStructure et Propriétés des Matériaux – Conditions Extrêmes25 Avenue des Martyrs, B.P. 166, F-38042 Grenoble Cedex, FranceTel: +33 (0)4 76 88 74 23First Mexican Synchrotron Radiation User’s Meeting

Michelle Alvarez CV2009-201220062004-2007M1 Internship2008Chemical EngineeringProcess Engineer inmicroelectronicsHP-HT synthesisPhD thesis on ID27In situ micro-XRD-tomography ofheterogeneous high pressurehightemperature forms of C60Thesis directors:Mohamed MezouarJean-Louis HodeauM2 Internship2009Multiferroics and Fe-Asbased superconductorsDiffraction-TomographyMethod

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