8/13/2019 National Physical Laboratory Strategy for Large Scale Facilities

1/1

QueensPrinterandControllerof

HMSO

,2013

.10696/1113

www.npl.co.uk

XMaS beamline at ESRF[1]

National Physical LaboratoryStrategy for Large Scale Facilities

Introduction

NPL is designing and building, in collaboration with x-ray and neutron large scale facilities around the world, new metrology systems to enable scientists from academia and industry toinvestigate and understand the coupling phenomena in ferroelectric and magnetoelectric materials. These include beamline devices and measurements kits, often associated with thedevelopment of advanced synchronisation and data reduction/analysis to enable complex experiments. Of particular interest are the cases where different techniques are combined in a singlein-situ experiment to perform real-time or stroboscopic measurements. New physics can therefore be investigated and both static and dynamic properties of functional materials can be trackedas function of various external stimuli (H, T, E, ).

References:

[1] J.Wooldridge,S.Ryding,S.Brown,T.Burnett,M.Cain,R.Cernik,R.Hino,M.Stewart,P.Thompson, Simultaneousmeasurement ofX-raydiffraction and ferroelectricpolarization dataas afunction ofappliedelectricfield and frequency,J. Synchrotron Rad.19,710-716( 2012).

[2] S.Ryding,R.Cernik,J.Wooldridge,T.Burnett,M.Stewart,C.Vecchini,M.Cain, A.Lennie,F. Yuan,C. Tang,P.Thompson,S imultaneousmeasurement ofX-ray powder diffraction and ferroelectric polarizationdata as a function ofapplied electric field at a rangeoffrequencies,Powder Diffraction J.,2013(in press)

[3] http://www.piezoinstitute.com/resources/wp1.php

I11 beamline at Diamond Light Source [2]

Incorporating traceable interferometricmeasurements in-situwith XRD willallow users of XMaS, for the first time, todirectly correlate the intrinsic (lattice, ionicdisplacement, ) and extrinsic (domainwall motion) piezoelectric response inpiezoelectric materials as function ofelectric field, temperature and magneticfield.

This new world unique metrology facilitywill therefore enable XMaS users to link themeasurement of strain between up to 8decades in length scales and will underpinthe development of novel piezoelectric

electronic devices, such as the Piezoelectric-Effect-Transistor (PET) under developmentby IBM (collaborators in this project), toenable More Than Moore strategyfor faster, low power transistors.

Time-of-Flight technique isintrinsically suited for time resolvedstudies. NPL is working together withthe WISH instrument team at ISIS-TS2(Rutherford Appleton Laboratory) toenable simultaneous real-time highresolution (powder and single crystal)diffraction and electric polarizationmeasurements.

This will extend the current(synchrotron) in-situ diffractioncapabilities to the study ofmagnetoelectric and multiferroicmaterials (with neutron scattering).

Moreover, the system will fit into thestandard ISIS sample environment,giving access to high magnetic fields(up to 14T) and temperatures from afew mK to a few hundred Kelvin.

Future plans:

Top panel: 2 plots of the cubic indexed 220 peak in PMNPTat 298 K as a function of applied E field cycled at 1 Hz from 0to 1 kV mm-1 (highest and lowest intensity data respectively)incremented in steps of 0.05 kV mm-1. Bottom panels: Fitsof the same peak at 0 and 1 kV mm-1. The intensity from themonoclinic phase is plotted in blue and the tetragonal phasein red. The model (green) shows very good agreement withthe total intensity (black) as shown by the difference curve atthe bottom in grey.

The function generatoris used to synchronizeand control experimentaldevices. The fast X-raydetector (APD) scans aroundthe sample in hkl space andcollects diffraction X-rays.The data are recorded as afunction of frequency on theultrafast digitalanalogueconverter MUSST card at thesame time as the electricaldata.

E field applied to the sample andcycled at 1 Hz (top), measuredelectric polarization (middle)and real time collected X-rayintensity (bottom) at the 200peak of PMNPT. Data were alsocollected at 0.01 and 0.1 Hz.

Diagram showing how the electrical

system interacts with the beamline I11system at Diamond.

Diffraction patter and Rietveld fit of data at E=0kVmm-1 stroboscopicallycollected at an electric field frequency of 0.01Hz.

PE loop for the 0.01Hz and 1Hz electric field f requencies and correspondingvolume changes of the tetragonal unit cell.

Initial drawing of the laser interferometer setup mounted on the XMaSdiffractometer

Future facility at XMaS:in-situinterferometer for nanostrain studies [3]

Future facility at ISIS:in-situ PE loop and time resolved high resolution diffraction for ferroelectricand magnetoelectric materials

Schematicsof theprinciple of operationof TOF-in-situ PEmeasurements:electric fieldfrequenciesequal to theneutronbeam pulsesfrequencies(10Hz).

An in-situPE loop measurement systemhas been successfully integrated atXMaS for the determination of thecrystallographic response to theapplication of dynamic E fields insingle-crystal ferroelectric materials.

Voltages as high as 10 kV ca n beapplied up to a maximum frequencyof 1 kHz.

The setup also allows samples to besimultaneously magnetized with a4 Tesla magnetic field.

An in-situPE loop measurementsystem has been integrated at I11beamline for the determinationof the crystallographic responseto the application of dynamic Efields in ferroelectric materials inpolycrystalline ceramic form.

Voltages as high as 10 kV c anbe applied up to a maximumfrequency of 100 Hz.

Data can be collectedstroboscopically (f > 0.125 Hz) or inreal time (f < 0.125 Hz).

Rapidly Oscillating Diamond Phase plate Flipper at XMaS beamline

Unique piezoelectric actuator based flexible hinge designed by NPL

Tested and assessed at NPL and in the metrology lab at ESRF

Commissioned on XMaS BM28, ESRF

Flipping the incident polarisation between +Pc and -Pc allows

synchronous detection.

Measurements made in both field directions

Minimise offsets and drifts

Reduction of the time needed to take XMCD measurements

Improves the signal to noise ratioX-ray absorption spectra of left (-Pc) and right (+Pc) circularly polarisedlight in a magnetic material taken in a magnetic field.

Ferroelectrics exhibit spontaneous polarisationbelow their Curie temperature and containareas of uniform polarisation known as domainswhich can be switched by the application ofan electric (E) field. These materials have manyapplications for actuators, sensors and switches.Ferroelectrics such as Pb(Mg

1/3Nb

2/3)O

3xPbTiO

3

(PMNPT) or PbZn0.53

Ti0.47

O3(PZT) exhibit

frequency dependent behaviour as well as highsensitivity to temperature, stress, electric field andhistory of poling. For these reasons, comparisonsbetween the crystallography and the ferroelectricpolarization are only possible when they aremeasured simultaneously, on the same sample.

Real time in-situ measurements of diffraction and ferroelectric polarization

Rapidly Oscillating Diamond Phase plate Flipper design: the yellowblocks represent piezoelectric materials.

C. Vecchini1, J. Wooldridge1, M. Stewart1, A. Muniz-Piniella1, T. L. Burnett1, M. Cain1,P. Thompson2,6, L. Bouchenoire2,6, S. Brown2,6, D. Wermeille2,6, O. Bikondoa2,7, C. Lucas2,6,

T. Hase2,7, S.Ryding3, R. Cernik3, A. Lennie4, F. Yuan4, C. Tang4, P. Manuel5, D. Khalyavin5

1) National Physical Laboratory,Hampton Road, Teddington,TW110LW,UK

2) XMaS,The UK-CRG,ESRF, BP 220,F-38043 GrenobleCEDEX,

3) School ofMaterials, Oxford Road,Manchester,M13 9PL,UK

4) Diamond Light SourceLtd., Harwell ScienceCampus, Didcot,OxfordshireOX110DE, UK

5) ISIS Facility,Rutherford Appleton Laboratory,Chilton,Didcot, OxfordshireOX110QX, United Kingdom

6) Department ofPhysics, University ofLiverpool, Liverpool,L693BX, UK

7) Department ofPhysics, University ofWarwick,Coventry CV47AL, United Kingdom