The PEEM-3 Photoemission Electron Microscope at the Advanced Light Source
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1 The PEEM-3 Photoemission Electron Microscope at the Advanced Light Source Andreas Scholl Introduction Advanced Light Source PEEM-3 Cryo-PEEM X-ray Linear Dichroism (XLD) Examples SRRC, Taiwan 2010
2 J. Stöhr, SLAC 2005 Ultrafast Dynamics and Nano Science
3 X-ray Spectromicroscopy
4 Applications of X-PEEM Main applications of X-PEEM that differentiate it from TXM techniques: Magnetism, structure, electronic properties of single crystalline, epitaxial materials Study of surface properties, ultrathin films, growth, catalysis. Electronic structure using (AR)PES. Fast surveying at high resolution, time domain imaging. Cryogenic PEEM of surfaces. Properties of nanostructures requiring thick supports. Other applications: Nanostructures (magnetism, composition, etc.) Ultrafast dynamics, pump probe studies
5 ALS PEEM-3 User Program Distribution of beamtime proposals Spring 2011 (out of 31). Materials Magnetism Materials not Magnetism Ferroelectric, Multiferroics Nanostructures Cryogenic PEEM Time-resolved PEEM
6 Beamline Variable linear and circular polarization High flux density using microfocusing (down to 10x10 microns) VLS plane grating monochromator Energy range 160 to 2000 ev with E/dE~4000 Undulator, monochromator are shared. PEEM has about 60% of the beamtime.
7 Advanced Light Source: PEEM-3 Transfer system and loadlock Preparation chamber Beamline Microscope Beamline staff: T. Young, A. Doran, A. Scholl Cooling CCD - Large machine with room inside to grow - Fully automated sample transfer system
8 A Look Inside the Microscope Single Straight Electron Column CCD Objective Lens X-rays Space for Mirror & Separator Sample Stage Optics laid out on an in-vacuum optical table. Facilitates easy upgrades and modifications. Triple layer Mu metal shields
9 Spatial Resolution Without aberration correction Element-resolved X-PEEM image of 25 nm thick Cr/Si layers. Simulation Aberration correction: 4-fold improvement of spatial resolution at a few % transmission (goal 10 nm) 10-fold improvement of transmission at several 10 nanometer spatial resolution. Using aberration correction
10 Staged Buildup of Aberration Corrected Endstation PEEM2.5 Mode Now CCD PEEM3 Mode Sample Addition of Dipole Separator and Mirror Section results in aberration correction and improved resolution Dipole separator Electrostatic mirror Electrostatic dodecapole Electrostatic Quadrupole CCD
11 Model of Aberration Correction Mechanical design complete, contingent on funding the corrector will be added in Back-focal-plane aperture 3-lens projector Field Twin Dodecapole Lens Water-cooled Dipole and Deflector Corrector Optics Transfer Lens Rail system Objective Lens Field Lens Optical Table Mirror Not shown: double magnetic/ electric dipole deflector
12 Liquid He-Cooled Sample Manipulator and Cartridges Cold sample holder with electro-magnet 6-strut 5-axis manipulator using fast PI stages and flexural joints. Large, easy to modify sample cartridges, suitable for fully automatic transfers. Piezo-driven strain stage
![Cooling Performance Helium Nitrogen 300 250 Temp [degk] 200 150 100 50 Spring-loaded Cu clamps grab a polished Si nose mounted on a massive Cu sample cover.](/docs-images/89/100796461/images/13-0.jpg "A one inch sapphire electrically isolates the sample. Co braids are used for vibration isolation.")
13 Cooling Performance Helium Nitrogen Temp [degk] Spring-loaded Cu clamps grab a polished Si nose mounted on a massive Cu sample cover. A one inch sapphire electrically isolates the sample. Co braids are used for vibration isolation. 0 00:00 00:10 00:20 00:30 00:40 00:50 01:00 01:10 01:20 01:30 Time Temperature as function of time using liquid He cooling. Lowest temperature reached: 16 K.
14 Applications of Cryo-PEEM Antiferromagnetism of high Tc superconductors (pnictide) Antiferromagnetism and charge, orbital order in CMR materials Antiferromagnetic vortices in CoO, NiO Interface exchange coupling in perovskite FM/AFMs Dilute magnetic semiconductors Ferroelectrics, multiferroics
15 Total Electron Yield edge white line J. Stohr, H. Siegmann: From Fundamentals to Nanoscale Dynamics
16 X-ray Linear Dichroism (XLD) ΔI XLD I charge Q zz (1 3cos 2 ( θ)) + I magn M 2 (1 3cos 2 ( ϕ)) charge (natural) linear dichroism magnetic linear dichroism θ E ϕ E M Q zz Magnetic and charge contribution need to be separated.
17 Linear Dichroism of a Partially Filled d-electron System Linear Charge Dichroism in a d-electron system C. T. Chen et al. PRL 68, 2543 (1992)
18 X-ray Magnetic Linear Dichroism (XMLD) Angle dependence ~ cos 2 θ
19 XMCD and XMLD Imaging of Ferromagnets and Antiferromagnets Spectroscopy Co Co LaFeO 3 Microscopy Ferromagnet XMCD TEY (a.u.) L 3 L 2 s Photon energy (ev) LaFeO 3 XMLD TEY (a.u.) B A E Photon energy (ev) F. Nolting et al., Nature 2000
20 Competing Interactions in FM/AFM Perovskite Superlattices LSFO/LSMO multilayers (70/30) F. Yang, Y. Takamura, et al., UC Davis AFM FM STO LSFO LSMO LSFO LSMO LSFO LSMO Spin flop coupling (BL 4, ALS) Takamura, Y., F. Yang, N. Kemik, E. Arenholz, M.D. Biegalski, and H.M. Christen, Physical Review B 80, (2009).
21 Xrays <100> Angle Dependent XMLD Contrast at Room Temperature LSMO is paramagnetic Experimental and simulated contrast Xrays <110> LSFO is antiferromagnetic AFM axis is along the in-plane <100> directions. Neither in a {111} plane (easy plane of LSFO) Nor along <110> direction (easy axis of LSMO) linearly polarized x-rays e - Rotate sample
![10 [6x6]10 x-rays Domain correlation and spin-flop coupling.](/docs-images/89/100796461/images/22-1.jpg "Both LSMO and LSFO magnetic moments align along <100>. T=38K")
22 XMCD and XMLD Below Tc of LSMO Mn FM Domains Fe AF Domains M Mn A Fe Strong contrast 10 white Weak contrast black 10 [6x6]10 x-rays Domain correlation and spin-flop coupling. Both LSMO and LSFO magnetic moments align along <100>. T=38K
23 Magnetic Domain Formation in LSMO/LSFO multilayers Fe AFM are mobile while cooling through the LSMO Curie temperature. Crystal twin domains strongly pin AFM domains in thick single layers. Formation of large regions with preferred axis below the STO cubic to tretragonal transition at about 105 K.
24 X-ray Linear Dichroism Imaging Structure and formation of bio-minerals Gilbert group, U Wisconsin BiFeO 3, a room temperature multiferroic material R. Ramesh group, UC Berkeley
25 Linear Dichroism Study of Aragonite R. Metzler, D. Zhou, M. Abrecht, S. Coppersmith, P. Gilbert University of Wisconsin Nacre: Goal: 95% aragonite (CaCO 3 ), + 5% organic matrix 3000x more resistant to fracture than aragonite - Determine the nacre microarchitecture (crystal orientation) - Nacre formation mechanism Light microscopy image of nacre. x ray linear dichroism as function of angle between linear x ray polarization and the c axis of aragonite.
26 Linear Dichroism Imaging of Nacre X-ray linear dichroism images as function of polarization angle EPU: Full polarization control 4 μm X-ray linear dichroism (XLD) images at horizontal, vertical and diagonal polarization show the columnar growth and the crystal orientation of nacre, mother-of-pearl. The contrast varies with angle between the linear x-ray polarization direction and the stacking direction of the tablets.
27 Haliotis iris Haliotis laevigata Atrinarigida Nautilus pompilius PEEM PIC PIC map PEEM PIC PIC map PEEM PIC PIC map PEEM PIC PIC map Nautilus pompilius Nacre, aragonite nacre Spherulitic aragonite Prismatic calcite
28 High resolution Ca and Mg mapping in the sea urchin tooth Pupa Gilbert et al. UW Madison PIC map reveals that the plates (arrows) are slightly mis oriented PEEM 3 data with 20 nm resolution Previous Ca and Mg mapping in sea urchin tooth from Robach et al. JSB 2006 (SIMS data, bars are 10 µm)
29 Electrical Control of Magnetism in Multiferroic Materials σ d Piezoelectricity ε χ E E P Magnetoelectricity α M χ M S Magnetoelasticity Multiferroics: Materials with simultaneous (anti-) ferro-magnetic, ferroelectric and/or ferroelastic ordering H Coupling between Different Ordering Parameters Intriguing Fundamental Science & Novel Design of Electronic Devices (i.e. Electrically Controllable Ferromagnet) Measure the magnetization microscopically
30 Magnetic Structure of BiFeO 3 Films BiFeO 3 - Ferroelectric antiferromagnet P P (μc/cm 2 ) Bulk T C ~ 1103K T N ~ 643K Bi Fe O M Applied Voltage (V) M Ederer and Spaldin, PRB 71(2005) Magnetic plane is believed to be perpendicular to the polarization direction. This sample: 600 nm BiFeO 3 / SrRuO 3 / SrTiO 3
31 Polarization Direction in BiFeO 3 (001) (001) + P v + P v P v + 1 P v 4 Fe Bi P v 3 P v 4 P v 2 P v 1 Polarization points in one of 8 possible {111} directions.
32 X-ray Magnetic (Linear) Dichroism Spectroscopy Co Co LaFeO 3 Microscopy Ferromagnet XMCD TEY (a.u.) L 3 L 2 s Photon energy (ev) LaFeO 3 XMLD TEY (a.u.) B A E Photon energy (ev) F. Nolting et al., Nature 2000
33 Domain Structure of BiFeO 3 Imaged Using X-ray Linear Dichroism PEEM (a) PEEM x-ray linear dichroism at Fe L 2 edge PFM E E PFM E contrast reversal proves dichroic origin images match PFM images of FE structure magnetic or charge dichroism? 10 8 μm 2 T. Zhao et al., Nature Materials 5, 823 (2006)
34 Natural Linear Dichroism in PbZrTiO 3 E Charge dichroism! 2.0 vertical lines outside lines Horizontal a domains a.u Out-of-plane polarization contrast 2.0 square outside in-plane a.u. 1.5 C.S. Ganpule et al., JAP 91, 1477 (2002) difference (a.u.) in-plane XMLD pol. contrast Photon energy (ev) XLD is indeed sensitive to ferroelectric structure.
35 Temperature Dependence Shows Contrast Dominated By Magnetism <M> T <M> T 2 <M 2 > T AFM FE? Normalized Order Parameter XLD #1 XLD #2 XLD #3 XLD #4 XLD #5 Bi Displacement Fe Displacement Polarization Out-of-plane lattice parameter T N <M 2 > T C Temperature (K) <M 2 >
36 Determine Antiferromagnetic Axis of BiFeO 3 <111> P M Six unique low index axes in (111) plane. linearly polarized e - Circularly (plane) polarized e - x-rays PEEM-3 Rotate sample x-rays PEEM-2 M. Holcomb et al., PRB 2010
37 linearly polarized Polarization Angle Dependence e- x-rays ~5 um FOV XLD Images M. Holcomb et al., PRB
38 Modeling the Angular Dependence bright dark 2nd bright 2nd dark Model (112 or 110 axis) Dichroic Contrast Angle dependent XMLD M. Holcomb et al., PRB 2010 Polarization
39 Antiferromagnetic Axis <111> P M Magnetic axis is either [11-2] or [1-10] in a [111] polarization domain for a (001) oriented thin film. ΔI XLD I charge Q zz (1 3cos 2 ( θ )) + I magn M 2 (1 3cos 2 ( ϕ)) Sign can be positive or negative making both [110] and [112] possible solutions. However: temperature dependence changes with sign.
40 E Domain contrast Temperature dependence Domain Contrast time Stack # Temperature dependence favors [11-2] direction M. Holcomb et al., PRB 2010 RT 220 C
41 Summary XNLD High spatial resolution XMLD 4 μm Photoemission Electron Microscopy Cryogenic temperatures XMCD, novel materials
42 The Future of X-PEEM Concentrate on our strengths: Study of materials, surfaces, thin films. Cryogenic studies, electronic structure. Fast full field imaging. Elmitec Our next steps: Modest improvement in spatial resolution Large improvement in transmission Flexible sample environment Improved user-friendliness Specs Commercial options available
43 STXM, PEEM or something else? Selection needs to be driven by the user community Should be a work-horse type experiment not a totally new concept with large risk PEEM and STXM communities have some overlap strength of PEEM in materials, epitaxial systems strength of STXM: very versatile, only drawback is the requirement in thickness My recommendation: To broaden the user community: STXM To deepen and empower the current community: PEEM SPEM: Need to go all the way towards mev energy resolution, competitive k resolution, cooling, sample prep. This is very challenging. Do both but probably STXM first, if a strong user community exist. Staffing and technical resources is an important concern. User support, and technical development is never finished.
44 The Future of X-PEEM Concentrate on strengths: Study of materials, surfaces, thin films. Cryogenic studies, electronic structure. Fast full field imaging. Elmitec Next steps: Modest improvement in spatial resolution Large improvement in transmission Flexible sample environment Improved user-friendliness Options for AC correction: Home-built, Specs, Elmitec Resolution: similar, sub 10 nm probably Sample environment: home built or a modified commercial PEEM has advantages User-friendliness: Requires software development beyond what vendors offer. Specs Commercial options available
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