Transmission Electron Microscopy. J.G. Wen, C.H. Lei, M. Marshall W. Swiech, J. Mabon, I. Petrov

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1 Advanced Materials Characterization Workshop Transmission Electron Microscopy J.G. Wen, C.H. Lei, M. Marshall W. Swiech, J. Mabon, I. Petrov Supported by the U.S. Department of Energy under grants DEFG02-07-ER46453 and DEFG02-07-ER University of Illinois Board of Trustees. All rights reserved. Outline 1. Introduction to TEM 2. Basic Concepts 3. Basic TEM techniques Diffraction contrast imaging High-resolution TEM imaging Diffraction 4. Scanning-TEM techniques 5. Spectroscopy X-ray Energy Dispersive Spectroscopy Electron Energy-Loss Spectroscopy 6. Advanced TEM techniques Spectrum imaging Energy-filtered TEM 7. Other TEM techniques Low-dose; in-situ; etc. 8. Summary

2 Why Use Transmission Electron Microscope? Optical Microscope Transmission Electron Microscope (TEM) Resolution record by TEM GaN [211] 0.63 Å Resolution limit: 200 nm 100k ev electrons λ: Å A N is 0.95 with air up to 1.5 with oil γ = 0.66(C s λ 3 ) 1/4 Sample thickness requirement: Thinner than 500 nm High quality image: <20 nm < 500 nm Thin foil, thin edge, or nanoparticles Basic Structure of a TEM Gun: LaB 6, FEG 100, 200, 300keV Gun and Illumination part TEM Sample Objective lens part View screen Mode selection and Magnification part

3 How does a TEM get Image and Diffraction? TEM Incident Electrons Sample < 500 nm Objective Lens Back Focal Plane Back Focal Plane Structural info First Image Plane First Image Plane u v Morphology 1 _ = u v f Object Image Conjugated planes View Screen 1. Transmitted electron (beam) 2. Diffracted electrons (beams) Bragg Diffraction 3. Coherent beams 4. Incoherent beams 5. Elastically scattered electrons 6. Inelastically scattered electrons Basic Concepts High energy electron sample interaction Incident high-kv beam Specimen X-rays TEM Diffracted beam Coherent beam Transmitted beam Incoherent beam magnetic prism Inelastically scattered electrons

4 d Electron Diffraction I SOLZ FOLZ Diffraction ZOLZ θ Zero-order Laue Zone (ZOLZ) First-order Laue Zone (FOLZ). Bragg s Law 2 d sin θ = nλ Wavelength X-ray: about 1A Electrons: 0.037A High-order Laue Zone (HOLZ) λ is small, Ewald sphere (1/λ) is almost flat Ewald Sphere Electron Diffraction II Diffraction Diffraction patterns from single grain and multiple grains Tilting sample to obtain 3-D structure of a crystal Lattice parameter, space group, orientation relationship 50 nm Polycrystal Amorphous To identify new phases, TEM has advantages: 1) Small amount of materials 2) No need to be single phases 3) determining composition by EDS or EELS

5 Major Imaging Techniques Major Imaging Contrast Mechanisms: 1. Mass-thickness contrast 2. Diffraction contrast 3. Phase contrast 4. Z-contrast Mass-thickness contrast Imaging 1) Imaging techniques in TEM mode a) Bright-Field TEM (Diff. contrast) b) Dark-Field TEM (Diff. contrast) Weak-beam imaging hollow-cone dark-field imaging a) Lattice image (Phase) b) High-resolution Electron Microscopy (Phase) Simulation and interpretation 2) Imaging techniques in scanning transmission electron microscopic (STEM) mode 1) Z-contrast imaging (Dark-field) 2) Bright-field STEM imaging 3) High-resolution Z-contrast imaging (Bright- & Dark-field) 3) Spectrum imaging 1) Energy-filtered TEM (TEM mode) 2) EELS mapping (STEM mode) 3) EDS mapping (STEM mode) TEM Imaging Techniques I. Diffraction Contrast Image: Contrast related to crystal orientation Diffraction Contrast Image Many-beam condition [111] Kikuchi Map [112] [001] [001] [110] Two-beam condition Transmitted beam Diffracted beam Application: Morphology, defects, grain boundary, strain field, precipitates

6 Diffraction Contrast Image TEM Imaging Techniques II. Diffraction Contrast Image: Bright-field & Dark-field Imaging Sample Sample Objective Lens T D Aperture Back Focal Plane Diffraction Pattern Two-beam condition Bright-field Image First Image Plane Dark-field Image Bright-field Dark-field thickness TEM Imaging Techniques III. Thickness fringes and bending contour Electron Wave t /ξ g ξ g Extinction distance Howie-Whelan equation dφ 0 πi = φ dz g exp{2πisz} ξ g To distinguish them from intrinsic defects inside sample: Tilting sample or beam slightly Diffraction Contrast Image θ B 0 g Excitation error S = g Δθ S Thickness fringes Bending contour Increasing S S=0 S<0 S=0 Increasing S S>0 S>0 I θb θb Bright-field s -g 0 g

7 TEM Imaging Techniques II. Diffraction Contrast Image Two-beam condition for defects Howie-Whelan equation dφ 0 πi = φ dz g exp{2πi(sz+g.r)} ξ g Dislocations Use g.b = 0 to determine Burgers vector b Stacking faults Phase = 2 π g R Each staking fault changes phase 2 3 -π Diffraction Contrast Image Diffraction contrast images of typical defects Sample g Dislocations Dislocation loop Stacking faults Diffraction Contrast Image Weak-beam Dark-field imaging High-resolution dark-field imaging Near Bragg Condition Exact Bragg condition g Weak-beam means Large excitation error S g Planes do not satisfy Bragg diffraction Possible planes satisfy Bragg diffraction Away from Bragg Condition Taken by I. Petrov 1g 2g 3g Experimental weak-beam C.H. Lei Bright-field Weak-beam Dislocations can be imaged as 1.5 nm narrow lines

8 Lattice imaging Phase Contrast Image Two-beam condition Many-beam condition [001] M. Marshall C.H. Lei Lattice imaging Phase Contrast Image Delocalization effect from a field-emission gun (FEG) From a LaB 6 Gun Field-Emission Gun Lattice image of film on substrates

9 Phase Contrast Image High-resolution Electron Microscopy (HREM) Weak-phase-object approximation (WPOA) 1 Δf sch 2 Δf sch f(x,y) = exp(iσv t (x,y)) ~1 + i σ V t (x,y) V t (x,y): projected potential Indirect imaging Depends on defocus Scherzer defocus Δf sch = (C s λ) 2 1 Resolution limit 1 3 r sch = 0.66 C 4 s λ 4 1 Scherzer Defocus: Positive phase contrast black atoms 2 Scherzer Defocus: ("2nd Passband" defocus). Contrast Transfer Function is positive Negative phase contrast ("white atoms") Contrast transfer function J.G. Wen Simulation of images Software: Web-EMAPS (UIUC) MacTempas Selected-area electron diffraction (SAD) Diffraction Major Diffraction Techniques 1) Selected-area Diffraction 2) Nanobeam Diffraction 3) Convergent-beam electron diffraction Example of SAD and dark-field imaging SAD aperture High-contrast aperture Selected-area aperture Objective aperture A. Ehiasrian, J.G. Wen, I. Petrov

10 Electron Nanodiffraction Diffraction 5 μm condenser aperture 30 nm M. Gao, J.M. Zuo, R.D. Twesten, I. Petrov, L.A. Nagahara & R. Zhang, Appl. Phys. Lett. 82, 2703 (2003) J.M. Zuo, I. Vartanyants, M. Gao, R. Zhang and L.A. Nagahara, Science, 300, 1419 (2003) This technique was developed by CMM Diffraction Convergent-beam electron diffraction (CBED) Parallel beam Convergent-beam Sample Sample Back Focal Plane Large-angle bright-field CBED SAD CBED 1. Point and space group 2. Lattice parameter (3-D) strain field 3. Thickness Bright-disk Dark-disk Whole-pattern 4. Defects 5. Chemical bonding

11 Diffraction Convergent-beam electron diffraction Quantitative Analysis of Local Strain Relaxation a b c CoSi 2 d e f g h i C. W. Lim, C.-S. Shin, D. Gall, M. Sardela, R. D. Twesten, J. M. Zuo, I. Petrov and J. E. Greene Use High-order Laue zone (HOLZ) lines to measure strain field SEM vs STEM STEM Scanning electron microscopy (SEM) secondary electrons <50 ev 1 O primary e-beam kev backscattered electrons characteristic & Bremsstrahlung Auger x-rays electrons Scanning transmission electron microscopy (STEM) Probe size 0.18 nm Coherent Scattering (i.e. Interference) primary e-beam kev characteristic & Bremsstrahlung x-rays Thickness <100 nm Incoherent Scattering i.e. Rutherford Dark-field Detector 1 μm Bright-field

12 TEM vs STEM STEM Ge quantum dots on Si substrate Ir nanoparticles 1. STEM imaging gives better contrast 2. STEM images show Z- contrast TEM Z θ 10nm 5 nm ADF-STEM Annular dark-field (ADF) detector I Z 2 Z-contrast imaging Z-contrast image J.G. Wen 5 nm L. Long HRTEM vs STEM STEM 1. Contrast High-resolution TEM (HRTEM) image is a phase contrast image (indirect image). The contrast depends on defocus. STEM image is a direct atomic column image (average Z-contrast in the column). 2. Delocalization Effect High-resolution TEM image from FEG has delocalization effect. STEM image has no such an effect. BaTiO 3 /SrTiO 3 /CaTiO 3 superlattice J.G. Wen From Pennycook s group

13 X-ray Energy-Dispersive Spectroscopy (EDS) Spectroscopy 1) TEM mode spot, area 2) STEM mode spot, line-scan and 2-D mapping 2-D mapping Spatial resolution ~1 nm HAADF voids Area Mapping Au Line scan Ti Mo A B B Si Al A A. Ehiasrian, I. Petrov Ti 0.85 Nb 0.15 metal ion etch Creates a mixed amorphised surface layer ~ 6 nm Ga Liang Wang Au Ti Mo Electron Energy-loss Spectroscopy (EELS) Spectroscopy ZLP Low-loss Post-column In-column ZLP EELS spectrum: 1. Zero-loss Peak (ZLP) 2. Low-loss spectrum (<50eV) Interacted with weakly bound outer-shell electrons Plasmon peaks Inter- & Intra-Band transition Application: Thickness measurement Elemental mapping I 0 I l Low-loss I t = λ ln( l ) I 0 λ : Mean free path

14 ZLP Low-loss Edge Peaks in EELS Ti O x100 Mn La 3. High-loss spectrum Interacted with tightly bound inn-shell electrons Edge peaks Application: Elements identification Chemistry Edge peak shape Spectroscopy Edge peak position Amorphous carbon Diamond Nanoparticle π bonding π bonding J.G. Wen TEM mode Energy-filtered TEM 1. ZLP imaging 2. Plasmon imaging 3. Edge imaging STEM mode 1. Plasmon imaging 2. Edge imaging x Image at ΔE1 Image at ΔE2 Image at ΔE3 y Spectrum imaging ZLP Low-loss Ti O Edges Mn Spectrum imaging Energy-filtered TEM Fill in data cube by taking one image at each energy STEM mode Fill in data cube by taking one spectrum at each location La Image at ΔEn ΔE

15 Energy-Filtered TEM (EFTEM) EFTEM - Zero-Loss Peak imaging Only elastic electrons contribute to image remove the inelastic fog 1. Improve contrast (especially good for medium thick samples) 2. Z<12, the inelastic cross-section is larger than elastic cross-section Spectrum imaging ZLP Low-loss EFTEM Plasmon Peak imaging Spectrum imaging Spectrum image (20 images) Al mapping image W mapping image A B Al W 30 nm A B J.G. Wen

16 EFTEM Edge Peak imaging Spectrum imaging Image Ti Three-window method Ti EELS spectrum Si Jump ratio J.G. Wen STEM + EELS Spectroscopy convergence angle ~ 10 mrad Spectrum imaging LaMnO 3 incident probe probe size φ ~ 0.2 nm scan coils SrTiO 3 LaMnO 3 SrTiO 3 specimen HAADF detector Z-contrast image Z-contrast image Ti O Mn La magnetic prism EELS spectrum

17 STEM + EELS Spectroscopy Spectrum imaging 2nm STO SMO STO 3LMO STO 2LMO STO 2LMO STO LMO STO STMO STO STMO Z-contrast Image ΔE Electron Energy-Loss Spectrum Z-contrast image shows where columns of atoms are and EELS spectrum identify chemical components Ti L 2,3 Ti Mn L 2,3 O La M 4,5 Mn O K La O K edge M 4,5 Scan direction La Electronic structure changes are observed in the fine structure of O K-edge J.G. Wen, Amish, J.M. Zuo New TEM: Cs-corrected Analytical STEM/TEM Sound Isolation Low Airflow JEOL 2010F, Cs = 1.0 mm JEOL 2200FS, Cs < 5 μm CEOS Corrector Ω-Filter Remote operation Vibration decoupling With this setup we can achieve a probe-size of <0.1nm Cs-corrected Ronchigram

18 Small probe size for high-resolution scanning transmission electron microscopic images 1.36Å Si [110] Zone Axis 2 x 2 LaMnO 3 -SrTiO 3 superlattice Dec June 2007 Dec Thick specimen Same specimen Thin Specimen Sr atom Ti atom Sr atom La atom Mn atom La atom JEOL 2010F, C s = 1 mm (2 nd smallest Probe) JEOL 2200FS with probe forming Cs Corrector

19 Epitaxial Oxide Films Grown on SrTiO 3 STEM Image of Superlattice LaMnO 3 SrMnO 3 LaMnO 3 SrMnO 3 Polarized neutron scattering shows interfacial ferromagnetic moment measured at 10 Kelvin is enhanced in LaMnO 3 at the sharp LaMnO 3 -SrMnO 3 interface and reduced at the rough SrMnO 3 -LaMnO 3 interface. Sharp Interface Rough Interface Sharp Interface Rough Interface High Mag. Image R Å SrTiO 3 Substrate S CdSe nanoparticles View along [110] zone axis Polarity of CdSe 100 Cd Se Se Cd 100

20 Hetero-structure nanoparticle ZnTe CdSe Zn Te Te Zn Cd Se Se Cd Quantitative STEM Imaging 1 nm Stacking fault Grain boundary Se Cd 1.5 Å

21 1 nm Quantitative STEM Imaging Projected potential Monometallic Pt 300 (111) (111) (110) x 10^ (110) (111) (111) Monometallic Pd The intensity at each atomic column is proportional to numbers of atoms No defects in Pt nanoparticles Pd nanoparticles contain many defects such as twin boundaries

22 Bimetallic Pd(core)-Pt(shell Pt(shell) x 10^ Pd (core) Pt (shell) structure Core-shell structure of FePd nanoparticles Twin in the nanoparticle 1 nm Core: Ordered Fe/Pd structure Shell: non-ordered structure Pd columns are shown as brighter spots in the core Amorphous nanoparticle

23 Study Nanoparticles by TEM Size distribution: STEM will give better contrast Bi-nanoparticles Au-nanoparticles > 5nm Both TEM & STEM STEM better contrast 2 nm < Size < 5nm < 2 nm Ultra thin carbon grid STEM better contrast Ultra thin carbon grid Only STEM Composition study: EDS counts are low 2200FS EDS system detector area 2 times bigger beam 4 times brighter Minimum-Dose for beam sensitive samples Minimum-dose in TEM mode Search in low magnification Focus at another area Photo with minimum dose Minimum-dose in STEM mode Z-contrast tilt-series Special TEM technique HAADF-STEM image Long exposure time 200 nm L. Menard, J.G. Wen 200 nm BF-STEM image Short exposure time MDS + tomography will be available on 2100 Cryo-TEM soon +/- 80 degree tilt J.G. Wen

24 1. Heating (hot stage 1000 C) 2. Cooling (liquid N 2 ) 3. Tensile-stage 4. MEMS tensile stage 5. Universal MEMS holder 6. Wet-cell 7. Nanomanipulator 8. Environmental holder 9. Applied voltage to sample 10. Cryo transfer holder In-situ capabilities In-situ holders universal MEMS holder MEMS straining stage nanomanipulation CNT in water Water front In-situ 30 nm N. Schmit liquid cell All developed at CMM J.G. Wen List of TEMs and functions 1. CM12 (120 KeV) (S)TEM TEM, BF, DF, CBED (good), EDS, large tilt angle, etc LaB6 TEM TEM, low dose, NBD, good for HREM, video function LaB6 (Cryo-TEM) TEM, Low dose, special cryoshielding; high-tilt angle (+/-80) (using special retainer) F (S)TEM TEM, BF, DF, NBD, CBED, EDS, STEM, EELS, EFTEM, Spectrum imaging, etc. 5. HB501 STEM STEM, BF, DF, EDS, EELS (cold FEG), ultra-high vacuum 6. JEOL 2200FS (S)TEM Cs-corrected probe, TEM, BF, DF, NBD, CBED, EDS, STEM, EELS, EFTEM, Spectrum imaging, etc. CM LaB Cryo 2010F 2200FS HB501

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