NanoDefine OutreachSeptember 20th 2017

BrusselsToni Uusimäki

Eawag

AutoEM-toolbox

AutoEM-toolbox

- An automatization program written in Digital Micrograph environment- Acquires images with the transmission electron microscope (TEM) in a

serial fashion- Connected to NanoDefine ParticleSizer (D5.1) for live data analysis- Works in TEM Bright Field mode and STEM Dark Field mode- Elemental analysis and thickness mapping (plateles) possible- Automatic exposure and focusing incorporated- Tested with 4 FEI Tecnai and 2 JEOL microscopes

ParticleSizer AutoEMAcquired Images

Segmented ImagesAnalysis Results

AutoEM-toolbox TEM mode

UI

Live PSDLive view

ParticleSizer results

3D Segmenation3D recordedimages

AutoEM-toolbox TEM mode

Main Tab Calibrations

User Interface

Camera parameters

AutoEM-toolbox TEM mode

TEM bright field imageof Au/SiO2 NPs

Pixel size: 2.95 nmFOV: 3 µm

AutoEM-toolbox TEM mode

A mosaic collection of TEM images (35x10, 1.4 gb) with FOV 0.11 mm x 0.3 mm

AutoEM-toolbox STEM mode

STEM HAADF imageof SiO2 NPs (ERM-FD304)

Pixel size: 1.17 nmFOV: 1.2 µm

AutoEM-toolbox STEM mode

A mosaic collection of STEM images (10x5, 0.2 gb) with FOV 12 µm x 6 µm

AutoEM-toolbox STEM EDS mode

AutoEM-toolbox STEM EDS mode

- User chooses the elements and defines Cutoff values for the peaks

- The EDS spectra integrated from theSI image is smoothed and an optimized Gaussian curve is fitted to the peak

- If the peak is above the cutoff value, theferet min value will be added to the PSD

AutoEM-toolbox STEM EDS mode

A video of AutoEM EDX in action

AutoEM-toolbox STEM EDS mode

Au/Si NPs (5x4) FOV 5 µm x 4 µm

PSD of Au NPs

PSD of Si NPs

AutoEM-toolbox STEM EELS mode

- EELS SI also possible- Core loss, ELNES…- Analysis not

supported- Custom analysis

scripts possible after every pixel/particle

AutoEM-toolbox TEM Core Loss Imaging

Si @99 eV Au @2206 eV Combined RGB

Core Loss Imaging provided for elemental analysis

AutoEM-toolbox TEM EFTEM modeThickness Map

ZLP image Unfiltered image Thickness Map t/λ

𝑡𝑡λ = ln

𝐼𝐼𝐼𝐼0

, λ =106𝐹𝐹 �𝐸𝐸0

𝐸𝐸𝑀𝑀

𝑙𝑙𝑙𝑙 �2𝐸𝐸0𝛽𝛽𝐸𝐸𝑀𝑀

=155.5 nm,

Ref: Egerton & Chang, Ultramicroscopy 21 (1987) 231-244

𝐹𝐹 = 1+ �𝐸𝐸01022

1+ �𝐸𝐸0511

2, 𝐸𝐸𝑀𝑀 = 7.6𝑍𝑍𝑒𝑒𝑒𝑒𝑒𝑒0.36

λ = 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑓𝑓𝑓𝑓𝑚𝑚𝑚𝑚 𝑝𝑝𝑚𝑚𝑡𝑡𝑝, 𝑡𝑡 = 𝑡𝑡𝑝𝑡𝑡𝑡𝑡𝑡𝑡𝑚𝑚𝑚𝑚𝑡𝑡𝑡𝑡, 𝐼𝐼 = 𝑢𝑢𝑚𝑚𝑓𝑓𝑡𝑡𝑢𝑢𝑡𝑡𝑚𝑚𝑓𝑓𝑚𝑚𝑢𝑢 𝑡𝑡𝑚𝑚𝑚𝑚𝑖𝑖𝑚𝑚, 𝐼𝐼0= 𝑍𝑍𝑍𝑍𝑍𝑍 𝑡𝑡𝑚𝑚𝑚𝑚𝑖𝑖𝑚𝑚𝐸𝐸0 = 𝑡𝑡𝑚𝑚𝑡𝑡𝑡𝑡𝑢𝑢𝑚𝑚𝑚𝑚𝑡𝑡 𝑚𝑚𝑚𝑚𝑚𝑚𝑓𝑓𝑖𝑖𝑒𝑒 𝑜𝑜𝑓𝑓 𝑚𝑚𝑢𝑢𝑚𝑚𝑡𝑡𝑡𝑡𝑓𝑓𝑜𝑜𝑚𝑚𝑡𝑡

AutoEM-toolbox TEM EFTEM mode

Thickness Map x Segmented image x λ = Masked Thickness Map

AutoEM-toolbox TEM EFTEM mode

Illite NPs (10x12, 2 gb) FOV 47 µm x 57 µm

PSD XY analysis

PSD 3D analysis

AutoEM-toolbox TEM EFTEM mode

Illite NPs video extracted from the Thickness Map

AutoEM-toolbox TEM EFTEM modeNanosteel NPs (35x6, 3 gb) FOV 0.17 mm x 0.03 mm

PSD in XY plane

AutoEM-toolbox

STEM TEM

EELS

EDS Core LossImaging

Thickness Map

ParticleSizer

CustomTasks

e.g. CBED e.g. EDS/EELS analysis

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This project has received funding from the European Union’s Seventh Programme for research, technological development and demonstration under grant agreement No 604347