Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for <i>In Situ</i> Atomic Resolution Scanning Transmission Electron Microscopic Observation

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

doi:10.1017/s1431927616000593

Cited by 12 publications

(6 citation statements)

References 25 publications

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“…An important feature of this protocol is that the whole preparation procedure can be completed within the chamber without breaking vacuum. This is in contrast to the modified H-bar approach described by Straubinger et al (2016) for producing specimens for gas environmental cell holder experiments.…”

Section: Specimen Preparation Proceduresmentioning

confidence: 93%

Focused Ion Beam Preparation of Specimens for Micro-Electro-Mechanical System-based Transmission Electron Microscopy Heating Experiments

et al. 2017

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Micro-electro-mechanical systems (MEMS)-based heating holders offer exceptional control of temperature and heating/cooling rates for transmission electron microscopy experiments. The use of such devices is relatively straightforward for nano-particulate samples, but the preparation of specimens from bulk samples by focused ion beam (FIB) milling presents significant challenges. These include: poor mechanical integrity and site selectivity of the specimen, ion beam damage to the specimen and/or MEMS device during thinning, and difficulties in transferring the specimen onto the MEMS device. Here, we describe a novel FIB protocol for the preparation and transfer of specimens from bulk samples, which involves a specimen geometry that provides mechanical support to the electron-transparent region, while maximizing the area of that region and the contact area with the heater plate on the MEMS chip. The method utilizes an inclined stage block that minimizes exposure of the chip to the ion beam during milling. This block also allows for accurate and gentle placement of the FIB-cut specimen onto the chip by using simultaneous electron and ion beam imaging during transfer. Preliminary data from Si and Ag on Si samples are presented to demonstrate the quality of the specimens that can be obtained and their stability during in situ heating experiments.

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Section: Specimen Preparation Proceduresmentioning

confidence: 93%

Focused Ion Beam Preparation of Specimens for Micro-Electro-Mechanical System-based Transmission Electron Microscopy Heating Experiments

et al. 2017

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“…The detailed preparation process of the lamella and the loading procedure of the finished specimen into the in situ cell will not be repeated here, but a detailed description can be found in Straubinger et al . 24 . In summary, an electron transparent lamella was prepared out of a wafer piece as described in Schaffer et al .…”

Section: Experimental Methodsmentioning

confidence: 99%

Thermally Introduced Bismuth Clustering in Ga(P,Bi) Layers under Group V Stabilised Conditions Investigated by Atomic Resolution In Situ (S)TEM

Straubinger

Widemann

Belz

et al. 2018

Sci Rep

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We report the formation of Bi clusters in Ga(P1-x,Bix) layers during an in situ (scanning) transmission electron microscopy ((S)TEM) annealing investigation. The non-destructive temperature regime in dependence on the tertiarybutylphosphine (TBP) pressure in the in situ cell was investigated to ensure that the results are not distorted by any destructive behaviour of the crystal during the thermal treatment. The following annealing series of the Ga(P92.6Bi7.4) and Ga(P96.4Bi3.6) layers reveals that the threshold temperature at which the Bi clustering takes place is 600 °C in the Ga(P92.6Bi7.4) layer. Further thermal treatments up to 750 °C show a relationship between the Bi fraction in the Ga(P1-x,Bix) layer and the initial temperature at which the Bi clustering takes place. Finally, we investigate one Bi cluster at atomic resolution conditions. In these conditions, we found that the Bi cluster crystallized in a rhombohedral phase, aligning with its {101} planes parallel to the Ga(P,Bi) {202} planes.

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“…The samples were prepared for the in situ annealing STEM investigation using a focused ion beam (FIB; JIB 4601 F; JEOL, Freising, Germany) system. A detailed description of the preparation and loading process of the specimens is given in Straubinger et al (2016). In summary, an electron transparent lamella was prepared out of a wafer piece as described in Schaffer et al (2012).…”

Section: Experimental Methodsmentioning

confidence: 99%

In Situ Thermal Annealing Transmission Electron Microscopy (TEM) Investigation of III/V Semiconductor Heterostructures Using a Setup for Safe Usage of Toxic and Pyrophoric Gases

et al. 2017

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In this study we compare two thermal annealing series of III/V semiconductor heterostructures on Si, where during the first series nitrogen is present in the in situ holder. The second, comparative, measurement is done in a tertiarybutylphosphine (TBP) environment. The sample annealed in a TBP environment shows favorable thermal stability up to 500°C compared to the unstabilized sample, which begins to degrade at less than 300°C. Evaporation of P from the material is tracked qualitatively by measuring the thickness of the sample during thermal annealing with and without stabilization. Finally, we investigate the in situ thermal annealing processes at atomic resolution. Here it is possible to study phase separation as well as the diffusion of As from a Ga(NAsP) quantum well in the surrounding GaP material during thermal annealing. To make these investigations possible we developed an extension for our in situ transmission electron microscopy setup for the safe usage of toxic and pyrophoric III/V semiconductor precursors. A commercially available gas cell and gas supply system were expanded with a gas mixing system, an appropriate toxic gas monitoring system and a gas scrubbing system. These components allow in situ studies of semiconductor growth and annealing under the purity conditions required for these materials.

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Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation

Cited by 12 publications

References 25 publications

Focused Ion Beam Preparation of Specimens for Micro-Electro-Mechanical System-based Transmission Electron Microscopy Heating Experiments

Focused Ion Beam Preparation of Specimens for Micro-Electro-Mechanical System-based Transmission Electron Microscopy Heating Experiments

Thermally Introduced Bismuth Clustering in Ga(P,Bi) Layers under Group V Stabilised Conditions Investigated by Atomic Resolution In Situ (S)TEM

In Situ Thermal Annealing Transmission Electron Microscopy (TEM) Investigation of III/V Semiconductor Heterostructures Using a Setup for Safe Usage of Toxic and Pyrophoric Gases

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