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1. In Situ Characterization of Phase-Change Materials

   Tripathi, s. ; Janish, M. ; Noor, N. ; Jungjohann, K. ; Pete, D. ; Kotula, P. ; Silva, H. ; Carter, C. ( November 2018 , Materials Research Society symposia proceedings)

   To understand the mechanism underlying the fast, reversible, phase transformation, information about the atomic structure and defects structures in phase change materials class is key. PCMs are investigated for many applications. These devices are chalcogenide based and use self heating to quickly switch between amorphous and crystalline phases, generating orders of magnitude differences in the electrical resistivity. The main challenges with PCMs have been the large power required to heat above crystallization or melting (for melt-quench amorphization) temperatures and limited reliability due to factors such as resistance drifts of the metastable phases, void formation and elemental segregation upon cycling. Characterization of devices and their unique switching behavior result in distinct material properties affected by the atomic arrangement in the respective phase. TEM is used to study the atomic structure of the metastable crystalline phase. The aim is to correlate the microstructure with results from electrical characterization, building on R vs T measurements on various thicknesses GST thin films. To monitor phase changes in real-time as a function of temperature, thin films are deposited directly onto Protochips carriers. The Protochips heating holders provides controlled temperature changes while imaging in the TEM. These studies can provide insights into how changes occur inmore »the various phase transformations even though the rate of temperature change is much slower than the PCM device operation. Other critical processes such as void formation, grain evolution and the cause of resistance drift can thereby be related to changes in structure and chemistry. Materials characterization is performed using Tecnai F30 and Titan ETEM microscopes, operating at 300kV. Both the microscopes can accept the same Protochips heating holders. The K2 direct electron detector camera equipped with the ETEM allows high-speed video recording (1600 f/s) of structural changes occurring in these materials upon heating and cooling. In this presentation, we will describe the effect of heating thin films of different thickness and composition, the changes in crystallinity and grain size, and how these changes correlate with changes in the electrical properties of the films. We will emphasize that it is always important to use low-dose and/or beam blanking techniques to distinguish changes induced by the beam from those due to the heating or introduction of an electric current.« less
2. Towards Horizontal Heterojunctions for Tunnel Field Effect Transistors with Template Assisted Selective Epitaxy via MOCVD

   Brunelli, Simone ; Markman, B ; Wu, J ; Tseng, HY ; Goswami, A ; Rodwell, M ; Palmstrøm, P ; Klamkin, K ( June 2018 , International conference on MOVPE)

   Tunneling field effect transistors (TFETs) have gained much interest in the previous decade for use in low power CMOS electronics due to their sub-thermal switching [1]. To date, all TFETs are fabricated as vertical nanowires or fins with long, difficult processes resulting in long learning cycle and incompatibility with modern CMOS processing. Because most TFETs are heterojunction TFETs (HJ-TFETs), the geometry of the device is inherently vertically because dictated by the orientation of the tunneling HJ, achieved by typical epitaxy. Template assisted selective epitaxy was demonstrated for vertical nanowires [2] and horizontally arranged nanorods [3] for III-V on Si integration. In this work, we report results on the area selective and template assisted epitaxial growth of InP, utilizing SiO2 based confined structures on InP substrates, which enables horizontal HJs, that can find application in the next generation of TFET devices. The geometries of the confined structures used are so that only a small area of the InP substrate, dubbed seed, is visible to the growth atmosphere. Growth is initiated selectively only at the seed and then proceeds in the hollow channel towards the source hole. As a result, growth resembles epitaxial lateral overgrowth from a single nucleation point [4], reapingmore »the benefits of defect confinement and, contrary to spontaneous nanowire growth, allows orientation in an arbitrary, template defined direction. Indium phosphide 2-inch (110) wafers are used as the starting substrate. The process flow (Fig.1) consists of two plasma enhanced chemical vapor deposition (PECVD) steps of SiO2, appropriately patterned with electron beam lithography (EBL), around a PECVD amorphous silicon sacrificial layer. The sacrificial layer is ultimately wet etched with XeF2 to form the final, channel like template. Not shown in the schematic in Fig.1 is an additional, ALD deposited, 3 nm thick, alumina layer which prevents plasma damage to the starting substrate and is removed via a final tetramethylammonium hydroxide (TMAH) based wet etch. As-processed wafers were then diced and loaded in a Thomas Swan Horizontal reactor. Successful growth conditions found were 600°C with 4E6 mol/min of group III precursor, a V/III ratio of 400 and 8 lpm of hydrogen as carrier gas. Trimethylindium (TMIn) and tertiarybutylphosphine (TBP) were used as In and P precursors respectively. Top view SEM (Fig.2) confirms growth in the template thanks to sufficient Z-contrast despite the top oxide layer, not removed before imaging. TEM imaging shows a cross section of the confined structure taken at the seed hole (Fig.3). The initial growth interface suggests growth was initiated at the seed hole and atomic order of the InP conforms to the SiO2 template both at the seed and at the growth front. A sharp vertical facet is an encouraging result for the future development of vertical HJ based III-V semiconductor devices.« less
3. Pushing the limits of high-resolution polymer microscopy using antioxidants

   https://doi.org/10.1038/s41467-020-20363-1  

   Kuei, Brooke ; Gomez, Enrique D. ( January 2021 , Nature Communications)

   High-resolution transmission electron microscopy (HRTEM) has been transformative to the field of polymer science, enabling the direct imaging of molecular structures. Although some materials have remarkable stability under electron beams, most HRTEM studies are limited by the electron dose the sample can handle. Beam damage of conjugated polymers is not yet fully understood, but it has been suggested that the diffusion of secondary reacting species may play a role. As such, we examine the effect of the addition of antioxidants to a series of solution-processable conjugated polymers as an approach to mitigating beam damage. Characterizing the effects of beam damage by calculating critical doseD_Cvalues from the decay of electron diffraction peaks shows that beam damage of conjugated polymers in the TEM can be minimized by using antioxidants at room temperature, even if the antioxidant does not alter or incorporate into polymer crystals. As a consequence, the addition of antioxidants pushes the resolution limit of polymer microscopy, enabling imaging of a 3.6 Å lattice spacing in poly[(5,6-difluoro-2,1,3-benzothiadiazol-4,7-diyl)-alt-(3,3″′-di(2-octyldodecyl)-2,2′;5′,2″;5″,2″′-quaterthiophene-5,5″′-diyl)] (PffBT4T-2OD).
4. PCM Materials and Devices: High Speed and Low-dose TEM Imaging

   Tripathi, S. ; Janish, M. ; Dirisaglik, F. ; Cywar, A. ; Zhu, Y. ; Jungjohann, K. ; Silva, H. ; Carter, C.B. ( September 2018 , International Microscopy Congress)

   Phase-change memory (PCM) materials are being developed for faster, non-volatile & high-density memory that can facilitate more efficient computation as well as data storage. The materials used for these PCM devices are usually chalcogenides that can be switched between their amorphous and crystalline phases thus producing orders of magnitude difference in the electrical resistivity [1, 2]. The operation of such devices is limited by elemental segregation and void formation, which occurs as a result of the extensive cycling. After crystallization, the structure gradually transforms from fcc to hexagonal. In the present work, we are studying these different phase changes in-situ as they occur in PCM materials basically using TEM imaging. The aim is to correlate device modeling and electrical characterization in order to improve the models and enable accurate, predictive simulations. The thin film materials and devices can be directly deposited onto Protochips devices, allowing controlled temperature changes while imaging in the TEM. Although the temperature change rate achievable is too slow as compared to the fastest PCM-device operation, these rates can provides valuable insights into the various property changes in the material and phase transformations as well. Both a Cs-image corrected Titan ETEM and a Tecnai F30 have beenmore »used for this study. The ETEM is equipped with a K2 direct electron detector camera allowing high-speed video recording of these PCM materials.« less
5. Gas-Phase Formation of Highly Luminescent 2D GaSe Nanoparticle Ensembles in a Nonequilibrium Laser Ablation Process

   https://doi.org/10.3390/nano10050908  

   Elafandi, Salah ; Ahmadi, Zabihollah ; Azam, Nurul ; Mahjouri-Samani, Masoud ( May 2020 , Nanomaterials)

   Interest in layered two-dimensional (2D) materials has been escalating rapidly over the past few decades due to their promising optoelectronic and photonic properties emerging from their atomically thin 2D structural confinements. When these 2D materials are further confined in lateral dimensions toward zero-dimensional (0D) structures, 2D nanoparticles and quantum dots with new properties can be formed. Here, we report a nonequilibrium gas-phase synthesis method for the stoichiometric formation of gallium selenide (GaSe) nanoparticles ensembles that can potentially serve as quantum dots. We show that the laser ablation of a target in an argon background gas condenses the laser-generated plume, resulting in the formation of metastable nanoparticles in the gas phase. The deposition of these nanoparticles onto the substrate results in the formation of nanoparticle ensembles, which are then post-processed to crystallize or sinter the nanoparticles. The effects of background gas pressures, in addition to crystallization/sintering temperatures, are systematically studied. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), photoluminescence (PL) spectroscopy, and time-correlated single-photon counting (TCSPC) measurements are used to study the correlations between growth parameters, morphology, and optical properties of the fabricated 2D nanoparticle ensembles.