Mobile setup for synchrotron based <i>in situ</i> characterization during thermal and plasma-enhanced atomic layer deposition

Dendooven, Jolien; Solano, Eduardo; Minjauw, Matthias; Kerckhove, Kevin Van de; Coati, Alessandro; Fonda, Emiliano; Portale, Giuseppe; Garreau, Y.; Detavernier, Christophe

doi:10.1063/1.4967711

Cited by 24 publications

(26 citation statements)

References 39 publications

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“…The Pt nanoparticle growth is studied on planar Si substrates covered with native SiO 2 . The Pt depositions are performed in an experimental ALD setup equipped with Be windows and positioned in the path of a 12.75 keV X-ray beam at the SixS beamline of the SOLEIL synchrotron radiation facility (Saint-Aubin, France) 48 . Prior to ALD growth, the Si/SiO 2 support is heated to 300 °C and exposed to oxygen plasma to clean the sample surface and improve the reproducibility between different experiments.…”

Section: Resultsmentioning

confidence: 99%

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Independent tuning of size and coverage of supported Pt nanoparticles using atomic layer deposition

et al. 2017

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Synthetic methods that allow for the controlled design of well-defined Pt nanoparticles are highly desirable for fundamental catalysis research. In this work, we propose a strategy that allows precise and independent control of the Pt particle size and coverage. Our approach exploits the versatility of the atomic layer deposition (ALD) technique by combining two ALD processes for Pt using different reactants. The particle areal density is controlled by tailoring the number of ALD cycles using trimethyl(methylcyclopentadienyl)platinum and oxygen, while subsequent growth using the same Pt precursor in combination with nitrogen plasma allows for tuning of the particle size at the atomic level. The excellent control over the particle morphology is clearly demonstrated by means of in situ and ex situ X-ray fluorescence and grazing incidence small angle X-ray scattering experiments, providing information about the Pt loading, average particle dimensions, and mean center-to-center particle distance.

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Section: Resultsmentioning

confidence: 99%

“…The technique has, for example, been used for real-time monitoring of noble metal growth by evaporation 43 and sputtering 44 – 47 . We recently designed a mobile setup for synchrotron-based in situ characterization during both thermal and plasma-enhanced ALD 48 .…”

Section: Introductionmentioning

confidence: 99%

Independent tuning of size and coverage of supported Pt nanoparticles using atomic layer deposition

et al. 2017

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“…Two different samples containing the same amount of Pt, but distinct as-deposited particle size and coverage were fabricated profiting the distinct nucleation regime of the O 2 and N 2 plasma (N 2 *) Pt ALD processes 30 . In brief, Pt nanoparticles were deposited on a -OH terminated Si (100) wafer heated to 300 o C in a pump-type ALD reac-tor 33 . The chamber base pressure was 1•10 −6 mbar.…”

Section: Fabrication Of Supported Pt Nanoparticlesmentioning

confidence: 99%

In situ study of the thermal stability of supported Pt nanoparticles and their stabilization via atomic layer deposition overcoating

et al. 2020

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“…X-ray fluorescence (XRF), X-ray diffraction (XRD), specular reflectivity (XRR), X-ray absorption fine structure spectroscopy (XAFS), and grazing incidence small angle X-ray scattering (GISAXS) are among the popular techniques used for in situ growth studies at various synchrotron centers. 17,[21][22][23] Here, we employ in situ synchrotron techniques to study the initial growth behavior of ZnO ALD on In x Ga 1−x As, as well as to characterize the resulting film morphology and crystallinity. We exploit a custombuilt thermal ALD reactor 24,25 equipped with a dedicated port for measuring X-ray fluorescence and a rotating flange for performing surface diffraction.…”

Section: Introductionmentioning

confidence: 99%

In situ x-ray studies of the incipient ZnO atomic layer deposition on In0.53Ga0.47As

Skopin

Rapenne

Deschanvres

et al. 2020

Phys. Rev. Materials

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We describe in detail how ZnO films grow on In0.53Ga0.47As substrates by Atomic Layer Deposition (ALD), employing a suite of in situ synchrotron X-ray techniques. Combining results from different measurements allows the distinguishment of three different growth behaviors: an initial, slow linear growth, often referred to as a growth delay (regime I), followed by a nonlinear growth (regime II), and finally, a steady, linear growth (regime III), the last of which is the self-limited growth behavior characteristic of ALD. By the end of the regime I, the In0.53Ga0.47As surface is covered with an ultra-thin, poorly-ordered Zn oxide layer. The transition from regime I to II is clearly evidenced by the appearance on the X-ray absorption spectra of characteristic features of the wurtzite structure, as well as the nucleation and growth of ZnO grains (3D) on top of the poorlyordered Zn oxide layer. Regime II ends when the growth per cycle reaches a constant level. We show that the water pressure during growth has an impact on the duration of the growth delay (regime I), unlike the substrate temperature. In the regime of steady growth, we observe that the rate of deposition obtained for all temperatures inside the ALD window is 0.17 nm.cy −1. The deposition temperature has clear effects on the film texture and initial crystallization behavior, as well as the final crystallinity and thicknesses of the layers adjacent to the In0.53Ga0.47As substrate. Based on the experimental results and earlier ab initio calculations and Monte Carlo simulations of ZnO ALD on ZnO, we suggest reaction mechanisms consistent with our findings and present a model of growth starting from the very earliest stages of deposition to the steady growth regime.

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Mobile setup for synchrotron based in situ characterization during thermal and plasma-enhanced atomic layer deposition

Cited by 24 publications

References 39 publications

Independent tuning of size and coverage of supported Pt nanoparticles using atomic layer deposition

Independent tuning of size and coverage of supported Pt nanoparticles using atomic layer deposition

In situ study of the thermal stability of supported Pt nanoparticles and their stabilization via atomic layer deposition overcoating

In situ x-ray studies of the incipient ZnO atomic layer deposition on In0.53Ga0.47As

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