In situ X-ray measurements over large Q-space to study the evolution of oxide thin films prepared by RF sputter deposition

Walter, Peter; Wernecke, Jan; Scholz, Markus; Reuther, D.; Rothkirch, André; Haas, Diana; Blume, Janet A.; Resta, Andrea; Vlad, Alina; Faley, O.; Schipmann, Susanne; Nent, Alexander; Seeck, O. H.; Dippel, Ann‐Christin; Klemradt, Uwe

doi:10.1007/s10853-020-05337-4

Cited by 3 publications

(5 citation statements)

References 31 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…After the crystallization of the whole thin film the arriving amorphous particle coming from the sputtering target will quickly crystallize. The high surface roughness stays until the end of the deposition which is also confirmed by the missing interference pattern in the q z -cuts at the q = 0 position shown in Figure 3c, which is in strong agreement with the literature [10]. A schematic of the thin film evolution during the deposition is shown in Figure 8.…”

Section: Resultssupporting

confidence: 90%

“…This means the surface is covered and the newly arriving particles contribute only in the vertical growth. This describes the early formation (nucleation, diffusion, adsorption and grain growth) for thin films as known from literature [5,6,10]. The relation D ≈ 2π/q enables us to track the mean cluster distance during the growth as a quantitative parameter.…”

Section: Resultsmentioning

confidence: 99%

“…The films were deposited on pre-cleaned SiO 2 wafers with a size of 10 × 10 mm 2 . A more detailed description of the measurement can be found here [8,10]. SiO 2 wafers are not the industrial standard for BaTiO 3 thin film deposition, but we have chosen it to avoid surface related influence on the crystallization process.…”

Section: Methodsmentioning

confidence: 99%

“…To follow the preparation of oxide thin films, we were using the characteristic features of the modern synchrotron radiation source PETRA III [7], a compact and low-weight sputtering unit [8], and the investigation techniques in situ grazing incidence small angle X-ray scattering (GISAXS) and in situ grazing incidence X-ray powder diffraction (GIXRPD) simultaneously, as well as in situ X-ray reflectivity (XRR) measurements [9,10].…”

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

In Situ X-ray Measurements to Follow the Crystallization of BaTiO3 Thin Films during RF-Magnetron Sputter Deposition

et al. 2021

Self Cite

View full text Add to dashboard Cite

Here, we report on adding an important dimension to the fundamental understanding of the evolution of the thin film micro structure evolution. Thin films have gained broad attention in their applications for electro-optical devices, solar-cell technology, as well storage devices. Deep insights into fundamental functionalities can be realized via studying crystallization microstructure and formation processes of polycrystalline or epitaxial thin films. Besides the fundamental aspects, it is industrially important to minimize cost which intrinsically requires lower energy consumption at increasing performance which requires new approaches to thin film growth in general. Here, we present a state of the art sputtering technique that allows for time-resolved in situ studies of such thin film growth with a special focus on the crystallization via small angle scattering and X-ray diffraction. Focusing on the crystallization of the example material of BaTiO3, we demonstrate how a prototypical thin film forms and how detailed all phases of the structural evolution can be identified. The technique is shaped to enable a versatile approach for understanding and ultimately controlling a broad variety of growth processes, and more over it demonstrate how to in situ investigate the influence of single high temperature sputtering parameters on the film quality. It is shown that the whole evolution from nucleation, diffusion adsorption and grain growth to the crystallization can be observed during all stages of thin film growth as well as quantitatively as qualitatively. This can be used to optimize thin-film quality, efficiency and performance.

show abstract

Section: Resultssupporting

confidence: 90%

Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

In Situ X-ray Measurements to Follow the Crystallization of BaTiO3 Thin Films during RF-Magnetron Sputter Deposition

et al. 2021

Self Cite

View full text Add to dashboard Cite

show abstract

“…However, the method is only compatible with sputter deposition processes when using differential pumping, which affects the growth conditions significantly. X-ray methods do not suffer from this limitation, and are therefore well established for monitoring industrially relevant sputter deposition processes. − We have combined real-time synchrotron experiments during magnetron sputter deposition and annealing of Pd/amorphous germanium (a-Ge) bilayers. The real-time information during deposition of Pd/a-Ge was obtained using simultaneous X-ray methods and stress monitoring. , The structure formation during subsequent annealing was studied by real-time X-ray diffraction (XRD).…”

Section: Introductionmentioning

confidence: 99%

In Situ Study of the Interface-Mediated Solid-State Reactions during Growth and Postgrowth Annealing of Pd/a-Ge Bilayers

Krause

Abadias

Babonneau

et al. 2023

ACS Appl. Mater. Interfaces

View full text Add to dashboard Cite

Ohmic or Schottky contacts in micro- and nanoelectronic devices are formed by metal–semiconductor bilayer systems, based on elemental metals or thermally more stable metallic compounds (germanides, silicides). The control of their electronic properties remains challenging as their structure formation is not yet fully understood. We have studied the phase and microstructure evolution during sputter deposition and postgrowth annealing of Pd/a-Ge bilayer systems with different Pd/Ge ratios (Pd:Ge, 2Pd:Ge, and 4Pd:Ge). The room-temperature deposition of up to 30 nm Pd was monitored by simultaneous, in situ synchrotron X-ray diffraction, X-ray reflectivity, and optical stress measurements. With this portfolio of complementary real-time methods, we could identify the microstructural origins of the resistivity evolution during contact formation: Real-time X-ray diffraction measurements indicate a coherent, epitaxial growth of Pd(111) on the individual crystallites of the initially forming, polycrystalline Pd2Ge[111] layer. The crystallization of the Pd2Ge interfacial layer causes a characteristic change in the real-time wafer curvature (tensile peak), and a significant drop of the resistivity after 1.5 nm Pd deposition. In addition, we could confirm the isostructural interface formation of Pd/a-Ge and Pd/a-Si. Subtle differences between both interfaces originate from the lattice mismatch at the interface between compound and metal. The solid-state reaction during subsequent annealing was studied by real-time X-ray diffraction and complementary UHV surface analysis. We could establish the link between phase and microstructure formation during deposition and annealing-induced solid-state reaction: The thermally induced reaction between Pd and a-Ge proceeds via diffusion-controlled growth of the Pd2Ge seed crystallites. The second-phase (PdGe) formation is nucleation-controlled and takes place only when a sufficient Ge reservoir exists. The real-time access to structure and electronic properties on the nanoscale opens new paths for the knowledge-based formation of ultrathin metal/semiconductor contacts.

show abstract

A combination of ion beam sputtering and in situ x-ray diffraction as a method for depth-resolved phase analysis using nitrogen-implanted austenitic stainless steel as an example

Manova

Schlenz

Mändl

2022

Journal of Applied Physics

View full text Add to dashboard Cite

In situ x-ray diffraction (XRD) during ion implantation or thin film deposition is a powerful method to follow the time evolution of diffusion and phase transition processes in thin films, even as the depth resolution is still dominated by the information depth of the x rays. However, in the case of sputter etching with energetic ions at moderate temperatures, where no diffusion or phase transformation processes are active, this limitation is no longer of concern. Here, thin surface layers which are removed by sputtering can be identified with a depth resolution of 25 nm or better—while information from the substrate—despite overlayers of several micrometers—is accessible. However, considerable mathematical operations are necessary to convert the time series of diffractograms measured by XRD into a depth series. In this paper, a method is highlighted describing which depth-resolved properties of thin films can be accessed using such in situ measurements during ion beam sputtering in the model system austenitic stainless steel + nitrogen: (i) the influence of concentration gradients on the peak shape and peak width for conventional XRD scans in Bragg–Brentano geometry is determined; (ii) correlations between the local nitrogen concentration and the local lattice expansion can be established; and (iii) the evolution of the scattering intensity with depth becomes accessible, thus depth-resolved information on defect densities or grain size (normal to the surface) can be extracted without resorting to transmission or scanning electron microscopy.

show abstract

In situ X-ray measurements over large Q-space to study the evolution of oxide thin films prepared by RF sputter deposition

Cited by 3 publications

References 31 publications

In Situ X-ray Measurements to Follow the Crystallization of BaTiO3 Thin Films during RF-Magnetron Sputter Deposition

In Situ X-ray Measurements to Follow the Crystallization of BaTiO3 Thin Films during RF-Magnetron Sputter Deposition

In Situ Study of the Interface-Mediated Solid-State Reactions during Growth and Postgrowth Annealing of Pd/a-Ge Bilayers

A combination of ion beam sputtering and in situ x-ray diffraction as a method for depth-resolved phase analysis using nitrogen-implanted austenitic stainless steel as an example

Contact Info

Product

Resources

About