Towards In-Situ Electron Microscopy Studies of Flash Sintering

Schwarzbach, Danny; González‐Julián, Jesús; Guillon, Olivier; Roddatis, Vladimir; Volkert, Cynthia A.

doi:10.3390/ceramics2030036

Cited by 8 publications

(9 citation statements)

References 52 publications

(44 reference statements)

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“…In particular, in transmission electron microscopy (TEM), the introduction of Micro Electronic Mechanical System (MEMS) chip‐based holders has led to the rapid development of methodologies allowing to directly relate structure and composition with material functionality (Alam et al, 2020; Allard et al, 2009; Creemer et al, 2010; Gaulandris et al, 2020; Mele et al, 2016; Niekiel et al, 2017; Vijayan & Aindow, 2019; Yokosawa et al, 2012; Zheng et al, 2022; Zintler et al, 2017). MEMS chips are also employed in conjunction with scanning electron microscopy (SEM) for in‐situ and operando experiments (Mølhave et al, 2004; Schwarzbach et al, 2019).…”

Section: Introductionmentioning

confidence: 99%

“…Such experiments have given insight into, for example, solid state battery dynamics (Basak et al, 2022; Hammad Fawey et al, 2016; Wang et al, 2020; Yang et al, 2016; Zhang et al, 2022). With the use of combined heating‐biasing holders, such measurements can be performed as a function of temperature (Schwarzbach et al, 2019). In a recent study, we showed that by combining the heating‐biasing chips with an environmental TEM (ETEM) it is possible to perform reliable electrochemical impedance spectroscopy (EIS) measurements of solid oxide cell components in the TEM (Ma et al, 2023).…”

Section: Introductionmentioning

confidence: 99%

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Ion‐beam deposited platinum as electrical contacting material in operando electron microscopy experiments at elevated temperatures

Simonsen¹,

Ma²,

Mariegaard³

et al. 2023

Microscopy Res & Technique

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Establishing a stable and well conducting contacting material is critical for operando electron microscopy experiments of electrical and electrochemical devices at elevated temperatures. In this contribution, the nanostructure and electrical conductivity of ion beam deposited Pt are investigated both in vacuum and in oxygen as a function of temperature. Its microstructure is relatively stable up to a temperature of approx. 800°C and up to an applied current density of approx. 100 kA/cm2. Its conductivity increases with temperature, attributed to densification, with changes in the hydrocarbon matrix being less important. Recommendations are provided with respect to the Pt deposition parameters in terms of maximizing stability and minimizing electrical resistance. Research Highlights It is feasible to use ion beam deposited Pt as electrical contacting material in operando electron microscopy. The deposited Pt is relatively stable up to 800°C and approx. 100 kA/cm2. The resistivity can be reduced by increasing the applied ion current during deposition and by thermal annealing at a temperature of 500°C in a few mbar of oxygen.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Ion‐beam deposited platinum as electrical contacting material in operando electron microscopy experiments at elevated temperatures

Simonsen¹,

Ma²,

Mariegaard³

et al. 2023

Microscopy Res & Technique

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“…One option is the processing of metals with magnetic and electric fields, which offers new possibilities for synthesis and control of microstructures. [ 1–6 ]…”

Section: Introductionmentioning

confidence: 99%

“…One option is the processing of metals with magnetic and electric fields, which offers new possibilities for synthesis and control of microstructures. [1][2][3][4][5][6] Electric fields, and the resultant currents produced in metals, have long been known to lead to directed atom transport or electromigration. [7,8] Electromigration has been a serious reliability issue for integrated circuits over the years because it can eventually result in the formation of voids and hillocks and lead to failure of conductor lines.…”

Section: Introductionmentioning

confidence: 99%

Control of Microstructure in Iron–Carbon Thin Films by Means of Electromigration

et al. 2023

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Herein, it is demonstrated that high DC electric current densities can be used to tailor the microstructure of iron–carbon thin films. Specifically, elongated ferrite grains can be formed in a nanocrystalline matrix via a process involving electromigration‐induced carbide migration. Herein this article, the parameters that are required to produce and control elongated grain formation in the Fe(C) system are mapped out and they are interpreted in terms of carbon electromigration, and the flux divergences need to reach a critical carbon concentration for precipitate growth and migration. Possible approaches to allow more precise control of the elongated grains are discussed, as are the requirements for material systems where microstructure control through electromigration should be feasible.

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“…As diferentes técnicas de conformação resultaram em diferenças microestruturais e de densificação. Os métodos de prensagem isostática e de colagem JESUS et al, 2016;RAFTERY et al, 2017;REN et al, 2018;CAMPOS et al, 2019;PRETTE;DICKEY, 2019;SCHWARZBACH et al, 2019;CAO;YOON et al, 2020).…”

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Influência dos parâmetros da sinterização >i<flash>/i< na densificação e microestrutura do ZnO

Storion

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STORION, A. G. Influence of the Flash Sintering parameters on the densification and microstructure of ZnO. 2023. 170 pp. Thesis (Doctorate) -University of São Paulo. Graduate Program in Materials Engineering and Science, Pirassununga, 2023.Alternative techniques to conventional sintering have been studied for controlling microstructure and grain growth, besides lower energy consumption. Among such techniques flash sintering stands out, providing fast shrinkage and densification in seconds. It applies to several materials, such as ZnO, an n-type semiconductor used in many electronic and optoelectronic devices. Despite numerous advances, flash sintering still faces some scientific challenges to overcome for its viability in industrial applications. To contribute to the advances in this scientific field, the present work aimed to evaluate the flash sintering parameters on ZnO microstructural homogeneity and application possibilities. During the parameterization step, it was possible to analyze the ideal process conditions, such as electrical and thermal parameters and material preparation. Subsequently, the influence of forming methods and the consequent density gradients formed in ZnO specimens on densification and microstructure when sintered via flash sintering was evaluated for the first time in the literature. The results indicated that the green density distribution generated during forming should be considered a decisive factor when evaluating specimens submitted to flash sintering. Also, flash sintering was investigated when coupled with thermal insulation with an alumina blanket (TIFS). The results showed that TIFS provided a more homogeneous microstructure, reducing the difference in grain size between the core and the surface of the specimen. TIFS, besides providing a 450°C decrease in the flash event onset temperature, was also able to achieve an estimated temperature during stage III only 100°C lower than that achieved for flash sintering under the same conditions, evidencing energy savings of up to 78% with the insulation process, compared to the uninsulated flash sintering experiments. The present work also aimed to evaluate the performance of flash-sintered ZnO when applied as a photocatalyst, since it may present great potential for application in the production of samples with refined microstructure, improving the surface reactivity. It was possible to prepare specimens with high porosity and sufficient integrity to be submitted to flash sintering. The results of the photocatalytic tests of the flash-sintered specimens were promising compared to the conventional-sintered ones, demonstrating the potential application of this alternative sintering route in the processing of photocatalysts.

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Towards In-Situ Electron Microscopy Studies of Flash Sintering

Cited by 8 publications

References 52 publications

Ion‐beam deposited platinum as electrical contacting material in operando electron microscopy experiments at elevated temperatures

Ion‐beam deposited platinum as electrical contacting material in operando electron microscopy experiments at elevated temperatures

Control of Microstructure in Iron–Carbon Thin Films by Means of Electromigration

Influência dos parâmetros da sinterização >i<flash>/i< na densificação e microestrutura do ZnO

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