Focused electron beam induced etching of copper in sulfuric acid solutions

Boehme, Lindsay; Bresin, Matthew; Botman, Aurélien; Ranney, James K.; Hastings, J. T.

doi:10.1088/0957-4484/26/49/495301

Cited by 7 publications

(11 citation statements)

References 41 publications

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“…Since electron and ion beam microscopes generally operate in high vacuum (with some limited exceptions), typically cells are used to encapsulate the liquid precursor. , These liquid cells are usually composed of silicon microchips and silicon nitride membranes, although a considerable amount of work has been done on polyimide membranes− and some nice work using graphene membranes, as well. The authors would also like to add that there are a few articles (and several conference papers) in which either environmental SEM or high-vacuum SEM with continuous liquid delivery enable processing without liquid cells. − In situ liquid cell electron microscopy has been used to investigate the mechanisms of electron-beam-induced nucleation, growth, and coalescence of nanoparticles in a variety of precursors at various concentrations. − To date, most in situ liquid cell studies have been performed using a SEM or a STEM.…”

Section: Ebid/ibid From Liquid Precursorsmentioning

confidence: 99%

Directing Matter: Toward Atomic-Scale 3D Nanofabrication

Jesse¹,

Borisevich²,

Fowlkes

et al. 2016

ACS Nano

104

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Enabling memristive, neuromorphic, and quantum-based computing as well as efficient mainstream energy storage and conversion technologies requires the next generation of materials customized at the atomic scale. This requires full control of atomic arrangement and bonding in three dimensions. The last two decades witnessed substantial industrial, academic, and government research efforts directed toward this goal through various lithographies and scanning-probe-based methods. These technologies emphasize 2D surface structures, with some limited 3D capability. Recently, a range of focused electron- and ion-based methods have demonstrated compelling alternative pathways to achieving atomically precise manufacturing of 3D structures in solids, liquids, and at interfaces. Electron and ion microscopies offer a platform that can simultaneously observe dynamic and static structures at the nano- and atomic scales and also induce structural rearrangements and chemical transformation. The addition of predictive modeling or rapid image analytics and feedback enables guiding these in a controlled manner. Here, we review the recent results that used focused electron and ion beams to create free-standing nanoscale 3D structures, radiolysis, and the fabrication potential with liquid precursors, epitaxial crystallization of amorphous oxides with atomic layer precision, as well as visualization and control of individual dopant motion within a 3D crystal lattice. These works lay the foundation for approaches to directing nanoscale level architectures and offer a potential roadmap to full 3D atomic control in materials. In this paper, we lay out the gaps that currently constrain the processing range of these platforms, reflect on indirect requirements, such as the integration of large-scale data analysis with theory, and discuss future prospects of these technologies.

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Section: Ebid/ibid From Liquid Precursorsmentioning

confidence: 99%

Directing Matter: Toward Atomic-Scale 3D Nanofabrication

Jesse¹,

Borisevich²,

Fowlkes

et al. 2016

ACS Nano

104

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“…35 Previously, we exploited these properties to demonstrate electron beam induced etching (EBIE) of copper using H2SO4. 36 Sulfuric acid is also a promising addition to solutions for liquid phase FEBID of Cu for several reasons. First, CuSO4-H2SO4-H2O is perhaps the most common system for copper electrodeposition and there is extensive guidance in the literature for choosing additives to control the morphology of the deposits.…”

Section: Copper Deposition From Cuso 4 and H 2 Somentioning

confidence: 99%

“…There is discussion in the literature as to the relative contributions of electrochemical and radiation chemical processes in LP-FEBID. 9,13,14,36,45 The reaction may be surface mediated, occurring in solution, or a combination of the two. In the first case, the e-beam is thought to create a localized virtual cathode on the substrate, thus enabling the electrodeposition of copper.…”

Section: Deposition Mechanismsmentioning

confidence: 99%

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Focused electron beam induced deposition of copper with high resolution and purity from aqueous solutions

2017

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Electron-beam induced deposition of high-purity copper nanostructures is desirable for nanoscale rapid prototyping, interconnection of chemically synthesized structures, and integrated circuit editing. However, metalorganic, gas-phase precursors for copper introduce high levels of carbon contamination. Here we demonstrate electron beam induced deposition of high-purity copper nanostructures from aqueous solutions of copper sulfate. The addition of sulfuric acid eliminates oxygen contamination from the deposit and produces a deposit with ∼95 at% copper. The addition of sodium dodecyl sulfate (SDS), Triton X-100, or polyethylene glycole (PEG) improves pattern resolution and controls deposit morphology but leads to slightly reduced purity. High resolution nested lines with a 100 nm pitch are obtained from CuSO-HSO-SDS-HO. Higher aspect ratios (∼1:1) with reduced line edge roughness and unintended deposition are obtained from CuSO-HSO-PEG-HO. Evidence for radiation-chemical deposition mechanisms was observed, including deposition efficiency as high as 1.4 primary electrons/Cu atom.

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“…Specifically, pattern reproducibility and consistency as well as electron scattering events are affected directly by liquid thickness. [27][28][29][30][31] However, controlling the thin liquid film in a partial vacuum has remained a serious challenge. Previously, we used shallow microwells to produce a meniscus which yielded a thin liquid layer close to the centre of the well.…”

Section: Introductionmentioning

confidence: 99%

Limiting regimes for electron-beam induced deposition of copper from aqueous solutions containing surfactants

Esfandiarpour

Hastings

2021

Nanotechnology

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Focused electron beam induced deposition of pure materials from aqueous solutions has been of interest in recent years. However, controlling the liquid film in partial vacuum is challenging. Here we modify the substrate to increase control over the liquid layer in order to conduct a parametric study of copper deposition in an environmental scanning electron microscope. We identified the transition from electron to mass-transport limited deposition as well as two additional regimes characterized by aggregated and high-aspect ratio deposits. We observe a high deposition efficiency of 1–10 copper atoms per primary electron that is consistent with a radiation chemical model of the deposition process.

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Focused electron beam induced etching of copper in sulfuric acid solutions

Cited by 7 publications

References 41 publications

Directing Matter: Toward Atomic-Scale 3D Nanofabrication

Directing Matter: Toward Atomic-Scale 3D Nanofabrication

Focused electron beam induced deposition of copper with high resolution and purity from aqueous solutions

Limiting regimes for electron-beam induced deposition of copper from aqueous solutions containing surfactants

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