Sculpting of Lead Sulfide Nanoparticles by Means of Acetic Acid and Dichloroethane

Gerdes, Frauke; Volkmann, Mirjam; Schliehe, Constanze; Bielewicz, Thomas; Klinke, Christian

doi:10.1515/zpch-2014-0584

Cited by 13 publications

(12 citation statements)

References 41 publications

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“…Octahedral PbS nanocrystals (NCs) were synthesized using a modified protocol . Briefly, 0.87 g (2.3 mmol) of lead(II) acetate trihydrate and 3.5 mL (11 mmol) of oleic acid were mixed in 15 mL of diphenyl ether in a three-neck flask.…”

Section: Methodsmentioning

confidence: 99%

“…Instead of using spherical NCs that display structural simplicity and morphological uncertainty, we synthesize octahedral PbS NCs with well-controlled dimensions as anisotropic building blocks to design the experiment, fabricate an environment cell, and develop the technique to investigate and analyze NC assembly (see the Experimental Section and the Supporting Information for full details). Such intelligent combination overcomes the limitations of previously studied samples of only several NC layers either with a fast nucleation rate or under a vacuum environment or both, enabling in situ and real time studies of NC assembly and subsequent growth at largely extended dimensions and under application-accessible operando conditions.…”

Section: Introductionmentioning

confidence: 99%

“…24−26 In order to leverage the large top-down control and fabrication of such superlattices discovered from the bottom-up NC assembly, 7,11,26 it is apparently critical to gain an in-depth understanding of the structural correlations of such superlattice polymorphs and underlying kinetics 27−31 and further to construct a distinct roadmap of NC assembly from the early nucleation and growth of a metastable lattice through additional intermediate events to the final formation of a stable one. 32−34 Instead of using spherical NCs that display structural simplicity and morphological uncertainty, we synthesize octahedral PbS NCs with well-controlled dimensions 35 as anisotropic building blocks to design the experiment, fabricate an environment cell, and develop the technique to investigate and analyze NC assembly (see the Experimental Section and the Supporting Information for full details). Such intelligent combination overcomes the limitations of previously studied samples of only several NC layers either with a fast nucleation rate or under a vacuum environment or both, enabling in situ and real time studies of NC assembly and subsequent growth at largely extended dimensions and under applicationaccessible operando conditions.…”

Section: ■ Introductionmentioning

confidence: 99%

See 2 more Smart Citations

In Situ Constructing the Kinetic Roadmap of Octahedral Nanocrystal Assembly Toward Controlled Superlattice Fabrication

Huang

Zhu

et al. 2021

J. Am. Chem. Soc.

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Crystallization and growth of anisotropic nanocrystals (NCs) into distinct superlattices were studied in real time, yielding kinetic details and designer parameters for scale-up fabrication of functional materials. Using octahedral PbS NC blocks, we discovered that NC assembly involves a primary lamellar ordering of NC-detached Pb(OA)2 molecules on the front-spreading solvent surfaces. Upon a spontaneous increase of NC concentration during solvent processing, PbS NCs preferentially self-assembled into an orientation-disordered face-centered cubic (fcc) superlattice, which subsequently transformed into a body-centered cubic (bcc) superlattice with single NC-orientational ordering across individual domains. Unlike the deformation-based transformation route claimed previously, this solid–solid phase transformation involved a hidden intermediate formation of a lamellar-confined liquid interface at cost of the disassembly (melting) of small fcc grains. Such highly condensed and liquidized NCs recrystallized into the stable bcc phase with an energy reduction of 1.16 k B T. This energy-favorable and high NC-fraction-driven bcc phase grew as a 2D film at a propagation rate of 0.74 μm/min, smaller than the 1.23 μm/min observed in the early nucleated fcc phase under a dilute NC environment. Taking such insights and defined parameters, we designed experiments to manipulate the NC assembly pathway and achieved scalable fabrication of a large/single bcc supercrystal with coherent ordering of NC translation and atomic plane orientation. This study not only provides a design avenue for controllable fabrication of a large supercrystal with desired superlattices for application but also sheds new light on the nature of crystal nucleation/growth and phase transformation by extending the lengths from the nanoscale into the atomic scale, molecular scale, and microscale levels.

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

See 1 more Smart Citation

In Situ Constructing the Kinetic Roadmap of Octahedral Nanocrystal Assembly Toward Controlled Superlattice Fabrication

Huang

Zhu

et al. 2021

J. Am. Chem. Soc.

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“…Under certain conditions, synthesis of 2D nanocrystals proceeds in two stages by self-assembly: at first, small objects are formed, then they combine with each other into nanosheets. This was observed in synthesis of lead chalcogenides [51][52][53].…”

Section: "Bottom-up" Methods For Obtaining 2d Nanocrystals [41]mentioning

confidence: 75%

Design of 2D-nanocrystals in water: preparation, structure and functionalization

Aslanov

Zakharov

Paseshnichenko

et al. 2018

Pure and Applied Chemistry

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A new method for synthesis of 2D nanocrystals in water was proposed. The use of perfluorothiophenolate ions as surfactant allowed us to produce 2D single-crystal nanosheets of CaS at pH=9 and flat nanocrystals of PbS at pH=9 at room temperature. Mesocrystalline nanobelts of CdS and mesocrystals of PbS were obtained at pH=3–5 and pH=10–12, respectively. Morphology, structure and chemical composition of nanoparticles were characterized by high-resolution transmission electron microscopy, electron diffraction and energy dispersive X-ray spectroscopy. A mechanism of nanoparticles formation was discussed.

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“…Alternatively, in the present work for the first time, various plasma treatment conditions have been employed in the ion energy range of 25-200 eV, and the physical processes occurring during surface modification have been analyzed using the crystals of one specific material: PbS. Considering that the formation of PbS nanostructures strongly depends on the synthesis conditions [28][29][30], one can anticipate that changing the plasma treatment conditions will result in various surface morphologies. Therefore, this work aims to study the formation of micro-and nanostructures on the surface of (100) PbS single crystals under various argon plasma treatment conditions.…”

Section: Introductionmentioning

confidence: 99%

Variation of Surface Nanostructures on (100) PbS Single Crystals during Argon Plasma Treatment

et al. 2022

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The nanostructuring of the (100) PbS single crystal surface was studied under varying argon plasma treatment conditions. The initial PbS single crystals were grown by high-pressure vertical zone melting, cut into wafer samples, and polished. Subsequently, the PbS single crystals were treated with inductively coupled argon plasma under varying treatment parameters such as ion energy and sputtering time. Plasma treatment with ions at a minimum energy of 25 eV resulted in the formation of nanotips with heights of 30–50 nm. When the ion energy was increased to 75–200 eV, two types of structures formed on the surface: high submicron cones and arrays of nanostructures with various shapes. In particular, the 120 s plasma treatment formed specific cruciform nanostructures with lateral orthogonal elements oriented in four <100> directions. In contrast, plasma treatment with an ion energy of 75 eV for 180 s led to the formation of submicron quasi-spherical lead structures with diameters of 250–600 nm. The nanostructuring mechanisms included a surface micromasking mechanism with lead formation and the vapor–liquid–solid mechanism, with liquid lead droplets acting as self-forming micromasks and growth catalysts depending on the plasma treatment conditions (sputtering time and rate).

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Sculpting of Lead Sulfide Nanoparticles by Means of Acetic Acid and Dichloroethane

Cited by 13 publications

References 41 publications

In Situ Constructing the Kinetic Roadmap of Octahedral Nanocrystal Assembly Toward Controlled Superlattice Fabrication

In Situ Constructing the Kinetic Roadmap of Octahedral Nanocrystal Assembly Toward Controlled Superlattice Fabrication

Design of 2D-nanocrystals in water: preparation, structure and functionalization

Variation of Surface Nanostructures on (100) PbS Single Crystals during Argon Plasma Treatment

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