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      Structural and optical properties of penicillamine-protected gold nanocluster fractions separated by sequential size-selective fractionation

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          Abstract

          Polydisperse water-soluble gold nanoclusters (AuNCs) protected by penicillamine have been synthesized in this work. The sequential size-selective precipitation (SSSP) technique has been applied for the size fractionation and purification of the monolayer-protected AuNCs. Through continuously adding acetone to a crude AuNC aqueous solution and controlling the volume percentage of acetone, we successfully separated the polydisperse AuNCs with diameters ranging from 0.5 to 5.4 nm into four different fractions sequentially. High-resolution transmission electron microscopy (HRTEM) shows that the four fractions are well-dispersed spherical particles of diameter 3.0 ± 0.6, 2.3 ± 0.5, 1.7 ± 0.4, and 1.2 ± 0.4 nm. Proton nuclear magnetic resonance spectroscopy suggests that disulfide, excess ligands and gold(I) complexes were removed from the AuNCs fractions. These results demonstrate the considerable potential of the SSSP technique for size-based separation and purification of AuNCs, achieving not only the isolation of larger nanoclusters (NCs) from small NCs in a continuous fashion, but also for the removal of small-molecule impurities. Based on the results from the mass spectrometry and thermogravimetric analysis, the average composition of the four fractions can be represented by Au 38(SR) 18, Au 28(SR) 15, Au 18(SR) 12, and Au 11(SR) 8, respectively. This indicates that the SSSP separation is mainly dependent on the core size and the ratio of Au atoms to ligands of AuNCs. X-ray photoelectron spectroscopy (XPS) has also been applied to observe the molecular dependence on the gold and sulfur chemical state of organosulfur monolayers of the fractions. The photoluminescence spectra of these AuNCs in the range of 900–790 nm was investigated at room temperature. The results show that the peak emission energy of the size-selected AuNCs undergoes a blue shift when the size is decreased, which can be attributed to the quantum confinement effect.

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          Selective oxidation with dioxygen by gold nanoparticle catalysts derived from 55-atom clusters.

          Mark Turner, Vladimir B Golovko, Owain Vaughan … (2008)
          Supported gold nanoparticles have excited much interest owing to their unusual and somewhat unexpected catalytic properties, but the origin of the catalytic activity is still not fully understood. Experimental work on gold particles supported on a titanium dioxide (110) single-crystal surface has established a striking size threshold effect associated with a metal-to-insulator transition, with gold particles catalytically active only if their diameters fall below approximately 3.5 nm. However, the remarkable catalytic behaviour might also in part arise from strong electronic interaction between the gold and the titanium dioxide support. In the case of industrially important selective oxidation reactions, explanation of the effectiveness of gold nanoparticle catalysts is complicated by the need for additives to drive the reaction, and/or the presence of strong support interactions and incomplete understanding of their possible catalytic role. Here we show that very small gold entities ( approximately 1.4 nm) derived from 55-atom gold clusters and supported on inert materials are efficient and robust catalysts for the selective oxidation of styrene by dioxygen. We find a sharp size threshold in catalytic activity, in that particles with diameters of approximately 2 nm and above are completely inactive. Our observations suggest that catalytic activity arises from the altered electronic structure intrinsic to small gold nanoparticles, and that the use of 55-atom gold clusters may prove a viable route to the synthesis of robust gold catalysts suited to practical application.
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            Rapid purification and size separation of gold nanoparticles via diafiltration.

            Scott Sweeney, Gerd H Woehrle, James E. Hutchison (2006)
            Purification and size-based separation of nanoparticles remain significant challenges in the preparation of well-defined materials for fundamental studies and applications. Diafiltration shows considerable potential for the efficient and convenient purification and size separation of water-soluble nanoparticles, allowing for the removal of small-molecule impurities and for the isolation of small nanoparticles from larger nanostructures in a single process. Herein, we report studies aimed at assessing the suitability of diafiltration for (i) the purification of water-soluble thiol-stabilized 3-nm gold nanoparticles, (ii) the separation of a bimodal distribution of nanoparticles into the corresponding fractions, and (iii) the separation of a polydisperse sample into fractions of differing mean core diameter. NMR, thermogravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS) measurements demonstrate that diafiltration produces nanoparticles with a much higher degree of purity than is possible by dialysis or a combination of solvent washes, chromatography, and ultracentrifugation. UV-visible spectroscopic and transmission electron microscopic (TEM) analyses show that diafiltration offers the ability to separate nanoparticles of disparate core size. These results demonstrate the applicability of diafiltration for the rapid and green preparation of high-purity gold nanoparticle samples and the size separation of heterogeneous nanoparticle samples. They also suggest the development of novel diafiltration membranes specifically suited to high-resolution nanoparticle size separation.
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              A recyclable supramolecular membrane for size-selective separation of nanoparticles.

              Elisha Krieg, Haim Weissman, Elijah Shirman … (2011)
              Most practical materials are held together by covalent bonds, which are irreversible. Materials based on noncovalent interactions can undergo reversible self-assembly, which offers advantages in terms of fabrication, processing and recyclability, but the majority of noncovalent systems are too fragile to be competitive with covalent materials for practical applications, despite significant attempts to develop robust noncovalent arrays. Here, we report nanostructured supramolecular membranes prepared from fibrous assemblies in water. The membranes are robust due to strong hydrophobic interactions, allowing their application in the size-selective separation of both metal and semiconductor nanoparticles. A thin (12 µm) membrane is used for filtration (∼5 nm cutoff), and a thicker (45 µm) membrane allows for size-selective chromatography in the sub-5 nm domain. Unlike conventional membranes, our supramolecular membranes can be disassembled using organic solvent, cleaned, reassembled and reused multiple times.
              Article 0 comments Cited 53 times – based on 0 reviews     Review now
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                Author and article information

                Contributors
                Xiupei Yang:
                ORCID: http://orcid.org/0000-0001-6799-5442
                Martin M F Choi
                Jörg J Schneider: Role: Associate Editor
                Journal
                Journal ID (nlm-ta): Beilstein J Nanotechnol
                Journal ID (iso-abbrev): Beilstein J Nanotechnol
                Title: Beilstein Journal of Nanotechnology
                Publisher: Beilstein-Institut (Trakehner Str. 7-9, 60487 Frankfurt am Main, Germany )
                ISSN (Electronic): 2190-4286
                Publication date Collection: 2019
                Publication date (Electronic): 25 April 2019
                Volume: 10
                Pages: 955-966
                Affiliations
                [1 ]College of Chemistry and Chemical Engineering, China West Normal University, Nanchong 637000, China
                [2 ]Partner State Key Laboratory of Environmental and Biological Analysis, and Department of Chemistry, Hong Kong Baptist University, 224 Waterloo Road, Kowloon Tong, Hong Kong SAR, China
                Author information
                http://orcid.org/0000-0001-6799-5442
                Article
                DOI: 10.3762/bjnano.10.96
                PMC ID: 6541327
                SO-VID: 8b0aab56-416a-481d-9fa2-b95db9289f73
                Copyright © Copyright © 2019, Yang et al.; licensee Beilstein-Institut.
                License:

                This is an Open Access article under the terms of the Creative Commons Attribution License ( http://creativecommons.org/licenses/by/4.0). Please note that the reuse, redistribution and reproduction in particular requires that the authors and source are credited.

                The license is subject to the Beilstein Journal of Nanotechnology terms and conditions: (https://www.beilstein-journals.org/bjnano)

                History
                Date received : 23 January 2019
                Date accepted : 3 April 2019
                Categories
                Subject: Full Research Paper
                Subject: Nanoscience
                Subject: Nanotechnology

                Keywords: gold nanoclusters,monolayer-protected gold nanoclusters,sequential size-selective fractionation
                Data availability:
                Keywords: gold nanoclusters, monolayer-protected gold nanoclusters, sequential size-selective fractionation

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