The formation of CdS quantum dots and Au nanoparticles
-
Andreas Schiener
,
Alexander Krach
Abstract
We report on microsecond-resolved in-situ SAXS experiments of the early nucleation and growth behavior of both cadmium sulfide (CdS) quantum dots in aqueous solution including the temperature dependence and of gold (Au) nanoparticles. A novel free-jet setup was developped to access reaction times as early as 20 μs. As the signal in particular in the beginning of the reaction is weak the containment-free nature of this sample environment prooved crucial. The SAXS data reveal a two-step pathway with a surprising stability of a structurally relaxed cluster with a diameter of about 2 nm. While these develop rapidly by ionic assembly, a further slower growth is attributed to cluster attachment. WAXS diffraction confirms, that the particles at this early stage are not yet crystalline. This growth mode is confirmed for a temperature range from 25°C to 45°C. An energy barrier for the diffusion of primary clusters in water of 0.60 eV was experimentally observed in agreement with molecular simulations. To access reaction times beyond 100 ms, a stopped-drop setup -again contaiment- free is introduced. SAXS experiments on the growth of Au nanoparticles on an extended time scale provide a much slower growth with one population only. Further, the influence of ionizing X-ray radiation on the Au particle fromation and growth is discussed.
Acknowledgments
We gratefully acknowledge funding by the German Research Foundation (DFG) through Priority Program SPP1415 and support by the Graduate School GRK 1896. We furthermore acknowledge the European Synchrotron Radiation Facility for provision of synchrotron radiation facilities and we would like to thank Pawel Kwasniewski for assistance in using beamline ID 02. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357. We furthermore acknowledge the support by the APS 12-ID beamline staff.
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©2017 Walter de Gruyter GmbH, Berlin/Boston
Articles in the same Issue
- Frontmatter
- Graphical Synopsis
- Editorial
- Synthesis and characterization of metastable transition metal oxides and oxide nitrides
- Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets
- Thermal annealing of natural, radiation-damaged pyrochlore
- The formation of CdS quantum dots and Au nanoparticles
- Crystalline chalcogenido metalates – synthetic approaches for materials synthesis and transformation
- Fundamental theoretical and practical investigations of the polymorph formation of small amphiphilic molecules, their co-crystals and salts
- A density-functional theory approach to the existence and stability of molybdenum and tungsten sesquioxide polymorphs
- The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms
- Element allotropes and polyanion compounds of pnicogenes and chalcogenes: stability, mechanisms of formation, controlled synthesis and characterization
- Structure and ion dynamics of mechanosynthesized oxides and fluorides
- Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In2O3)
- Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials
- Phase formation and stability in TiOx and ZrOx thin films: Extremely sub-stoichiometric functional oxides for electrical and TCO applications
- Investigations on the growth of bismuth oxido clusters and the nucleation to give metastable bismuth oxide modifications
- Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
- Type-I silicon clathrates containing lithium
- Experimental and theoretical investigation of the chromium–vanadium–antimony system
- Synthesis and crystal structure of three new bismuth(III) arylsulfonatocarboxylates
- Snapshots of calcium carbonate formation – a step by step analysis
Articles in the same Issue
- Frontmatter
- Graphical Synopsis
- Editorial
- Synthesis and characterization of metastable transition metal oxides and oxide nitrides
- Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets
- Thermal annealing of natural, radiation-damaged pyrochlore
- The formation of CdS quantum dots and Au nanoparticles
- Crystalline chalcogenido metalates – synthetic approaches for materials synthesis and transformation
- Fundamental theoretical and practical investigations of the polymorph formation of small amphiphilic molecules, their co-crystals and salts
- A density-functional theory approach to the existence and stability of molybdenum and tungsten sesquioxide polymorphs
- The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms
- Element allotropes and polyanion compounds of pnicogenes and chalcogenes: stability, mechanisms of formation, controlled synthesis and characterization
- Structure and ion dynamics of mechanosynthesized oxides and fluorides
- Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In2O3)
- Development and application of novel NMR methodologies for the in situ characterization of crystallization processes of metastable crystalline materials
- Phase formation and stability in TiOx and ZrOx thin films: Extremely sub-stoichiometric functional oxides for electrical and TCO applications
- Investigations on the growth of bismuth oxido clusters and the nucleation to give metastable bismuth oxide modifications
- Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
- Type-I silicon clathrates containing lithium
- Experimental and theoretical investigation of the chromium–vanadium–antimony system
- Synthesis and crystal structure of three new bismuth(III) arylsulfonatocarboxylates
- Snapshots of calcium carbonate formation – a step by step analysis
