Challenges and opportunities in the bottom-up mechanochemical synthesis of noble metal nanoparticles

Oliveira, P. M. S.; Torresi, Roberto Manuel; Emmerling, Franziska; Camargo, Pedro H. C.

doi:10.1039/d0ta05183g

Cited by 183 publications

(98 citation statements)

References 144 publications

(259 reference statements)

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“…Metal and mixed metal and semiconductor oxides are widely applied in several fields, as supercapacitors [1][2][3], gas sensors based on chemoresistivity [4][5][6][7][8] or dielectric excitation [9,10], heterojunctions [11,12], energy storage in batteries [13][14][15], and electrochemistry [16][17][18]. Their properties can be varied in different ways, by doping [19,20], capping, and controlling the structure, shape, and size with bottom-up and top-down approaches [21][22][23][24][25][26][27][28]. The types of synthesis include sol-gel methods, hydrothermal synthesis, solvothermal synthesis, and electrospinning [29][30][31][32][33][34][35].…”

Section: Introductionmentioning

confidence: 99%

Room Temperature Syntheses of ZnO and Their Structures

et al. 2021

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ZnO has many technological applications which largely depend on its properties, which can be tuned by controlled synthesis. Ideally, the most convenient ZnO synthesis is carried out at room temperature in an aqueous solvent. However, the correct temperature values are often loosely defined. In the current paper, we performed the synthesis of ZnO in an aqueous solvent by varying the reaction and drying temperatures by 10 °C steps, and we monitored the synthesis products primarily by XRD). We found out that a simple direct synthesis of ZnO, without additional surfactant, pumping, or freezing, required both a reaction (TP) and a drying (TD) temperature of 40 °C. Higher temperatures also afforded ZnO, but lowering any of the TP or TD below the threshold value resulted either in the achievement of Zn(OH)2 or a mixture of Zn(OH)2/ZnO. A more detailed Rietveld analysis of the ZnO samples revealed a density variation of about 4% (5.44 to 5.68 gcm−3) with the synthesis temperature, and an increase of the nanoparticles’ average size, which was also verified by SEM images. The average size of the ZnO synthesized at TP = TD = 40 °C was 42 nm, as estimated by XRD, and 53 ± 10 nm, as estimated by SEM. For higher synthesis temperatures, they vary between 76 nm and 71 nm (XRD estimate) or 65 ± 12 nm and 69 ± 11 nm (SEM estimate) for TP =50 °C, TD = 40 °C, or TP = TD = 60 °C, respectively. At TP = TD = 30 °C, micrometric structures aggregated in foils are obtained, which segregate nanoparticles of ZnO if TD is raised to 40 °C. The optical properties of ZnO obtained by UV-Vis reflectance spectroscopy indicate a red shift of the band gap by ~0.1 eV.

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Section: Introductionmentioning

confidence: 99%

Room Temperature Syntheses of ZnO and Their Structures

et al. 2021

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“…The properties of nanoparticles are highly dependent on the method of synthesis and preparative conditions such as precursor nature and concentration, synthesis temperature and time, solution pH, and the nature of the chelating agent [ 16 ]. To exploit the novel properties of nanoparticles for a variety of applications, it is essential to tune the size, phase, structure, shape, and composition by optimizing the above-mentioned parameters.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of π-SnS Nanoparticles and Corresponding Thin Films

et al. 2021

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Tin sulfide polymorph (π-SnS) nanoparticles exhibit promising optoelectrical characteristics for photovoltaic and hydrogen production performance, mainly because of the possibility of tuning their properties by adjusting the synthesis conditions. This study demonstrates a chemical approach to synthesize π-SnS nanoparticles and the engineering of their properties by altering the Sn precursor concentration (from 0.04 M to 0.20 M). X-ray diffraction and Raman studies confirmed the presence of pure cubic SnS phase nanoparticles with good crystallinity. SEM images indicated the group of cloudy shaped grains, and XPS results confirmed the presence of Sn and S in the synthesized nanoparticles. Optical studies revealed that the estimated energy bandgap values of the as-synthesized π-SnS nanoparticles varied from 1.52 to 1.68 eV. This work highlights the effects of the Sn precursor concentration on the properties of the π-SnS nanoparticles and describes the bandgap engineering process. Optimized π-SnS nanoparticles were used to deposit nanocrystalline π-SnS thin films using the drop-casting technique, and their physical properties were improved by annealing (300 °C for 2 h).

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“…Mechanochemistry has emerged as an attractive and sustainable synthetic tool 1,2 with applications for the synthesis of organic, [3][4][5][6][7] inorganic, [8][9][10] and hybrid metal-organic molecules and materials. [11][12][13][14] It is increasingly clear that many traditional solution based chemical reactions can be performed in the presence of very little or no solvent using mechanochemical approaches.…”

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confidence: 99%

Changing the Game of Time Resolved X-Ray Diffraction on the Mechanochemistry Playground by Downsizing

Lampronti¹,

Michalchuk

Mazzeo³

et al. 2021

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Time resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. We report how a combination of new miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by ex situ measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.

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Challenges and opportunities in the bottom-up mechanochemical synthesis of noble metal nanoparticles

Abstract: Mechanochemistry is a promising alternative to solution-based protocols across the chemical sciences, enabling different types of chemistries in solvent-free and environmentally benign conditions. The use of mechanical energy to promote...

Cited by 183 publications

References 144 publications

Room Temperature Syntheses of ZnO and Their Structures

Room Temperature Syntheses of ZnO and Their Structures

Synthesis and Characterization of π-SnS Nanoparticles and Corresponding Thin Films

Changing the Game of Time Resolved X-Ray Diffraction on the Mechanochemistry Playground by Downsizing

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