Synthesis of active tin: an efficient reagent for allylation reaction of carbonyl compounds

Sinha, Arun K.; Sil, Amit; Sasmal, Anup Kumar; Pradhan, Mukul; Pal, Tarasankar

doi:10.1039/c4nj01913j

Cited by 11 publications

(8 citation statements)

References 31 publications

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“…However, after aerobic CO oxidation reaction the A 1g peak was more clearly observed as generally expected for SnO 2 NPs 15 44 . Upon anaerobic ethanol oxidation, no Raman signal was observed, in good consistent with the literature for metallic Sn 77 . For SnO 2 @C core-shells formed after aerobic ethanol oxidation, new strong Raman signals was observed, attributed to the shell-carbon species.…”

Section: Methodssupporting

confidence: 90%

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Kim

Lee

Sohn

2015

Sci Rep

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SnO2 has been studied intensely for applications to sensors, Li-ion batteries and solar cells. Despite this, comparatively little attention has been paid to the changes in morphology and crystal phase that occur on the metal oxide surface during chemical reactions. This paper reports anaerobic and aerobic ethanol and CO oxidation reactions over SnO2 nanoparticles (NPs), as well as the subsequent changes in the nature of the NPs. Uniform SnO2@C core-shells (10 nm) were formed by an aerobic ethanol oxidation reaction over SnO2 NPs. On the other hand, metallic Sn spheres were produced by an anaerobic ethanol oxidation reaction at 450 °C, which is significantly lower than that (1200 °C) used in industrial Sn production. Anaerobic and aerobic CO oxidation reactions were also examined. The novelty of the methods for the production of metallic Sn and SnO2@C core-shells including other anaerobic and aerobic reactions will contribute significantly to Sn and SnO2-based applications.

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Section: Methodssupporting

confidence: 90%

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Kim

Lee

Sohn

2015

Sci Rep

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“…At first, the E g , A 1g , and B 1g peaks at 467, 630, and 772 cm –1 were clearly visible but slowly decreased as the conversion reaction proceeded. This is due to the disappearance of the Sn–O bond, which is direct evidence that SnO 2 is transformed to metallic Sn (the peak that is related to the surface defect), , confirming that the phase transition is in agreement with in situ TEM analysis. The results suggest that reliable in situ TEM observation of electrode materials upon lithiation can be possible by using GLC, as realistic electrolyte conditions can be viable in the GLC system.…”

Section: Resultssupporting

confidence: 73%

Direct Realization of Complete Conversion and Agglomeration Dynamics of SnO₂ Nanoparticles in Liquid Electrolyte

et al. 2017

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The conversion reaction is important in lithium-ion batteries because it governs the overall battery performance, such as initial Coulombic efficiency, capacity retention, and rate capability. Here, we have demonstrated in situ observation of the complete conversion reaction and agglomeration of nanoparticles (NPs) upon lithiation by using graphene liquid cell transmission electron microscopy. The observation reveals that the Sn NPs are nucleated from the surface of SnO 2 , followed by merging with each other. We demonstrate that the agglomeration has a stepwise process, including rotation of a NP, formation of necks, and subsequent merging of individual NPs.

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“…S4 ‡), presumably a result of laser induced reaction between atmospheric O 2 and the tin metal. 53 For complexes 14, 16 and 18, AA-CVD afforded a range of thin films: for complex 14 deposition at both 300°C and 400°C, results in thin films with non-continuous crystalline material deposited over the substrates. SEM images (see Fig.…”

Section: Thin Film Deposition and Analysismentioning

confidence: 99%

Tin guanidinato complexes: oxidative control of Sn, SnS, SnSe and SnTe thin film deposition

et al. 2018

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A family of tin(ii) guanidinate complexes of the general form [{RNC(NMe2)NR}2Sn] (R = iPr (6), Cy (7), Tol (9) and Dipp (10)) and [{tBuNC(NMe2)NtBu}Sn{NMe2}] (8) have been synthesised and isolated from the reaction of tin(ii) bis-dimethylamide and a series of carbodiimides (1-5). The cyclic poly-chalcogenide compounds [{CyNC(NMe2)NCy}2Sn{Chx}] (Ch = S, x = 4 (11); Ch = Se, x = 4 (12), and Ch = S, x = 6 (13)) with {SnChx} rings were prepared by the oxidative addition of elemental sulfur and selenium to the heteroleptic stannylene complex [{CyNC(NMe2)NCy}2Sn] (7) in THF at room temperature. Similarly, reaction of compounds 6 and 7 with an equimolar amount of the chalcogen transfer reagents (SC3H6 and Se[double bond, length as m-dash]PEt3, respectively) led to the formation of the chalcogenide tin(iv) complexes [{RNC(NMe2)NR}Sn(Ch)] (R = Cy: Ch = S (14); R = iPr, Ch = Se (15); R = Cy, Ch = Se (16)) with terminal Sn[double bond, length as m-dash]Ch (14 and 16) and dimeric bridged seleno-tin {Sn2Se2} rings (15), respectively. The mono telluro-compounds [{RNC(NMe2)NR}Sn(Te)] (R = iPr (17); R = Cy (18)) were similarly prepared by the oxidative addition of elemental tellurium to 7 and 8, respectively. All of the tin containing compounds have been investigated by multinuclear NMR (1H, 13C 119Sn and 77Se/125Te, where possible), elemental analysis and single crystal X-ray structural analysis (7, 8, 10-13, 15-18). Thermogravimetric analysis (TGA) was used to probe the possible utility of complexes 6-8, 11-12 and 14-18 as single source Sn and SnCh precursors. The Sn(ii) compounds 6 and 7 have been utilised in the growth of thin films by aerosol-assisted chemical vapor deposition (AACVD) at both 300 and 400 °C. The thin films have been analysed by pXRD, EDS, SEM and AFM and shown to be Sn metal. Subsequent studies provided film growth at temperatures as low as 200 °C. Similarly, the mono-chalcogenide systems 14, 16 and 18 have been utilised in the AACVD of thin films. These latter studies provided films, grown at 300 and 400 °C, which have also been analysed by pXRD, Raman spectroscopy, AFM, and SEM and are shown to comprise phase pure SnS, SnSe and SnTe, respectively. These preliminary results demonstrate the potential of such simple guanidinate complexes to act as single source precursors with a high degree of oxidative control over the deposited thin films.

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Synthesis of active tin: an efficient reagent for allylation reaction of carbonyl compounds

Abstract: High purity Sn(0), synthesized through reduction of SnO by Na2SnO2, is applied for allylation of carbonyls in distilled water at room temperature.

Cited by 11 publications

References 31 publications

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Direct Realization of Complete Conversion and Agglomeration Dynamics of SnO₂ Nanoparticles in Liquid Electrolyte

Tin guanidinato complexes: oxidative control of Sn, SnS, SnSe and SnTe thin film deposition

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Synthesis of active tin: an efficient reagent for allylation reaction of carbonyl compounds

Abstract: High purity Sn(0), synthesized through reduction of SnO by Na2SnO2, is applied for allylation of carbonyls in distilled water at room temperature.

Cited by 11 publications

References 31 publications

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Metallic Sn spheres and SnO2@C core-shells by anaerobic and aerobic catalytic ethanol and CO oxidation reactions over SnO2 nanoparticles

Direct Realization of Complete Conversion and Agglomeration Dynamics of SnO2 Nanoparticles in Liquid Electrolyte

Tin guanidinato complexes: oxidative control of Sn, SnS, SnSe and SnTe thin film deposition

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Direct Realization of Complete Conversion and Agglomeration Dynamics of SnO₂ Nanoparticles in Liquid Electrolyte