Thermal decomposition of some silver(I) carboxylates under nitrogen atmosphere

Szczęsny, Robert; Szłyk, Edward

doi:10.1007/s10973-012-2485-1

Cited by 39 publications

(20 citation statements)

References 23 publications

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“…Furthermore, the electron beam induced deposition of silver is challenging. Many potential precursor candidates have to be heated above 100 °C and show extremely low vapor pressures [ 22 – 25 ]. This is related to the main oxidation state of +1 for silver, which severely limits the possibility to attach appropriate ligands.…”

Section: Introductionmentioning

confidence: 99%

Towards the third dimension in direct electron beam writing of silver

Höflich¹,

Jurczyk²,

Madajska³

et al. 2018

Beilstein J. Nanotechnol.

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Carboxylates constitute an extremely promising class of precursor compounds for the electron beam induced deposition of silver. In this work both silver 2,2-dimethylbutyrate and silver pentafluoropropionate were investigated with respect to their dwell-time-dependent deposition behavior and growth characteristics. While silver 2,2-dimethylbutyrate showed a strong depletion in the center of the impinging electron beam profile hindering any vertical growth, silver pentafluoropropionate indicated a pronounced dependency of the deposit height on the dwell time. Truly three-dimensional silver structures could be realized with silver pentafluoropropionate. The pillars were polycrystalline with silver contents of more than 50 atom % and exhibit strong Raman enhancement. This constitutes a promising route towards the direct electron beam writing of three-dimensional plasmonic device parts from the gas phase.

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Section: Introductionmentioning

confidence: 99%

Towards the third dimension in direct electron beam writing of silver

Höflich¹,

Jurczyk²,

Madajska³

et al. 2018

Beilstein J. Nanotechnol.

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“…The synthesis of silver nanoparticles (Ag NPs) is well described in the literature (García-Barrasa et al 2011) and concerns thermolysis (Kashiwagi et al 2006; Keum et al 2008; Yamamoto and Nakamoto 2003) and reduction with commonly reducing agents such as acrylic or ascorbic acid (Vo et al 2010), hydrazine (N 2 H 4 ) (Dong et al 2009) or sodium borohydride (NaBH 4 ) in biphasic medium (Sarkar et al 2005), hydrogenolysis (Uznanski and Bryszewska 2010), sonolysis (Veith et al 2012), etc. Thus, thermolysis of carboxylate metal complex with no use of solvent, stabilizer, or reducing agent should be conducted at high temperatures (~250 °C) since too low temperature leads to a stabilization shell composed of silver ions rather than the fully reduced silver atoms (Shim et al 2008; Szczęsny and Szłyk 2013). Other methods require the use of solvent, stabilizer, or reducing agent and thus the post-reaction cleaning procedures connected with removing by-products (Bromberg et al 2010; Rao and Trivedi 2005).…”

Section: Introductionmentioning

confidence: 99%

Synthesis and characterization of silver nanoparticles from (bis)alkylamine silver carboxylate precursors

Uznański¹,

Zakrzewska²,

Favier³

et al. 2017

J Nanopart Res

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A comparative study of amine and silver carboxylate adducts [R1COOAg-2(R2NH2)] (R1 = 1, 7, 11; R2 = 8, 12) as a key intermediate in NPs synthesis is carried out via differential scanning calorimetry, solid-state FT-infrared spectroscopy, 13C CP MAS NMR, powder X-ray diffraction and X-ray photoelectron spectroscopy, and various solution NMR spectroscopies (1H and 13C NMR, pulsed field gradient spin-echo NMR, and ROESY). It is proposed that carboxyl moieties in the presence of amine ligands are bound to silver ions via chelating bidentate type of coordination as opposed to bridging bidentate coordination of pure silver carboxylates resulting from the formation of dimeric units. All complexes are packed as lamellar bilayer structures. Silver carboxylate/amine complexes show one first-order melting transition. The evidence presented in this study shows that phase behavior of monovalent metal carboxylates are controlled, mainly, by head group bonding. In solution, insoluble silver salt is stabilized by amine molecules which exist in dynamic equilibrium. Using (bis)amine-silver carboxylate complex as precursor, silver nanoparticles were fabricated. During high-temperature thermolysis, the (bis)amine-carboxylate adduct decomposes to produce silver nanoparticles of small size. NPs are stabilized by strongly interacting carboxylate and trace amounts of amine derived from the silver precursor interacting with carboxylic acid. A corresponding aliphatic amide obtained from silver precursor at high-temperature reaction conditions is not taking part in the stabilization. Combining NMR techniques with FTIR, it was possible to follow an original stabilization mechanism. Graphical abstractThe synthesis of a series (bis)alkylamine silver(I) carboxylate complexes in nonpolar solvents were carried out and fully characterized both in the solid and solution. Carboxyl moieties in the presence of amine ligands are bound to silver ions via chelating bidentate type of coordination. The complexes form layered structures which thermally decompose forming nanoparticles stabilized only by aliphatic carboxylates.

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“…Considering these requirements, metal aliphatic carboxylates, unsaturated, branched and/or substituted with a hydroxyl group, are preferred because they are easy to be transformed into metal atoms at low temperature via a decarboxylation reaction. 62,63 Besides, it is advantageous to use a precursor with higher metal content in the ink (10-40 wt% metal), so that a good balance between the printability of the formulated ink and the conductivity of the printed pattern can be obtained. 64 The solubility of the metal precursors in common solvents is also a factor to consider in metal precursor selection.…”

Section: Selection Of Metal Precursorsmentioning

confidence: 99%

“…However, others suggested that there are two stages in the thermal decomposition process of silver carboxylates. 63 The first stage is the formation of the silver(I) oxide and the anhydride of the corresponding acid. The anhydride and silver oxide are then transformed into the final products: RCOOH and Ag 0 .…”

Section: Selection Of Metal Precursorsmentioning

confidence: 99%