This thesis is devoted to the research and development of low processing temperature lead-free interconnect materials for microelectronic packaging applications with an emphasis on fundamental studies of nanoparticles synthesis, dispersion and oxidation prevention, and nanocomposites fabrication. Oxide-free tin (Sn), tin/silver (96.5Sn3.5Ag) and tin/silver/copper (96.5Sn3.0Ag0.5Cu) alloy nanoparticles with different sizes were synthesized by a low temperature chemical reduction method. Both size dependent melting point and latent heat of fusion of the synthesized nanoparticles were obtained. The nano lead-free solder pastes/composites created by dispersing the SnAg or SnAgCu alloy nanoparticles into an acidic type flux spread and wet on the cleaned copper surface at 220 to 230 ¡æ. This study demonstrated the feasibility of nano sized SnAg or SnAgCu alloy particle pastes for low processing temperature lead-free interconnect applications in microelectronic packaging. Surface functionalized silver nanoparticles and silver fakes were used as fillers for electrically conductive adhesives (ECAs) applications. During the curing of epoxy resin (150 ¡æ), the surfactants were debonded from the particles and at the same time the oxide layers on the particle surfaces were removed which facilitated the sintering of Ag nanoparticles. The contact interfaces between fillers were significantly reduced and an ultra highly conductive ECA with a resistivity of 5 ¡Á 10-6 ohm.cm was obtained. To enhance the adhesion of carbon nanotube (CNT) films to substrates, an ultra highly conductive ECA were used as a media to transfer the CNT films to copper substrates. The polymer wetted along the CNTs during curing process by the capillary force. An ohmic contact was formed between the copper substrates and the transferred CNTs. This process could overcome the serious obstacles of integration of CNTs into integrated circuits and microelectronic device packages by offering low processing temperatures and improved adhesion of CNTs to substrates. The transferred CNTs can be used to simultaneously form electrical and mechanical connections between chips and substrates.

abstract: Gold-silver alloy nanoparticles (NPs) capped with adenosine 5'-triphosphate were synthesized by borohydride reduction of dilute aqueous metal precursors. High-resolution transmission electron microscopy showed the as-synthesized particles to be spherical with average diameters ~4 nm. Optical properties were measured by UV-Visible spectroscopy (UV-Vis), and the formation of alloy NPs was verified across all gold:silver ratios by a linear shift in the plasmon band maxima against alloy composition. The molar absorptivities of the NPs decreased non-linearly with increasing gold content from 2.0 x 108 M-1 cm-1 (fÉmax = 404 nm) for pure silver to 4.1 x 107 M-1 cm-1 (fÉmax = 511 nm) for pure gold. The NPs were immobilized onto transparent indium-tin oxide composite electrodes using layer-by-layer (LbL) deposition with poly(diallyldimethylammonium) acting as a cationic binder. The UV-Vis absorbance of the LbL film was used to calculate the surface coverage of alloy NPs on the electrode. Typical preparations had average NP surface coverages of 2.8 x 10-13 mol NPs/cm2 (~5% of cubic closest packing) with saturated films reaching ~20% of ccp for single-layer preparations (1.0 ~ 10-12 mol NPs/cm2). X-ray photoelectron spectroscopy confirmed the presence of alloy NPs in the LbL film and showed silver enrichment of the NP surfaces by ~9%. Irreversible oxidative dissolution (dealloying) of the less noble silver atoms from the NPs on LbL electrodes was performed by cyclic voltammetry (CV) in sulfuric acid. Alloy NPs with higher gold content required larger overpotentials for silver dealloying. Dealloying of the more-noble gold atoms from the alloy NPs was also achieved by CV in sodium chloride. The silver was oxidized first to cohesive silver chloride, and then gold dealloyed to soluble HAuCl4- at higher potentials. Silver oxidation was inhibited during the first oxidative scan, but subsequent cycles showed typical, reversible silver-to-silver chloride voltammetry. The potentials for both silver oxidation and gold dealloying also shifted to more oxidizing potentials with increasing gold content, and both processes converged for alloy NPs with >60% gold content. Charge-mediated electrochemistry of silver NPs immobilized in LbL films, using Fc(meOH) as the charge carrier, showed that 67% of the NPs were electrochemically inactive. / Dissertation/Thesis / M.S. Chemistry 2014

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Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2016-06-22T13:42:56Z No. of bitstreams: 0 / Made available in DSpace on 2016-06-22T13:42:56Z (GMT). No. of bitstreams: 0 / Tese (Doutorado em Tecnologia Nuclear) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2016-06-22T13:42:56Z No. of bitstreams: 0 / Made available in DSpace on 2016-06-22T13:42:56Z (GMT). No. of bitstreams: 0 / Eletrocatalisadores baseados em Pd/C, PdCu/C, PdNi/C e PdAg/C foram produzidos pelo método de micro-ondas para serem utilizados como cátodo na célula a combustível alcalina na ausência e presença de álcool. Este método se mostrou bastante efetivo para a produção dos materiais, uma vez que as partículas apresentaram boa dispersão no suporte de carbono e produziram eletrocatalisadores com tamanho de partícula em torno de 3,5 nm, de acordo com as análises de DRX e MET. A partir das voltametrias cíclicas observa-se que para os eletrocatalisadores de PdCu/C e PdNi/C quanto maior a quantidade de Cu ou Ni, respectivamente, maior a área ativa do material estudado. Análises de disco anel rotatório foram realizadas nos eletrocatalisadores demonstrando que, independente da composição estudada, a quantidade produzida de peróxido foi de no máximo 4%. Estes dados corroboram com as inclinação das retas nas análises de Koutecky-Levich, uma vez que em ambos os casos a RRO ocorre via 4 elétrons. Análises de estabilidade dos materiais demonstraram que todos eles mantiveram ou melhoraram seu desempenho diante da RRO, quando se compara os dados obtidos antes e depois de 1000 ciclos voltamétricos. Testes de tolerância ao metanol e etanol foram realizados em meia célula com todas as composições de eletrocatalisadores produzidos. Na presença tanto de metanol quanto de etanol as composições atômica de 50:50, para todos os materiais estudados, foram as que demonstraram menor influência da presença do álcool durante a varredura linear da RRO. Nas medidas realizadas em célula unitária, com relação à tolerância ao metanol durante a RRO, o eletrocatalisador que demonstrou melhor desempenho foi o PdAg/C 70:30 enquanto que na presença de etanol o eletrocatalisador que demonstrou melhor desempenho foi o PdNi/C 70:30. / Tese (Doutorado em Tecnologia Nuclear) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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