Organic electrical energy storage (EES) is a growing field of research that is expected to play an important role in the future, as the need for sustainable EES increases. Conducting redox polymers (CRPs), i.e. conducting polymers with incorporated redox active moieties e.g. as pendant groups (PGs), are proposed as a promising class of compounds for this purpose. Redox cycling of the PGs can be utilized for high charge storage capacity, while the conducting polymer backbone provides fast charge transport through the material. Some of the major challenges with small-molecule systems for EES could be solved by using CRPs, e.g. capacity fading due to dissolution of the active compound, and high resistance due to slow charge transport between molecules. The latter issue is often solved by adding large amounts of conducting additives to the active material, drastically lowering the specific capacity. In this project, CRPs are shown to be able to function in battery cells without any additives, making both high capacity and high power possible. Although several CRPs have been reported in the literature, very few detailed studies have been conducted on the electrochemical processes of the two systems (i.e. the conducting polymer backbone and the redox active PGs). An important factor to consider in CRP design is the possibility for interaction between the two redox systems, which could be either beneficial or detrimental to the function as EES material. In this thesis, CRP model systems composed of hydroquinone functionalized polypyrrole have been studied, and they exhibit separate redox reactions for the PGs and the backbone, overlapping in potential. Significant interaction between them was observed, as oxidation of the PGs has severe impact on the backbone: When the oxidized and hydrophobic p-benzoquinone PGs are formed, they pack and force the polymer backbone to twist, localizing the bipolarons, and decreasing the conductivity. This is accompanied by a contraction of the polymer film and expulsion of electrolyte. Overall, the interaction in these polymers is destructive for their EES function, and it could be eliminated by introduction of a long linker unit between the PGs and the backbone.

Interactions between carbohydrates and proteins are increasingly being recognized as crucial in many biological processes, such as cellular adhesion and communication. In order to investigate the interactions of carbohydrates and proteins, the development of efficient analytic technologies, as well as novel strategies for the synthesis of carbohydrates, have to be explored. To date, several methods have been exploited to analyze interactions of carbohydrates and proteins, for example, biosensors, nuclear magnetic resonance (NMR); enzyme-linked immunosorbent assays (ELISA), X-ray crystallography and array technologies. This thesis describes the development of novel strategies for the synthesis of carbohydrates, as well as new efficient strategies to Quartz Crystal Microbalance- (QCM-) biosensors and carbohydrate microarrays technologies. These methodologies have been used to probe carbohydrate-lectin-interactions for a range of plant and animal lectins. / QC 20100915

Made available in DSpace on 2014-06-11T19:23:05Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-02-25Bitstream added on 2014-06-13T20:29:48Z : No. of bitstreams: 1 pesquero_nc_me_araiq.pdf: 1328191 bytes, checksum: b43c0dd0e4c51db5570dd9acd342760e (MD5) / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / No presente trabalho foi avaliada a equivalência entre as formas nativa e recombinante da lectina Artin M utilizando como ligante a peroxidase de raiz forte (HRP) por meio da técnica de microbalança a cristal de quartzo. Para tal foi preparado um biossensor por meio da imobilização da lectina, tanto nativa como recombinante, na superfície do cristal de quartzo piezelétrico. A imobilização das lectinas foi realizada por meio da construção de uma monocamada auto organizada utilizando dois alcanotióis, ácido 11-mercaptoundecanóico e o 2-mercaptoetanol. Para o acoplamento das proteínas foram utilizados N-etil-N- (dimetilaminopropil) carbodiimida (EDC) e N-hidoxisuccinimida (NHS) que formam com os grupamentos carboxílicos um intermediário reativo. Após a preparação do biossensor foi utilizado um sistema de injeção em fluxo acoplado à microbalança de cristal a quartzo para o estudo da interação lectina-glicoconjugado. Desta forma, as interações da Artin M nativa e recombinante com a glicoproteína peroxidase de raiz forte foram estudadas por meio da determinação das suas constantes de afinidade aparente e de associação cinética, sendo que foram encontrados os valores de constante de afinidade aparente (4,6 ± 0,9) x 103 e (2,6 ± 0,5) x 103 L mol -1 para as interações jArtinM-HRP e rArtinM-HRP, e os valores de constante cinética (7 ± 3) x 103 e (7 ± 2) x 103 L mol -1 para as interações jArtinM-HRP e rArtinM-HRP. Os valores das constantes de interação obtidos evidenciaram a equivalência entre ambas as formas da lectina Artin M. Neste trabalho também foi determinada a constante de associação cinética da interação entre a lectina Artin M recombinante e linhagens celulares de leucemia mielóide aguda humana (NB4, K562 e U937), no intuito de melhor entender a diferença na citotoxicidade observada da Artin M sobre estas células... / In the present work was evaluated the equivalence between the native and recombinant forms of Artin M using horseradish peroxidase as ligand by means the quartz crystal microbalance technique. In this way, a biosensor was prepared immobilizing the lectin, native and recombinant forms, on piezoelectric quartz crystal surface. Lectins immobilization was realized constructing self assembled monolayers using the alkanethiols 11-mercaptoundecanoic acid and 2-mercaptoethanol. To the binding of proteins was used N-ethyl-N-(dimethylaminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS), which form with carboxylic groups a reactive intermediary. After biosensor preparation was utilized a flow injection system coupled to quartz crystal microbalance to study the lectin-glycoconjugated interaction. Thus the native Artin M and recombinant Artin M interaction with horseradish peroxidase glycoprotein were studied by determining its apparent affinity constant and association kinetic constants. The values obtained to apparent affinity constant were (4,6 ± 0,9) x 103 e (2,6 ± 0,5) x 103 L mol -1 to jArtinM-HRP e rArtinM-HRP interactions, and the values obtained to association kinetic constant were (7 ± 3) x 103 e (7 ± 2) x 103 L mol -1 to jArtinM-HRP e rArtinM-HRP interactions. These constant values evidence the equivalence between native and recombinant forms of Artin M lectin. During this work were also determined the association kinetic constant of the interaction between recombinant Artin M and leukemic lineages from human acute myeloid leukemia (NB4, K562 and U937), with the purpose of a better understanding in the different cytotoxic effect of Artin M on these cells. In this way the values of association kinetic constant obtained was (0,3 ± 0,1) x 10-7 , (0,9 ± 0,1) x 10-7 e (2,7 ± 0,3) x 10-7 mL cel -1 to the interactions between Artin M and NB4, K562 and U937, respectively

Orientador: Paulo Roberto Bueno / Banca: Marcelo Mulato / Banca: Maria Cristina Roque Antunes Barreira / Resumo: No presente trabalho foi avaliada a equivalência entre as formas nativa e recombinante da lectina Artin M utilizando como ligante a peroxidase de raiz forte (HRP) por meio da técnica de microbalança a cristal de quartzo. Para tal foi preparado um biossensor por meio da imobilização da lectina, tanto nativa como recombinante, na superfície do cristal de quartzo piezelétrico. A imobilização das lectinas foi realizada por meio da construção de uma monocamada auto organizada utilizando dois alcanotióis, ácido 11-mercaptoundecanóico e o 2-mercaptoetanol. Para o acoplamento das proteínas foram utilizados N-etil-N- (dimetilaminopropil) carbodiimida (EDC) e N-hidoxisuccinimida (NHS) que formam com os grupamentos carboxílicos um intermediário reativo. Após a preparação do biossensor foi utilizado um sistema de injeção em fluxo acoplado à microbalança de cristal a quartzo para o estudo da interação lectina-glicoconjugado. Desta forma, as interações da Artin M nativa e recombinante com a glicoproteína peroxidase de raiz forte foram estudadas por meio da determinação das suas constantes de afinidade aparente e de associação cinética, sendo que foram encontrados os valores de constante de afinidade aparente (4,6 ± 0,9) x 103 e (2,6 ± 0,5) x 103 L mol -1 para as interações jArtinM-HRP e rArtinM-HRP, e os valores de constante cinética (7 ± 3) x 103 e (7 ± 2) x 103 L mol -1 para as interações jArtinM-HRP e rArtinM-HRP. Os valores das constantes de interação obtidos evidenciaram a equivalência entre ambas as formas da lectina Artin M. Neste trabalho também foi determinada a constante de associação cinética da interação entre a lectina Artin M recombinante e linhagens celulares de leucemia mielóide aguda humana (NB4, K562 e U937), no intuito de melhor entender a diferença na citotoxicidade observada da Artin M sobre estas células ... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In the present work was evaluated the equivalence between the native and recombinant forms of Artin M using horseradish peroxidase as ligand by means the quartz crystal microbalance technique. In this way, a biosensor was prepared immobilizing the lectin, native and recombinant forms, on piezoelectric quartz crystal surface. Lectins immobilization was realized constructing self assembled monolayers using the alkanethiols 11-mercaptoundecanoic acid and 2-mercaptoethanol. To the binding of proteins was used N-ethyl-N-(dimethylaminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS), which form with carboxylic groups a reactive intermediary. After biosensor preparation was utilized a flow injection system coupled to quartz crystal microbalance to study the lectin-glycoconjugated interaction. Thus the native Artin M and recombinant Artin M interaction with horseradish peroxidase glycoprotein were studied by determining its apparent affinity constant and association kinetic constants. The values obtained to apparent affinity constant were (4,6 ± 0,9) x 103 e (2,6 ± 0,5) x 103 L mol -1 to jArtinM-HRP e rArtinM-HRP interactions, and the values obtained to association kinetic constant were (7 ± 3) x 103 e (7 ± 2) x 103 L mol -1 to jArtinM-HRP e rArtinM-HRP interactions. These constant values evidence the equivalence between native and recombinant forms of Artin M lectin. During this work were also determined the association kinetic constant of the interaction between recombinant Artin M and leukemic lineages from human acute myeloid leukemia (NB4, K562 and U937), with the purpose of a better understanding in the different cytotoxic effect of Artin M on these cells. In this way the values of association kinetic constant obtained was (0,3 ± 0,1) x 10-7 , (0,9 ± 0,1) x 10-7 e (2,7 ± 0,3) x 10-7 mL cel -1 to the interactions between Artin M and NB4, K562 and U937, respectively / Mestre

Orientador: Lauro Tatsuo Kubota / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-07T10:16:36Z (GMT). No. of bitstreams: 1 Damos_FlavioSantos_D.pdf: 8044516 bytes, checksum: a3443f4130ad6150c52dfa20c571bb04 (MD5) Previous issue date: 2006 / Resumo: O presente trabalho descreve as aplicações da ressonância de plásmon de superfície (surface plasmon resonance-SPR) e da microbalança de cristal de quartzo (quartz crystal microbalance-QCM) na investigação de processos interfaciais, visando o melhor entendimento e aplicação dos sistemas investigados bem como o estabelecimento das aplicações da técnica SPR aliada à eletroquímica. Neste sentido são apresentadas investigações do comportamento óptico-eletroquímico da molécula de azul de metileno (sistema 1), polímeros condutores (sistema 2) e monocamadas auto-organizadas (sistema 3). A escolha de tais sistemas, embora distintos, tem a finalidade de exploração ampla da técnica SPR na investigação de processos superficiais e interfaciais. O uso da técnica SPR na investigação do sistema 1 mostra a sua aplicabilidade no monitoramento do intumescimento de filmes em dimensões nanométricas e a investigação de processos adsortivos e difusionais com elevada sensibilidade. Assim sendo, a técnica SPR foi aplicada na investigação de processos de formação de filmes finos de polímeros condutores, bem como os processos de dopagem destes filmes. Neste sentido, foi investigada a eletropolimerização do pirrol e da polianilina bem como o efeito de dopantes aniônicos sobre as propriedades ópticas e eletroquímicas destes materiais. As medidas ópticas obtidas foram correlacionadas aos processos de dopagem e desdopagem dos filmes confeccionados mediante um estudo comparativo destes processos por QCM tendo em vista a consolidação da mesma na investigação de tais processos. Por fim, com o propósito de explorar a sensibilidade da técnica SPR a sistemas de dimensões sub-nanométricas, foram investigadas monocamadas auto-organizadas de ácido 11-mercapto-undecanóico e mono(6-deoxi-6-mercapto)-b-ciclodextrina. Neste sentido, foram determinadas a espessura e a constante dielétrica destes filmes, assim como a cinética de adsorção destes empregando um modelo de adsorção fundamentado na adsorção, desorção e re-arranjo molecular / Abstract: The present work describes the applications of surface plasmon resonance (SPR) and quartz crystal microbalance (QCM) in the investigation of interface processes in the attempt to improve the understanding and application of the investigated systems as well as the establishment of the applications of the SPR allied with electrochemical techniques. In this sense, are presented the investigation of the electrochemical behavior of the methylene blue molecule (system 1), conducting polymers (system 2) and self-assembled monolayers (system 3). The selection of these systems, although distinct, has a focus on the exploration of the SPR technique in the investigation of surface and interface processes. The use of SPR technique in the investigation of the system 1 shows its applicability in the monitoring of swelling of films in nanometric size as well as the investigation of adsorptive and diffusional processes with high sensitivity. Thus, SPR was applied in the investigation of construction of thin conducting polymer films as well as its doping processes. In this sense, were investigated pyrrole and aniline electropolymerization as well as the effects of anionic dopants on its optical and electrochemical properties. The optical measurements were correlated with the doping and dedoping processes of the films by means of a comparative study of these processes by QCM due to the better establishment of this technique in the investigation of these processes. Finally, with the purpose of explore the sensitivity of the SPR technique in sub-nanometric size systems, the SPR technique was applied in the investigation of selfassembled monolayers of 11-mercapto-undecanoic acid and mono(6-deoxy-6-mercapto)-b- cyclodextrin. In this sense, were determined the thickness and dielectric constant of these films as well as the adsorption kinetic by using a kinetic model based on adsorption, desorption and re-arrangement of molecules / Doutorado / Físico-Química / Mestre em Química

Orientador: David Mendez Soares / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-15T00:08:17Z (GMT). No. of bitstreams: 1 Gomes_WyllersonEvaristo1983-_M.pdf: 20027750 bytes, checksum: ac9756c2723f3eb80a562d792355af61 (MD5) Previous issue date: 2010 / Resumo: As propriedades dinâmicas e estruturais de filmes de surfatantes adsorvidos em superfícies são de interesse fundamental e aplicado. Investigamos a formação de estruturas auto-organizadas de surfatantes sobre superfícies de substrato sólido de ouro. Estudamos sua dinâmica de formação e estabilidade. As estruturas foram feitas em ambiente aquoso, sob condições físico-químicas controladas. Tais estruturas são potenciais candidatas a modelos in vitro de membrana biológica (sistema biomimético) / Abstract: The structural and dynamical properties of surfactant films are both of fundamental and applied interest. To understand the formation mechanism of these structures we have studied the formation of surfactant self-assembled aggregates on gold surfaces. Their dynamic and stability were investigated. All experiments were performed in aqueous media, under specific physical and chemical conditions. These structures are potential candidates of in vitro models for biological membranes (bio-mimetic systems) / Mestrado / Físico-Química / Mestre em Física

O presente trabalho tem como objetivo principal a eletrofiação de nanofibras poliméricas de poliacrilonitrila (PAN) e polifluoreto de vinilideno (PVDF), incorporadas com negro de fumo (NF) e ftalocianina de cobre (CuPc), visando aplicações em dispositivos sensores. Inicialmente foram preparadas soluções de PAN puro a 6 % em peso e PVDF puro a 20% em peso e foram misturadas a essas soluções partículas de negro de fumo e ftalocianina de cobre, obtendo soluções de PAN/NF, PVDF/NF, PAN/CuPc e PVDF/CuPc. Foi determinada a viscosidade absoluta das soluções. Realizou-se a eletrofiação para obtenção de nanofibras que foram caracterizadas segundo o diâmetro e morfologia, usando microscópio óptico e microscópio eletrônico de varredura. Para avaliar as interações polímero-polímero, polímero-partícula foram analisadas por espectroscopia FITR e Raman. Com as fibras de PAN/NF foi analisada a resistência e condutância elétrica das membranas usando um picoamperímetro digital, visando aplicação como filtro eletrostático. Foi construído canal na lâmina de silício usando um feixe de laser visando a deposição de fibras dentro do canal usando a técnica de focagem eletrodinâmica com tensão aplicada em máscaras de cobre. Foi usada a técnica da microbalança de cristal de quartzo para determinar a variação de massa adsorvida por membranas de PAN/CuPc e PVDF/CuPc por meio da medida da variação de frequência usando um frequencímetro digital, onde se observou que essas membranas são promissoras para atuar como sensores de vapor de amônia. / The main objective of this work is the incorporation of different particles in order to electrospun polymeric nanofibers of polyacrylonitrile (PAN) and polyvinylidene fluoride (PVDF), aiming at applications in sensor devices. Initially, solutions of PAN pure 6 wt% and PVDF pure 20 wt% were prepared and these solutions were mixed with carbon black (NF) particles and copper phthalocyanine (CuPc), obtaining solutions of PAN/NF, PVDF/NF, PAN/CuPc and PVDF/CuPc. The absolute viscosity of the solutions was determined. The electrospinning was performed to obtain nanofibers that were characterized according to the diameter and morphology, using optical microscope and scanning electron microscopy. To evaluate the polymer-polymer and polymer-particle interactions, FITR and Raman spectroscopy were performed. The resistance and conductance of the membranes electrospun from PAN/NF solution were analyzed using a digital picoammeter, and an increase in the resistance was measured. This result shows that the membrane is suitable to be applied as electrostatic filter. A channel was constructed on the silicon wafer using a laser beam for the deposition of fibers inside the channel using the electrodynamic focusing technique. The quartz crystal microbalance technique was used to determine the applicability of the membranes as sensor layer. The results of PAN/CuPc and PVDF/CuPc membranes suggests that these membranes are promising to act such as ammonia vapor sensors.

Amostras com pequenos volumes e matrizes complexas, como sistemas biológicos, necessitam de preparação criteriosa. Muitas dessas amostras são melhor analizadas em estruturas miniaturizadas devido à necessidade de detectar células e microorganismos em diferentes matrizes. Por essa razão, equipamentos capazes de detectar e destruir microorganismos e estruturas para prévia retenção desses se faz necessários na vida moderna. Chicanas, constrições usadas para reduzir velocidade de fluxo, que podem ser utilizadas para reter compostos, são estruturas macroscópicas para remover resíduos de lagos, fazendas e etc. e chicanas miniaturizadas foram usadas para a adsorção de compostos orgânicos do ar e da água. Assim, esse trabalho tem dois diferentes objetivos: 1) Produção de um equipamento de baixo custo, para teste de partículas ou eliminação de microorganismos e 2) O desenvolvimento de estruturas miniaturizadas para retenção e/ou seleção de partículas e substâncias viscosas de um fluido líquido. A metodologia utilizada foi: 1) Dois software foram escolhidos para esse trabalho. O LabVIEW® 7.0 foi utilizado como plataforma para o desenvolvimento do software do equipamento e o FemLAB® 3.1 para a simulação de estruturas. O equipamento produzido usou Microbalança de Quartzo como detector e um sistema de admissão baseado em uma bomba e tubos. 2) O desenho da estrutura foi otimizado por simulação do comportamento do fluxo. A estrutura otimizada foi feita desmontável, e usinada em polimetilmetacrilato ? acrílico, com ferramentas convencionais. Acrílico foi usado devido à sua transparência óptica, que permite testes com microsocpia óptica. As simulações consideraram N2 e Água como fluidos gasoso e líquido, respectivamente. Avaliou-se o comportamento das partículas (50?m and 13?m) em fluxo gasoso e polidimetilsiloxano (silicone, com viscosidade de 350 cSt) e partículas em fluxo líquido. As estruturas foram caracterizadas quanto à adsorção e retenção de partículas usando equipamento desenvolvido e por microscopia óptica. As estruturas foram, também, continuamente fotografadas durante a execução do experimento e fotos foram utilizadas para determinar o comportamento do fluxo. Os reagentes foram injetados na estrutura em pequenos pulsos. O equipamento mostrou boa performance para detecção de adsorção em fluxo líquido e reprodutibilidade no monitoramento do aquecimento de estruturas. As chicanas mostraram boa capacidade de reter partículas grandes (50?m), mas não pequenas (13?m), tanto para fluxos gasosos como líquidos. Contudo, a estrutura tem pequena capacidade de carga para fluidos líquidos (? 1mg); além disso, a retenção de amostras de silicone na estrutura, utilizando fluido líquido, ocorreu devido à diferença de velocidade entre os fluidos. A simulação e os resultados experimentais apresentam boa correlação. Assim, a chicana mostrou a possibilidade de, seletivamente, separar partículas em fluxos gasosos e líquidos ou reter substâncias viscosas em fluxo líquido. Esses resultados apontam para diversas aplicações, como por exemplo, pré-tratamento para análises biológicas e retenção ou eliminação de microorganismos. / Samples with small volume and complex matrix, such as biological systems, require careful preparation. Many of these samples are better analyzed in miniaturized structures owing to the need of detect cells and microorganisms in different arrays. Therefore equipment able to detect and destroy microorganisms and structures to previously retain them are require in the modern life. Chicanes, i.e. constrictions used to reduce flow velocity, can be useful to retain compounds, are macroscopic devices to remove waste removal from lakes, farms, etc. and miniaturized chicane was used to adsorption of organic compounds from air and water. Thus, this work has two different targets: 1) Production of a low-cost equipment useful for tests of particle or microorganisms elimination and 2) The development of miniaturized structures useful for retention and/or selection of particles and viscous substances from a liquid flow. The methodology used was: 1) Two software were chosen to this work. The LabVIEW® 7.0 was used for development of equipment software and FemLAB® 3.1 for structures simulation. The equipment production used Quartz Crystal Microbalance as detector and an admission system based on simple pumps and plumbing. 2) The design of the structure design was optimized using flow simulation. The optimized design was manufactured in poly(methyl methacrylate) -acrylic, with conventional tools. Acrylic was used due to the optical transparency that allows photographic tests and the structures can be easily disassembled. The simulations considered nitrogen and water for gaseous and liquid flow, respectively. It was evaluated the behavior of particles (50?m and 13?m) on gaseous flow and polydimethylsiloxane (silicone, viscosity of 350 cSt) and particles on liquid flow. The structures were characterized using equipment produced to measure adsorption and optical microscopy to evaluate particle retention. The structures were also continuously photographed during the experiments and the photos were analyzed to determine flow behavior. The reactants were inserted in the structure in small pulses. The equipment shows good performance for detection of adsorption in liquid flows and reproducibility on monitoring heated structures. Chicanes showed good ability to retain big particles (50 ?m) but not small ones (13 ?m) for both liquid and gaseous flow. However, the structure has small load capacity for liquids (? 1 mg). Moreover, the retention of silicone samples in the structure on liquid flow occurs due to the difference in the fluid velocity. The simulation and experimental results are in good agreement and also chicane structure shows the possibility of selectively separate particles from gaseous and liquid flow or retain viscous substances from a liquid flow. These results point out to several applications, such as sample pretreatment for biological analysis and microorganism retention or elimination.

Accurate prediction of long-term moisture expansion in fired clay ceramics requires finding a relationship between the reactivity of a ceramic material with moisture and time. Recently a (time)1/4 law has been proposed which provides a precise relationship between moisture expansion and mass gain in fired clay ceramics and time. However, mass gain studies rather than expansive strain studies provide a more accurate and fundamental measure of the reactivity of fired clay ceramics with moisture. The possibility of using the (time)1/4 law to describe rate of mass gain and consequently to predict moisture expansion in fired clay ceramics with time requires study of the effect of chemical composition and firing temperature on the linear dependence of mass gain on (time)1/4. Pure kaolinite as well as kaolinite mixed with controlled additions of alkali and alkaline-earth metals were employed in this study. These materials were fired at temperatures between 800°C and 1200°C. Mass gain due to the chemical combination of the fired materials with moisture was measured using a recording microbalance under tightly controlled environmental conditions of temperature and relative humidity. The mass gain results show that the (time)1/4 law can be used to obtain an accurate linear relationship between long-term mass gain and time at almost all firing temperatures and at all different compositions. The presence of alkali metals was found to strongly affect the chemical combination of fired clay ceramics with moisture and hence affect the rate of mass gain. On the other hand, alkaline earth metals were found to produce similar reaction kinetics to kaolinite alone. BET surface area and X-ray diffraction results confirm that there is a correlation between the reactivity with moisture and both the specific surface area and crystallinity of fired clay ceramics.

The electrochemical quartz crystal microbalance (EQCM) has been proven an effective mean of monitoring up to nano-scale mass changes related to electrode potential variations at its surface. The principles of operation are based on the converse piezoelectric response of quartz crystals to mass variations on the crystal surface. In this work, principles and operations of the EQCM and piezo-electrodes are discussed. A conductive oxide, ruthenium oxide (RuO2) is a promising material to be used as a diffusion barrier for metal interconnects. Characterization of copper underpotential deposition (UPD) on ruthenium and RuO2 electrodes by means of electrochemical methods and other spectroscopic methods is presented. Copper electrodeposition in platinum and ruthenium substrates is investigated at pH values higher than zero. In pH=5 solutions, the rise in local pH caused by the reduction of oxygen leads to the formation of a precipitate, characterized as posnjakite or basic copper sulfate by means of X-ray electron spectroscopy and X-ray diffraction. The mechanism of formation is studied by means of the EQCM, presenting this technique as a powerful in-situ sensing device.