This thesis presents the results of an investigation of factors which influence the geotechnical properties of frozen mine backfill (FMB). FMB has extensive application potential for mining in permafrost areas. The uniaxial compressive strength (UCS) of hardened backfill is often used to evaluate mine backfill stability. However, the deformation behaviour and stiffness of the FMB are also key design properties of interest. In this thesis, uniaxial compressive tests were conducted on FTB and FCPB samples. Information about the geotechnical properties of FMB is obtained. The effects of FMB mix components and vertical compression pressure on the geotechnical properties of FMB are discussed and summarized. An optimum total water content of 25%-35% is found in which the strength and the modulus of elasticity of the FTB are 1.4-3.2 MPa and 35-58 MPa, respectively. It is observed that a small amount (3-6%) of cement can significantly change the geotechnical properties of FTB.

Neste trabalho foram estudadas as etapas de processo envolvidas na tecnologia Pin-in-Paste (PIP) de soldagem por refusão de componentes convencionais (THCs - Through Hole Components ou Componentes de Furo Passante) em placas de circuito impresso (PCIs), utilizando pasta de solda sem chumbo (lead-free) com liga SAC (Sn-Ag-Cu) de forma a atender as novas exigências ambientais para a montagem eletrônica. Inicialmente foi feito o projeto da PCI de teste com três diferentes componentes THCs e três componentes SMD com encapsulamentos distintos, com o objetivo de reproduzir uma PCI comercial. Foram gerados dois diâmetros de furos diferentes para inserir os THCs, possibilitando o estudo da variação de preenchimento com solda no PTH. Foi proposta uma equação para o cálculo do volume de pasta de solda a ser impresso sobre os furos no processo de montagem. A partir desta equação foram calculadas as dimensões dos furos do estêncil para a PCI de teste. Os parâmetros de impressão foram otimizados em função da variação de pressão e da velocidade do rodo. Duas curvas de refusão foram utilizadas, uma convencional e outra otimizada para verificar a variação na geração de defeitos. A impressão de pasta de solda ficou superior ao projetado, o que resultou em todas as amostras terem solda acima do parâmetro mínimo de aceitabilidade de volume de 75% de preenchimento do PTH. Esta sobre impressão ocasionou defeitos em boa parte dos componentes, excesso de solda nos filetes e resíduos de fluxo na solda nos PTHs. Tais defeitos foram expressivos para todos os THCs, mostrando que o excesso de pasta impressa foi decisivo na geração de defeitos para todas as combinações das variáveis estudadas. Os SMDs tiveram solda aceitável, apresentando apenas alguns casos de excesso de fluxo ou pouca solda em alguns QFPs devido ao uso de ilhas com dimensões maiores que o exigido em norma. O processo de Pin In Paste se mostra viável como substituto da solda onda em linhas de montagem para placas com SMDs e THCs, mas estudos posteriores deverão ser realizados para a geração de um modelo confiável de projeto de PCIs e estêncil com solda lead-free para que tal processo seja utilizado em grande escala na indústria. / This study describes the process steps involved in Pin-in-Paste (PIP) reflow soldering technology in printed circuit boards (PCBs) using lead-free solder paste with SAC alloy (Sn-Ag-Cu) in order to attend new environmental requirements for the electronics assembly. Initially it was designed a PCB test with three different THCs (Through Hole Component) and three different SMD (Surface Mount Device) packages in order to reproduce a commercial board. It was generated two different diameters of holes to insert the THCs, aiming to study the solder fill variation in PTH. An equation was proposed for calculating the volume of solder paste to be printed over the holes in the assembly process. From this equation it was calculated the dimensions of the holes of the stencil. The printing parameters were optimized according to the variation of pressure and speed of the squeegee. Two reflow curves were used in the process, a conventional one and an optimized one to determine the variations in the generation of soldering defects. The printed solder paste volume was higher than projected, which resulted in solder excess, causing defects in most of the components, such as excess solder in the fillet and solder flux residues in PTHs. Such defects were significant for all THCs, showing that the excess paste that was printed caused critical defects for all combinations of variables. Regarding that all samples were above the reflow minimum acceptable volume of 75% coverage of PTH. The SMDs solders were acceptable, with only few cases of solder flux excess. The Pin in Paste process was observed as a good option to replace the wave soldering thermal process for mixed PCBs. Further studies should be conducted to generate a reliable model of PCB and stencil design.

This thesis presents the results of an investigation of factors which influence the geotechnical properties of frozen mine backfill (FMB). FMB has extensive application potential for mining in permafrost areas. The uniaxial compressive strength (UCS) of hardened backfill is often used to evaluate mine backfill stability. However, the deformation behaviour and stiffness of the FMB are also key design properties of interest. In this thesis, uniaxial compressive tests were conducted on FTB and FCPB samples. Information about the geotechnical properties of FMB is obtained. The effects of FMB mix components and vertical compression pressure on the geotechnical properties of FMB are discussed and summarized. An optimum total water content of 25%-35% is found in which the strength and the modulus of elasticity of the FTB are 1.4-3.2 MPa and 35-58 MPa, respectively. It is observed that a small amount (3-6%) of cement can significantly change the geotechnical properties of FTB.

Objectives: To determine whether treatment of demineralized enamel white spot lesions with CPP-ACP paste, CPP-ACFP paste or microabrasion technique decreases lesion depth in vitro. Additionally, to determine whether treatment of demineralized enamel white spot lesions with microabrasion technique in combination with CPP-ACP paste or CPP-ACFP paste decreases lesion depth greater than any of the three techniques alone. Background: White spot lesions (WSLs) after the removal of orthodontic appliances remain a problem for clinicians and patients. Previous studies suggest that application of casein phosphopeptide amorphous calcium phosphate (CPP-ACP) and casein phosphopeptide amorphous calcium fluoride phosphate (CPP-ACFP) may promote enamel remineralization. Recently, microabrasion of enamel was proposed as another treatment modality of white spot lesions. A review of literature showed that there was no comprehensive in vitro study that combined microabrasion, casein phosphopeptide amorphous calcium phosphate and casein phosphopeptide amorphous calcium fluoride phosphate for treatment of WSLs. Methods: A total of one hundred and twelve bovine incisor teeth were randomly assigned to seven treatment groups: 1. Control 1 (demineralization control), 2. Control 2 (remineralization solution control), 3. CPP-ACP paste, 4. CPP-ACFP paste, 5. Microabrasion, 6. Microabrasion with CPP- ACP paste, and 7. Microabrasion with CPP-ACFP paste. Teeth in all groups were placed in demineralizing solution for 96 hours to produce artificial caries-like lesions. At the end of the 96 hr period, teeth in Control 1 group were sectioned to establish adequate amount of demineralization. The rest of samples were treated with assigned regimen once a day for 10 days and stored in remineralization solution. At the end of ten days, teeth were sectioned with a hard tissue microtome and observed under polarized microscopy to analyze enamel lesion depth. One-way ANOVA at α=0.05 was performed to assess difference in lesion depth between groups followed with post hoc Tukey's test. Results: Statistical analysis showed a significant difference between groups (pConclusions: Based on the results from this study, we can conclude that: (1) treatment of WSLs with CPP-ACP paste, CPP-ACFP paste or microabrasion decreases lesion depth in vitro; (2) microabrasion in combination with CPP-ACP paste or CPP-ACFP paste did not decrease lesion depth greater than that observed with either paste technique alone; (3) both CPP-ACP and CPP-ACFP pastes in combination with microabrasion treatments showed greater decrease in lesion depth than microabrasion alone.

<p>Superabsorbent polymer (SAP) hydrogel particles have been used as internal curing agents in concrete mixes as they are capable of absorbing and subsequently releasing large amounts of water. This reduces autogenous shrinkage during early stages of hydration. The size, shape, and composition of the hydrogel particles can be controlled during the synthesis, hence providing the opportunity to custom synthesize these internal curing agents to elicit desired structure-property relationships. Utilization of optimized dosage and formulation of SAP has the potential to improve the microstructure, durability, and strength of internally cured concrete. </p> <p>The first study focuses on the synthesis and application of novel composite hydrogel particles as internal curing agents in cementitious mixes. Composite polyacrylamide hydrogel particles containing two different amorphous silica–either nanosilica or silica fume–were used to investigate whether the internal curing performance of hydrogel particles could be enhanced. The dosage and type of silica, crosslinker amount were varied to identify the composite polyacrylamide hydrogel particle composition that provides optimum benefits to internally cured cementitious systems. The synthesized hydrogels were characterized by means of absorption capacity tests, compositional and size analysis. The beneficial impacts of the addition of composite hydrogels on cement paste microstructure are highlighted, including the preferential formation of cement hydration products (such as portlandite) within the hydrogel-induced voids that appeared to be influenced by the composition of the hydrogel particles. The interrelationship between extent of hydration, size of hydrogel voids, and void-filling with hydration products was found to strongly influence mechanical strength and is thus an important structure-property relationship to consider when selecting hydrogels for internal curing purposes. This study informs the design of composite hydrogel particles to optimize performance in cementitious mixes. Additionally, it provides a novel means of incorporating other commonly used admixtures in concrete without facing common challenges related to dispersion and health hazards.</p> <p>The second study focuses on the utilization of two retarding admixture-citric acid and sucrose-to custom synthesize composite polyacrylamides to investigate whether the composite hydrogels could delay hydration of cement paste. Isothermal calorimetry analysis results showed that composite sucrose-containing polyacrylamide hydrogel particles were successfully able to retard main hydration peak of cement paste, beyond the retardation capabilities of the pure polyacrylamide hydrogels. Thus, this study provides avenues of exploring the utilization of common admixtures to formulate novel composite hydrogels that imparts specific properties to cementitious systems.</p> <p>In another study, SAP formulated by admixture industries were used to investigate the feasibility of internal curing of bridge decks and pavement patches with SAP particles. The microstructure and early age hydration properties of SAP-cured cementitious systems were studied. Mitigation of microcracks in the matrix, along with portlandite growth in SAP voids, were observed in SAP-cured mortars. Presence of SAP also mitigated autogenous shrinkage and improved early age hydration as observed by isothermal calorimetry analysis. This thesis highlights some of the beneficial impacts of SAP-cured cementitious systems, and the potential to harness those benefits in large-scale applications of SAP-cured concrete.</p> <br>

This study determined if any of six endodontic solutions would have a softening effect on resorcinol-formalin paste in extracted teeth, and if there were any differences in the solvent action between these solutions. Forty-nine single-rooted extracted teeth were decoronated two mm coronal to the CEJ, and the roots sectioned apically to a standard length of 15 mm. Canals were prepared to a 12mm WL and a uniform size with a #7 Parapost drill. Teeth were then mounted in a cylinder ring with acrylic. The resorcinol-formalin mixture was placed into the canals and was allowed to set for 60 days in a humidor. The solutions tested were 0.9% sodium chloride, 5.25% sodium hypochlorite, chloroform, Endosolv R®, 3% hydrogen peroxide, and 70% isopropyl alcohol. Seven samples per solution were tested and seven samples using water served as controls. One drop of the solution was placed over the set mixture in the canal, and the depth of penetration of a 1.5 mm probe was measured at 2, 5, 10, and 20 min using a dial micrometer gauge. A repeated-measures ANOVA showed a difference in penetration between the solutions at 10 min (p=0.04) and at 20 min (p=0.0004). At 20 min, Endosolv R®, had significantly greater penetration than 5.25% sodium hypochlorite (p=0.0033) and chloroform (p=0.0018); however, it was not significantly better than the control (p=0.0812). Although Endosolv R®, had statistically superior probe penetration at 20 min, the softening effect could not be detected clinically at this time.

Propyl gallate (PG) is a significant synthetic antioxidant and preservative. Its determination has been studied at carbon paste electrode (CPE) using differential pulse voltammetry (DPV) and high performance liquid chromatography with electrochemical detection (HPLC-ED) and with UV spectrometric detection (HPLC-UV). Concentration dependences were measured in the media of Britton-Robinson buffer (pH 5) and methanol (20 %, v/v) by DPV and the limit of detection 0,6110-7 moldm-3 was obtained. Using HPLC with a mobile phase consisting of 0,01 moldm-3 phosphate buffer (pH 4) and methanol (50 %, v/v) with potential of working electrode E = +0,8 V and detection wavelength λ = 280 nm, concentration dependences were measured. Limit of detection was determined to 0,39 moldm-3 for HPLC-ED and 4,95 moldm-3 for HPLC-UV. After verification of the extraction procedure PG was determined in vegetable oil. The resulting value of 3,2 mgkg-1 corresponds with permited limits.

Les superplastifiants sont des adjuvants développés pour conférer aux matériaux cimentaires une plus grande fluidité pour un même rapport eau/ciment (E/C) en favorisant la dispersion des particules. De nombreuses études ont été réalisées pour approfondir la compréhension de leur mode d'action. La plupart du temps, elles relient directement la quantité adsorbée au comportement rhéologique des matériaux dans lesquels ils sont incorporés. Cependant, à une échelle intermédiaire, l'organisation mésostructurale de la pâte cimentaire contrôle non seulement sa fluidité, mais également son homogénéité et sa stabilité physicochimique.Ces travaux de thèse portent sur une dernière génération de superplastifiant : les polycarboxylates (PCE). Une approche expérimentale multi-échelles a été développée en intégrant les caractéristiques mésostructurales de la pâte de façon à faire le lien entre les interactions organo-minérales, notamment l'adsorption des PCE, et les propriétés macroscopiques (comportements en sédimentation et rhéologique). L'identification et la caractérisation granulaire de la pâte a été abordée à l'échelle de la particule, par une approche morpho-granulométrique. Des indices de dispersion ont été définis de façon à quantifier l'influence des PCE sur l'organisation mésostructurale des particules (particules unitaires ou agglomérées). Dans un second temps, l'évolution de cette organisation a été étudiée par l'analyse des colonnes de sédimentation. Un indice de séparation de phase a été défini, mettant en évidence l'existence de plages de stabilité en fonction du dosage et de la structure moléculaire du PCE incorporé.La mise en relation de ces observations avec l'étude des interactions organo-minérales a permis d'approfondir la compréhension du mode d'action et de l'influence des PCE. Cette démarche analytique représente un outil potentiel au développement de superplastifiants novateurs. / Superplasticizers are admixtures developed to give the cementitious materials greater fluidity for the same water to cement ratio (w/c), promoting the particles dispersion. Many studies were conducted to deepen the understanding of their mode of action. Usually, they connect directly the amount adsorbed with the rheological behavior of the materials in which they are incorporated. However, at an intermediate scale, mesostructurale organization of the cement paste controls not only its fluidity, but also its homogeneity and physicochemical stability.This work focuses on a new generation of superplasticizers: polycarboxylates (PCE). A multi-scale experimental approach has been developed by integrating mesostructural characteristics of cement paste to make the link between the organo-mineral interactions, particularly PCE adsorption, and the macroscopic properties (sedimentation and rheological behavior). Identification and granular characterization of cement paste was discussed, at the level of the particle, by a morpho-granulometric approach. Dispersion indices were defined to quantify the influence of PCE on mesostructural organization of particles (unit particles or agglomerates). In a second step, the evolution of this organization has been studied by analysis of sedimentation columns. A phase separation index has been defined, highlighting the existence of stability ranges as a function of the dosage and molecular structure of the PCE incorporated.Linking these observations with study of organo-mineral interactions has allowed to deepen the understanding of the mode of action and influence of PCE. This analytical approach is a potential tool to the development of innovative superplasticizers.

As argamassas de revestimento são amplamente utilizadas na construção civil e, suas propriedades no estado endurecido são fortemente influenciadas pelas propriedades no estado fresco, as quais dependem de fatores como: materiais empregados; forma de aplicação; e interação entre substrato e argamassa. Os ensaios utilizados para caracterização reológica das argamassas não contemplam as alterações que ocorrem devido o contato com o substrato, gerando discordâncias nas teorias sobre os fenômenos pelo qual ocorre a resistência de aderência. Sendo assim, o presente trabalho visa identificar as alterações do comportamento reológico de suspensões cimentícias aplicadas em substratos porosos por meio do ajuste do método do squeeze-flow. Para tanto, foram utilizadas duas configurações do squeeze-flow, com e sem confinamento do fluxo radial; três tipos de base, sendo uma metálica e duas porosas; e, pastas com diferentes materiais, a saber: cimento; cal e filler calcário. A escolha da pasta ao invés da argamassa foi basicamente por duas razões: primeiro, porque a pasta é a parcela da argamassa mais suscetível aos efeitos de sucção capilar do substrato; e segundo, para simplificar o cenário de análise, eliminando a variável areia. Ambas as configurações apresentaram-se viáveis na identificação da alteração do comportamento reológico da pasta, devido aos fatores como: tipo de substrato; o tempo de contato entre pasta e substrato; perda de água da pasta; e energia de mistura. Além disso, observou-se que os procedimentos adotados, assim como o auxílio de outros ensaios, podem colaborar em estudos da influência de fatores como: temperatura; rugosidade; ângulo de contato; distribuição granulométrica de pastas e argamassas; e, principalmente, compreender os fenômenos que ocorre no período denominado como tempo de puxamento, ao passo que este influencia diretamente na resistência de aderência. / Mortar renderings are used in most of the constructions and their properties in the hardened state are strongly influenced by the properties in the fresh state, which depend on factors such as materials used; application form; and interaction between substrate and mortar. The determination of rheological parameters of fresh mortars doesn\'t include the changes that occur due to contact with the substrate. It generates disagreements in the theories about the phenomena of formation of the bond strength. Therefore, this study aims to identify changes in the rheological behavior of cementitious paste applied to porous substrates by adjusting the squeeze flow method. For this, two configurations of squeeze flow were used, with and without confinement of the radial flow; three substrate types; and pastes with different materials, namely cement, lime and sand. The choice of paste instead of mortar was basically for two reasons: first, because the paste is the portion of mortar more susceptible to the effects of capillary suction of substrate; and second, to simplify scenario analysis, eliminating the variable sand. Both configurations were viable in the identification of the alteration of rheological behavior of paste, due to factors such as substrate type; the contact time between paste and substrate; loss of water from paste; and mixing energy. In addition, it was observed that the procedures adopted as well as the aid of the other tests can collaborate on studies of the influence of factors such as temperature, roughness, contact angle, particle size distribution of pastes and mortars; and above all to understand the phenomena that occurs in the initial periods of contact paste/substrate and consequently in the bond strength.

The fundamental requirement of the research reported within this thesis is the provision of physical models to enable model based simulation of mainstream printed circuit assembly (PCA) process discrete events for use within to-be-developed (or under development) software tools which codify cause & effects knowledge for use in product and process design optimisation. To support a national competitive advantage in high reliability electronics UK based producers of aircraft electronic subsystems require advanced simulation tools which offer model based guidance. In turn, maximization of manufacturability and minimization of uncontrolled rework must therefore enhance inservice sustainability for 'power-by-the-hour' commercial aircraft operation business models.