Hollow glass microspheres have been used extensively in the automotive and marine industries as an additive for reducing weight and saving material costs. They are also added to paints and other materials for their reflective properties. They have shown promise for weight critical applications, but have thus far resulted in materials with low fracture toughness and impact resistance when combined with thermosetting resins in syntactic foam. The advent of commercially available microspheres with a wide range of crushing strengths, densities and adhesive properties has given new impetus to research into syntactic foam with better fracture behaviour. Current research suggests that the beneficial effects on fracture and impact resistance gained by the addition of solid reinforcements such as rubber and ceramic particles are not seen with the addition of hollow glass microspheres. The research presented in this paper has examined the mechanisms for fracture resistance in glass microsphere filled epoxy (GMFE) syntactic foams, as well as determined the effect microsphere crushing strength and adhesion strength has on the material???s fracture toughness. The flexural properties of various GMFE have also been determined. GMFE were manufactured with varying microsphere volume fraction up to 50%, and with variances in microsphere crushing strength and adhesion. The specimens were tested for Mode I fracture toughness in a three point single edge notched bending setup as described in ASTM D5045 as well as a three point flexural setup as described in ASTM D790-3. Fracture surfaces were inspected using scanning electron microscope imaging to identify the fracture mechanisms in the presence of microspheres. Results indicate a positive effect on fracture toughness resulting from new fracture areas created as tails in the wake of the microspheres in the fracture plane. Results also indicate a negative effect on fracture toughness resulting from weak microspheres or from interfacial disbonding at the fracture plane. These two effects combine to show an increase in GMFE fracture toughness as the volume fraction of microspheres is increased to between 10 ??? 20% volume fraction (where the positive effect dominates), with a reduction in fracture toughness as microspheres are added further (where the negative effect dominates).

Hollow glass microspheres have been used extensively in the automotive and marine industries as an additive for reducing weight and saving material costs. They are also added to paints and other materials for their reflective properties. They have shown promise for weight critical applications, but have thus far resulted in materials with low fracture toughness and impact resistance when combined with thermosetting resins in syntactic foam. The advent of commercially available microspheres with a wide range of crushing strengths, densities and adhesive properties has given new impetus to research into syntactic foam with better fracture behaviour. Current research suggests that the beneficial effects on fracture and impact resistance gained by the addition of solid reinforcements such as rubber and ceramic particles are not seen with the addition of hollow glass microspheres. The research presented in this paper has examined the mechanisms for fracture resistance in glass microsphere filled epoxy (GMFE) syntactic foams, as well as determined the effect microsphere crushing strength and adhesion strength has on the material???s fracture toughness. The flexural properties of various GMFE have also been determined. GMFE were manufactured with varying microsphere volume fraction up to 50%, and with variances in microsphere crushing strength and adhesion. The specimens were tested for Mode I fracture toughness in a three point single edge notched bending setup as described in ASTM D5045 as well as a three point flexural setup as described in ASTM D790-3. Fracture surfaces were inspected using scanning electron microscope imaging to identify the fracture mechanisms in the presence of microspheres. Results indicate a positive effect on fracture toughness resulting from new fracture areas created as tails in the wake of the microspheres in the fracture plane. Results also indicate a negative effect on fracture toughness resulting from weak microspheres or from interfacial disbonding at the fracture plane. These two effects combine to show an increase in GMFE fracture toughness as the volume fraction of microspheres is increased to between 10 ??? 20% volume fraction (where the positive effect dominates), with a reduction in fracture toughness as microspheres are added further (where the negative effect dominates).

Made available in DSpace on 2016-03-15T19:36:43Z (GMT). No. of bitstreams: 1 Cindy Yuri Ueki Peres.pdf: 14079358 bytes, checksum: e18673ab8406f72692d9a0a35b414328 (MD5) Previous issue date: 2014-06-09 / Fundo Mackenzie de Pesquisa / This work aims to evaluate the concrete with addition of hollow glass microspheres . The specific objectives of this work is to evaluate the influence of the addition of hollow glass microspheres with different combinations of dosage in concrete concerning resistance and workability. It was proved that in other studies glass microspheres may influence the workability of the concrete , because due to its geometry, the balls can roll on each other and on the other solid components of the concrete. In view of the foregoing, it becomes important to study the effect of varying the dosage of these glass microspheres in the concrete properties, such as fluidity, strength and compactn ess. Tests are carried out Workability Slump in each dosage of concrete , and in every age of curing of concrete , the bodies of the test piece was be submitted to ultrasound and axial strength test . we used the Weibull to compare the results. With the results obtained in the tests, the comparative analysis of the variation of each factor chosen were performed. The analysis of the results shows that for some formulations, the addition of hollow glass microspheres imparts high mechanical strength to compressive strength above 30MPa at all periods analyzed. Importantly, the workability of the concrete had to be substantially reduced, showing no improvement in workability due to the addition of hollow glass microsphere / Este trabalho tem como objetivo avaliar o concreto com adição de microesferas ocas de vidro. O objetivo específico deste trabalho é avaliar a influencia da adição de microesferas ocas de vidro com diferentes combinações de dosagem no concreto, em relação à resistência e à trabalhabilidade. Foi provado em outros trabalhos que as microesferas de vidro podem influenciar na trabalhabilidade do concreto, pois, devido a sua geometria, as esferas podem rolar umas sobre as outras e sobre os demais componentes sólidos do concreto. Em virtude do exposto, torna-se importante estudar a influência da variação da dosagem dessas microesferas de vidro nas propriedades do concreto, como fluidez , resistência e compacidade. Foram realizados ensaios de trabalhabilidade ou Slump em cada dosagem de concreto, e em cada idade de cura do concreto, os corpos-de-prova foram submetidos ao ultrassom e ao ensaio de resistência axial, utilizou-se o método de Weibull para comparar os resultados de resistência a compressão. Com os resultados obtidos nos ensaios, foram realizadas as análises comparativas da influência da variação de cada fator escolhido. A análise dos resultados obtidos mostra que para algumas formulações, a adição das microesferas ocas de vidro confere alta resistência mecânica de compressão do concreto, acima de 30MPa, em todos os períodos de cura analisados. Importante destacar qu e a trabalhabilidade do concreto apresentou-se substancialmente reduzida, não apresentando qualquer melhora de trabalhabilidade devido à adição da microesfera oca de vidro.

The curing characteristics of photopolymer resin determine the relationship between the vat polymerization (VP) process parameters and the layer thickness, geometric accuracy, and surface quality of the 3D printed specimen. Dispersing filler material into the photopolymer resin changes its curing characteristics because the filler scatters and absorbs light, which modifies the curing reaction. However, the ability to cure photopolymer resin with high filler volume fraction is important to 3D print material specimens for specific engineering applications, e.g. structural polymer composite materials, electrical and thermal conductive materials, and ceramic materials for biological and high-temperature environments. We methodically measure the curing characteristics of diacrylate/epoxy photopolymer resin with dispersed glass microspheres. The experiments show that the curing depth, degree-of-cure, and surface roughness depend on both the light exposure dose and the filler fraction. We determine that the degree-of-cure increases with increasing filler fraction for constant exposure dose, and approaches 90% with increasing exposure dose, independent of the filler fraction. The geometric accuracy of the 3D printed specimens decreases with increasing exposure dose and with increasing filler volume fraction due to so-called profile broadening. Finally, we show that the average surface roughness of the 3D printed specimens decreases with increasing exposure dose and filler fraction. This work has implications for VP of photopolymer resins with high filler fraction. / Master of Science / Photopolymer resin is a gel-like liquid material that hardens (cures) into solid after absorbing light energy, and such a material is often used in the field of additive manufacturing (3D printing) to create complex geometry. Certain types of filler materials, such as metal powder or carbon fiber, can be added into the photopolymer resin to tailor the material properties, and thus, affects the curing behavior of photopolymer resin mixed with these filler materials. We conducted an experiment to understand how adding glass microspheres to a consumer grade photopolymer resin affects the process of creating 3D objects. This is important in the context of 3D printing engineered composite materials that derive their function from the organization and orientation of filler material in a matrix. To do this, we created many samples in the shape of a "VT" logo using the composite resin we made and measured their thickness (curing depth), degree-of-cure, surface roughness, and geometric accuracy, as a function of the amount of light energy being exposed to the resin (exposure dose) and the amount of the glass filler being added into the resin (filler fraction). We observed that when we increased the amount of light exposure, it resulted specimens that are thicker and more in degree of cure. Adding the glass filler to the liquid had mixed effects on the hardening process, because glass can scatter light and change how light travels within the resin. As a result, the printed objects became less accurate in shape and have smoother surface with increasing exposure dose and filler fraction, because more light is scattered off the designed curing profile and unintentionally cured the surrounding resin.

[pt] Esta pesquisa teve como principal objetivo contribuir para a avaliação da influência da forma dos grãos na condutividade hidráulica (k) de areias. Para tanto, ensaios de laboratório foram realizados em uma amostra da areia da Praia de Ipanema (D10 = 0,28 mm, D30 = 0,34 mm, D50 = 0,41 mm, D60 = 0,45 mm, CNU = 1,61 e CC = 0,92), constituída por grãos subarredondados a arredondados (esfericidade = 0,65 e arredondamento = 0,70), e em uma amostra de microesferas de vidro, tipo Drop-On II A (esfericidade = 0,95 e arredondamento = 0,95), preparada com granulometria igual à da areia. O programa experimental envolveu: (a) limpeza e tratamento das amostras; (b) análises microscópicas para avaliação da forma dos grãos; (c) ensaios de granulometria por peneiramento; (d) reconstituição granulométrica da amostra de microesferas de vidro; (e) densidade relativa (Gs) das microesferas de vidro; (f) ensaios de índices de vazios máximo, pelo método B da ABNT (2020), e ensaios de índices de vazios mínimo e intermediários, pela método MSP de Miura e Toki (1982); e (g) ensaios de permeabilidade sob carga hidráulica constante em permeâmetro de parede rígida e em permeâmetro de parede flexível. Para ambas as amostras, verificou-se experimentalmente a validade da relação linear entre a condutividade hidráulica (k) e e(3)/(1+e), sendo e o índice de vazios, em consonância com as formulações teóricas propostas por Kozeny-Carman (1927) e por Taylor (1948). Para um dado índice de vazios, constatou-se que a condutividade hidráulica da amostra de microesferas de vidro é maior do que a da amostra da areia da Praia de Ipanema. / [en] The main objective of this research was to contribute to the evaluation of the influence of the grain shape on the hydraulic conductivity (k) of sands. For that, laboratory tests were carried out on a sample from Ipanema Beach sand (D10 = 0.28 mm, D30 = 0.34 mm, D50 = 0.41 mm, D60 = 0.45 mm, CNU = 1.61 e CC = 0.92), composed by sub-rounded to rounded grains (sphericity = 0.65 and roundness = 0.70), and on a sample of glass microspheres, Drop-On II A type (sphericity = 0.95 and roundness = 0.95), prepared with the same grain size distribution of the sand. The experimental program comprised: (a) cleaning and processing of the samples; (b) microscopic analysis to evaluate the grain shape; (c) grain-size analysis by sieving; (d) reconstitution of the grain-size distribution of the glass microspheres sample; (e) glass microspheres specific gravity (Gs); (f) maximum void ratio tests, by method B of ABNT (2020), and minimum and intermediate void ratio tests, by MSP method of Miura and Toki (1982); and (g) constant head permeability tests in rigid-wall permeameter and in flexible-wall permeameter. For both samples, it was experimentally verified the validity of the linear relationship between the hydraulic conductivity (k) and e (3)/(1+e), being e the void ratio, in agreement with the theoretical formulations proposed by Kozeny-Carman (1927) and by Taylor (1948). For a given void ratio, it was observed that the hydraulic conductivity of the glass microsphere sample is higher than that of the sample from Ipanema Beach sand.

For many metal components the presence of hard, non-metallic inclusions such as oxides lowers the impact toughness by acting as fracture initiation points and easing crack propagation. In components produced by powder metallurgy hot isostatic pressing (PM HIP), oxides often form a continuous network of small, spherical inclusions after consolidation at the prior particle boundaries (PPB). It is therefore of great importance to reduce surface oxides before consolidation in order to improve mechanical properties. In this work, oxides were attempted to be reduced directly prior to the consolidation of one tool steel and one low-alloy steel by introducing H2 into sealed PM HIP capsules. The two H2-carriers were hollow glass microspheres and the compound ammonia borane (H3NBH3). The H2-carriers were placed separately from the metal powder. Microspheres were filled at 300 °C with a gas mixture at 675 bar resulting in a storage capacity of 0.16 wt%. Gaseous species released from the H2-carriers during heating were analysed by mass spectrometry. Results showed that the microspheres only release H2 while ammonia borane in addition releases other nitrogen and boron containing species. Impact testing as well as chemical and microstructural analysis were performed on the two consolidated materials with samples retrieved from different vertical and radial positions. Both H2-carriers had leaked into the material resulting in decreased impact toughness compared to the reference. Further from the source of the contaminants, oxygen content was reduced and impact toughness was improved. Microspheres showed overall better reduction ability even though they release less hydrogen compared to ammonia borane. Impact toughness was not improved as much with ammonia borane even though similar oxygen levels were achieved. Ammonia borane’s decomposition products likely obstruct the oxide reduction or introduce new inclusions lowering the impact toughness. / Det är för många metallkomponenter viktigt att så mycket som möjligt undvika hårda, icke metalliska inneslutningar. Detta eftersom de sänker slagsegheten genom sprickinitiering men även genom att underlätta spricktillväxt. Ytoxider i komponenter tillverkade genom pulvermetallurgisk het-isostatisk pressning (PM HIP) bildar ofta ett kontinuerligt nätverk av små, sfäriska inneslutningar efter konsolidering vid de tidigare partikelgränserna. Det är därför viktigt att reducera ytoxider före konsolidering för att förbättra de mekaniska egenskaperna av komponenter tillverkade genom PM HIP. I detta examensarbete har ytoxider reduceras direkt före konsolidering av ett låglegerat stål och ett verktygsstål genom att tillsätta H2 i de förseglade PM HIP kapslarna. Två vätgasbärare testades, ihåliga mikrosfärer av glas och ammoniak boran (H3NBH3). Vätgasbärarna var placerade i ett område avskilt från metallpulvret. Mikrosfärerna fylldes med en gasblandning vid 675 bar och 300 °C vilket resulterade i en lagringskapacitet på 0.16 vikt%. Gaser som frigjordes från vätgasbärarna vid uppvärmning analyserades med en masspektrometer. Resultatet visade att mikrosfärerna bara frigör H2 medan ammoniak boran också frigör andra ämnen innehållande kväve och bor. Slagprovning och analys av mikrostruktur samt syre- och kvävehalter utfördes på de två konsoliderade materialen med prover från olika vertikala och radiella positioner. Båda vätgasbärarna hade läckt in i materialet vilket resulterade i minskad slagseghet jämfört med referensmaterialet. Längre från vätgasbärarnas ursprungsposition var slagsegheten bättre och syrehalten lägre. De vätgasfyllda mikrosfärerna uppvisade överlag bättre förmåga att minska syrehalten trots att de innehöll mindre H2 jämfört med ammoniak boran. Slagsegheten förbättrades inte lika mycket med ammoniak boran trots att liknade syrenivåer uppmättes. Ammoniak boranets pyrolysprodukter förhindrar möjligtvis oxidreduktionen eller introducerar nya inneslutningar som resulterar i en försämrad slagseghet.