Strength prediction and experimental validation of adhesive joints including polyethylene, carbon-epoxy and aluminium adherends

Polyolefins are especially difficult to bond due to their non-polar, non-porous and chemically inert surfaces. Acrylic adhesives used in industry are particularly suited to bond these materials, including many grades of polypropylene (PP) and polyethylene (PE), without special surface preparation. In this work, the tensile strength of single-lap PE and mixed joints bonded with an acrylic adhesive was investigated. The mixed joints included PE with aluminium (AL) or carbon fibre reinforced plastic (CFRP) substrates. The PE substrates were only cleaned with isopropanol, which assured cohesive failures. For the PE CFRP joints, three different surfaces preparations were employed for the CFRP substrates: cleaning with acetone, abrasion with 100 grit sand paper and peel-ply finishing. In the PE AL joints, the AL bonding surfaces were prepared by the following methods: cleaning with acetone, abrasion with 180 and 320 grit sand papers, grit blasting and chemical etching with chromic acid. After abrasion of the CFRP and AL substrates, the surfaces were always cleaned with acetone. The tensile strengths were compared with numerical results from ABAQUS® and a mixed mode (I+II) cohesive damage model. A good agreement was found between the experimental and numerical results, except for the PE AL joints, since the AL surface treatments were not found to be effective.

Shear modulus and strength of an acrylic adhesive by the notched plate shear method (Arcan) and the thick adherend shear test (TAST)

In this work, the shear modulus and strength of the acrylic adhesive 3M® DP 8005 was evaluated by two different methods: the Thick Adherend Shear Test (TAST) and the Notched Plate Shear Method (Arcan). However, TAST standards advise the use of a special extensometer attached to the specimen, which requires a very experienced technician. In the present study, the adhesive shear displacement for the TAST was measured using an optical technique, and also with a conventional inductive extensometer of 25 mm used for tensile tests. This allowed for an assessment of suitability of using a conventional extensometer to measure this parameter. Since the results obtained by the two techniques are identical, it can be concluded that using a conventional extensometer is a valid option to obtain the shear modulus for the particular adhesive used. In the Arcan tests, the adhesive shear displacement was only measured using the optical technique. This work also aimed the comparison of shear modulus and strength obtained by the TAST and Arcan test methods.

Interlaminar fracture characterization of a carbon-epoxy composite in pure mode II

The interlaminar fracture toughness in pure mode II (GIIc) of a Carbon-Fibre Reinforced Plastic (CFRP) composite is characterized experimentally and numerically in this work, using the End-Notched Flexure (ENF) fracture characterization test. The value of GIIc was extracted by a new data reduction scheme avoiding the crack length measurement, named Compliance-Based Beam Method (CBBM). This method eliminates the crack measurement errors, which can be non-negligible, and reflect on the accuracy of the fracture energy calculations. Moreover, it accounts for the Fracture Process Zone (FPZ) effects. A numerical study using the Finite Element Method (FEM) and a triangular cohesive damage model, implemented within interface finite elements and based on the indirect use of Fracture Mechanics, was performed to evaluate the suitability of the CBBM to obtain GIIc. This was performed comparing the input values of GIIc in the numerical models with the ones resulting from the application of the CBBM to the numerical load-displacement (P-) curve. In this numerical study, the Compliance Calibration Method (CCM) was also used to extract GIIc, for comparison purposes.

Synthesis of titanate nanostructures using amorphous precursor material and their adsorption/photocatalytic properties

This article reports on a new and swift hydrothermal chemical route to prepare titanate nanostructures (TNS) avoiding the use of crystalline TiO2 as starting material. The synthesis approach uses a commercial solution of TiCl3 as titanium source to prepare an amorphous precursor, circumventing the use of hazardous chemical compounds. The influence of the reaction temperature and dwell autoclave time on the structure and morphology of the synthesised materials was studied. Homogeneous titanate nanotubes with a high length/diameter aspect ratio were synthesised at 160 degrees C and 24 h. A band gap of 3.06 +/- 0.03 eV was determined for the TNS samples prepared in these experimental conditions. This value is red shifted by 0.14 eV compared to the band gap value usually reported for the TiO2 anatase. Moreover, such samples show better adsorption capacity and photocatalytic performance on the dye rhodamine 6G (R6G) photodegradation process than TiO2 nanoparticles. A 98% reduction of the R6G concentration was achieved after 45 min of irradiation of a 10 ppm dye aqueous solution and 1 g L-1 of TNS catalyst.

Evaluation of tools and cutting conditions on carbon fibre reinforced laminates

The distinctive characteristics of carbon fibre reinforced plastics, like low weight or high specific strength, had broadened their use to new fields. Due to the need of assembly to structures, machining operations like drilling are frequent. In result of composites inhomogeneity, this operation can lead to different damages that reduce mechanical strength of the parts in the connection area. From these damages, delamination is the most severe. A proper choice of tool and cutting parameters can reduce delamination substantially. In this work the results obtained with five different tool geometries are compared. Conclusions show that the choice of an adequate drill can reduce thrust forces, thus delamination damage.

Biofunctional composite coating architectures based on polycaprolactone and nanohydroxyapatite for controlled corrosion activity and enhanced biocompatibility of magnesium AZ31 alloy

In this work a biofunctional composite coating architecture for controlled corrosion activity and enhanced cellular adhesion of AZ31 Mg alloys is proposed. The composite coating consists of a polycaprolactone (PCL) matrix modified with nanohydroxyapatite (HA) applied over a nanometric layer of polyetherimide (PEI). The protective properties of the coating were studied by electrochemical impedance spectroscopy (EIS), a non-disturbing technique, and the coating morphology was investigated by field emission scanning electron microscopy (FE-SEM). The results show that the composite coating protects the AZ31 substrate. The barrier properties of the coating can be optimized by changing the PCL concentration. The presence of nanohydroxyapatite particles influences the coating morphology and decreases the corrosion resistance. The biocompatibility was assessed by studying the response of osteoblastic cells on coated samples through resazurin assay, confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). The results show that the polycaprolactone to hydroxyapatite ratio affects the cell behavior and that the presence of hydroxyapatite induces high osteoblastic differentiation. (C) 2014 Elsevier B.V. All rights reserved.

Aquisição por Visão Artificial e Medição Automática de Micro Dureza Vickers

O ensaio de dureza, e mais concretamente o ensaio de micro dureza Vickers, é no universo dos ensaios mecânicos um dos mais utilizados quer seja na indústria, no ensino ou na investigação e desenvolvimento de produto no âmbito das ciências dos materiais. Na grande maioria dos casos, a utilização deste ensaio tem como principal aplicação a caracterização ou controlo da qualidade de fabrico de materiais metálicos. Sendo um ensaio de relativa simplicidade de execução, rapidez e com resultados comparáveis e relacionáveis a outras grandezas físicas das propriedades dos materiais. Contudo, e tratando-se de um método de ensaio cuja intervenção humana é importante, na medição da indentação gerada por penetração mecânica através de um sistema ótico, não deixa de exibir algumas debilidades que daí advêm, como sendo o treino dos técnicos e respetivas acuidades visuais, fenómenos de fadiga visual que afetam os resultados ao longo de um turno de trabalho; ora estes fenómenos afetam a repetibilidade e reprodutibilidade dos resultados obtidos no ensaio. O CINFU possui um micro durómetro Vickers, cuja realização dos ensaios depende de um técnico treinado para a execução do mesmo, apresentando todas as debilidades já mencionadas e que o tornou elegível para o estudo e aplicação de uma solução alternativa. Assim, esta dissertação apresenta o desenvolvimento de uma solução alternativa ao método ótico convencional na medição de micro dureza Vickers. Utilizando programação em LabVIEW da National Instruments, juntamente com as ferramentas de visão computacional (NI Vision), o programa começa por solicitar ao técnico a seleção da câmara para aquisição da imagem digital acoplada ao micro durómetro, seleção do método de ensaio (Força de ensaio); posteriormente o programa efetua o tratamento da imagem (aplicação de filtros para eliminação do ruído de fundo da imagem original), segue-se, por indicação do operador, a zona de interesse (ROI) e por sua vez são identificadas automaticamente os vértices da calote e respetivas distâncias das diagonais geradas concluindo, após aceitação das mesmas, com o respetivo cálculo de micro dureza resultante. Para validação dos resultados foram utilizados blocos-padrão de dureza certificada (CRM), cujos resultados foram satisfatórios, tendo-se obtido um elevado nível de exatidão nas medições efetuadas. Por fim, desenvolveu-se uma folha de cálculo em Excel com a determinação da incerteza associada às medições de micro dureza Vickers. Foram então comparados os resultados nas duas metodologias possíveis, pelo método ótico convencional e pela utilização das ferramentas de visão computacional, tendo-se obtido bons resultados com a solução proposta.

Performance assessment of waste fibre-reinforced mortar

Materials Science Forum Vols. 730-732 (2013) pp 617-622

Evaluation of Pozzolanic Reactivity of Artificial Pozzolans

Materials Science Forum Vols. 730-732 (2013) pp 433-438

Compact ion-source based on superionic rubidium silver iodide (RbAg4I5) solid electrolyte

Dissertação para obtenção do Grau de Mestre em Engenharia Física

Development of polymer wicks for the fabrication of bio-medical sensors

Polymer based wicking structures were fabricated by sintering powders of polycarbonate (PC), ultra-high molecular weight polyethylene and polyamide 12, aiming at selecting a suitable material for an innovative electroencephalography (EEG) bio-electrode. Preliminary experiments showed that PC based wicks displayed the best mechanical properties, therefore more detailed studies were carried out with PC to evaluate the influence of powder granulometry and processing parameters (pressure, temperature and time) on the mechanical properties, porosity, mean pore radius and permeability of the wicks. It was concluded that the mechanical properties are significantly enhanced by increasing the processing time and pressure, although at the expense of a significant decrease of porosity and mean pore diameter (and thus permeability), particularly for the highest applied pressures (74kPa). However, a good compromise between porosity/permeability and mechanical properties could be obtained by sintering PC powders of particle sizes below 500μm at 165°C for 5min, upon an applied pressure of 56kPa. Moreover, PC proved to be chemically stable in contact with an EEG common used disinfectant. Thus, wicking structures with appropriate properties for the fabrication of reusable bio-electrodes could be fabricated from the sintering of PC powders.

Dielectric relaxation dynamics of high-temperature piezoelectric polyimide copolymers

Polyimide co-polymers have been prepared based on different diamines as co-monomers: a diamine without CN groups and a novel synthesized diamine with two CN groups prepared by polycondensation reaction followed by thermal cyclodehydration. Dielectric spectroscopy measurements were performed and the dielectric complex function, ac conductivity and electric modulus of the co-polymers were investigated as a function of CN group content in the frequency range from 0.1 Hz to 107 Hz at temperatures from 25 to 260 °C. For all samples and temperatures above 150ºC, the dielectric constant increases with increasing temperature due to increaseing conductivity. The α-relaxation is just detected for the sample without CN groups, being this relaxation overlapped by the electrical conductivity contributions in the remaining samples. For the copolymer samples and the polymer with CN groups an important Maxwell-Wagner-Sillars contribution is detected. The mechanisms responsible for the dielectric relaxation, conduction process and electric modulus response have been discussed as a function of the CN groups content present in the samples.

Tailoring microstructure and physical properties of poly(vinylidene fluoride–hexafluoropropylene) porous films

This paper presents a systematic study for the production of poly(vinylidene fluoride-hexafluoropropylene), P(VDF-HFP), porous films using solvent evaporation (SE) and non-solvent induced phase separation (NIPS) techniques. Parameters such as volume fraction of the copolymer solution, film thickness, time exposure to air, non-solvent and temperature of the coagulation bath were investigated on the morphology, crystallization and mechanical properties of the samples. Films with different porous morphologies including homogeneous pore sizes, macrovoids and spherulites were obtained depending on the processing conditions, which in turn affect the wettability and mechanical properties of the material. Knowing that the phase content of the films also depends on the processing conditions, this paper shows that P(VDF-HFP) films with tailored porous morphology, electroactive phase content, hydrophobicity, cristallinity and mechanical properties can be achieved for a specific application using the adequate SE and NIPS techniques conditions.

Gd2O3: Eu3+/PPO/POPOP/PS composites for digital imaging radiation detectors

Polymer based scintillator composites have been produced by combining polystyrene (PS) and Gd2O3:Eu3+ scintillator nanoparticles. Polystyrene has been used since it is a flexible and stable binder matrix, resistant to thermal and light deterioration and with suitable optical properties. Gd2O3:Eu3+ has been selected as scintillator material due to its wide band gap, high density and visible light yield. The optical, thermal and electrical characteristics of the composites were studied as a function of filler content, together with their performance as scintillator material. Additionally 1wt.% of 2,5 dipheniloxazol (PPO) and 0.01wt.% of (1,4-bis(2-(5-phenioxazolil))-benzol (POPOP) were introduced in the polymer matrix in order to strongly improve light yield, i.e. the measured intensity of the output visible radiation, under X-ray irradiation. Whereas increasing scintillator filler concentration (from 0.25wt.% to 7.5wt.%) increases scintillator light yield, decreases the optical transparency of the composite. The addition of PPO and POPOP, strongly increased the overall 2 transduction performance of the composite due to specific absorption and re-emission processes. It is thus shown that Gd2O3:Eu3+/PPO/POPOP/PS composites in 0.25 wt.% of scintillator content with fluorescence molecules is suitable for the development of innovate large area X-ray radiation detectors with huge demand from the industries.

Inkjet printing technology for flexible pressure sensors

Tese de Doutoramento Ciência e Engenharia de Polímeros e Compósitos.