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Thesis (MScEng) -- Stellenbosch University, 2014. / ENGLISH ABSTRACT: In this study, commercially pure titanium foam was produced using space holder powder metallurgy techniques. Titanium foam is attractive as a scaffolding material for bone replacement and implants in the body. The porous morphology of the foam promotes osteogenesis, while the mechanical behaviour of the foam is closer to that of bone, which has an elastic moduli range of 5 - 40 GPa. Titanium foam was manufactured from powder mixtures of commercially pure titanium (CPTi) powder mixed with 41.4 wt% ammonium bicarbonate (ABC) powder and 1.45 wt% polyethyl glycol (PEG) powder. In this study, two CPTi powders with different particle size distributions, < 75 μm (-200 mesh, designated TiAA) and < 200 μm (-100 mesh, designated TiG), were mixed with the space holder ABC powder, that had been sieved into specified particle size ranges. The size ranges of space holder material studied were: 0 - 710, 250 - 425, 425 - 560, and 560 - 710 μm. This allowed foams with different large or macropore distributions to be produced from the different mixtures. The mixtures were uniaxially compacted at 100 MPa into transverse rupture bars. The ABC and PEG was then removed by thermal debinding in air for 5 hours at 100 °C and 1 hour at 330 °C each, consecutively. The debound samples are then sintered under high (10-6 mbar) vacuum on yttria-stabilised zirconia substrates, heating at 5 °C/min to 1200 °C, with a 2 hour hold at temperature. The microstructures of the different foams were evaluated by examining the polished samples using light optical microscopy. Three point bend tests were conducted on the sintered bars in order to determine the flexural strength and flexural modulus of the different foams. The produced foams had a relative density range between 37.5 - 62.5 % and average macro pore size range between 300 - 500 μm. The foams were found to have an elastic modulus similar to that of bone, 2 - 7 GPa. Finally, the mechanical properties of the foams were compared to known open foam mechanical models and other research projects. It was found that: (i) changes in either metal or space holder powder influences the sintering behaviour of metal foams, (ii) sintered titanium foams with similar densities but different macro/micropore size distributions have different mechanical responses to stress and (iii) the Ashby-Gibson model, based on foam density alone, gives a rough estimate of mechanical properties for the titanium foams studied, but does not capture variations due to pore size distribution. / AFRIKAANSE OPSOMMING: In hierdie studie is kommersiële suiwer titaanskuim geproduseer met behulp van ruimtehouer poeier metallurgie tegnieke. Titaanskuim is aantreklik as 'n raamwerkmateriaal vir beenvervanging en -inplantings in die liggaam. Die poreuse morfologie van die skuim bevorder osteogenese, terwyl die meganiese gedrag van die skuim naby aan dié van been is, met ‘n elasticiteitsmodulus tussen 5 - 40 GPa. Titaanskuim is vervaardig van ‘n poeier mengsel van kommersiële suiwer titaan (CPTi) poeier gemeng met 41,4 gew% ammonium bikarbonaat (ABC) poeier en 1.45 gew% poli-etileenglikol (PEG) poeier. In hierdie studie is twee tipes CPTi poeiers met verskillende deeltjiegrootteverspreiding, < 75 μm (-200 stofdigtheid, TiAA genoem) en <200 μm (-100 stofdigtheid, TiG genoem), met die ruimtehouer ABC-poeier, wat in bepaalde deeltjiegroottereekse gesif is, gemeng. Die wisselende groottes van ruimtehouer wat bestudeer is, was: 0 - 710, 250 - 425, 425 - 560, 560 - 710 μm. Dit het die vervaardiging van skuim met verskillende groot of macroporeuse vanaf die verskillende mengsels toegelaat. Die mengsel is teen 100 MPa in een rigting gekompakteer. Die ABC en PEG is dan verwyder word deur termiese ontbinding in lug vir 5 uur by 100 °C en 1 uur by 330 °C elk, onderskeidelik. Die ontbinde monsters is dan onder hoë (10-6 mbar) leemte op yttrium-gestabiliseer zirconia-substraat, met verwarming teen 5 °C/min tot 1200 °C met 'n verdere 2 uur by 1200 °C, gesinterd. Die mikrostrukture van die verskillende skuim is geëvalueer deur gepoleerde monsters met behulp van ‘n ligmikroskopie te ondersoek . Driepunt draaitoetse is op die gesinterd stawe uitgevoer om die buigsterkte en buigmodulus van die verskillende skuime te bepaal. Die vervaardigde skuime se relatiewe digtheid het tussen 37,5 - 62,5 % gewissel en die gemiddelde makroporiegrootte tussen 300 - 500 μm gewissel. Die skuim het 'n elastisiteitsmodulus soortgelyk aan dié van been getoon, 2 – 7 GPa. Ten slotte is die meganiese eienskappe van die skuim met bekende oop skuim meganiese modelle en ander navorsingsprojekte vergelyk. Daar is bevind dat: (i) veranderinge in óf metaal of ruimtehouer poeier beïnvloed die sinteringgedrag van metaalskuime, (ii) gesinterd titaniumskuim met soortgelyke digthede, maar verskillende makro / mikroporeuse verdelings, toon verskillende meganiese reaksies op stres en die Ashby-Gibson model, gebaseer op die skuimdigtheid alleen, (iii) wat 'n rowwe skatting van die meganiese eienskappe vir die bestudeerde titaniumskuime gee, maar nie die variasies ingrootteverspreiding van porieë ondervang nie.

Dental and orthopaedic implants are currently the solutions of choice for teeth and joint replacements with success rates continually improving, but they still have undesirable failure rates in patients who are compromised by disease or age, and who in many cases are the ones most in need. The success of titanium (Ti) implants depends on their ability to osseointegrate with the surrounding bone and this, in turn, is greatly dependent on the surface characteristics of the device. Advancements in surface analysis and surface modification techniques have improved the biological performance of metallic implants by mimicking the hierarchical structure of bone associated with regular bone remodeling. In this process, damaged bone is resorbed by osteoclasts, which produce resorption lacunae containing high microroughness generated after mineral dissolution under the ruffled border, as well as superimposed nanoscale features created by the collagen fibers left at the surface. Indeed, increasing Ti surface roughness at the micro and sub-microscale level has been shown to increase osteoblast differentiation in vitro, increase bone-to-implant contact in vivo, and accelerate healing times clinically. Recently, the clinical application of surface nanomodification of implants has been evaluated. Still, most clinically-available devices remain smooth at the nanoscale and fundamental questions remain to be elucidated about the effect of nanoroughness on the initial response of osteoblast lineage cells. Another property that could be used to control osteoblast development and the process of osseointegration is the electrical surface charge of implants. The presence of endogenous electrical signals in bone has been implicated in the processes of bone remodeling and repair. The existence of these native signals has prompted the use of external electrical stimulation to enhance bone growth in cases of fractures with delayed union or nonunion, with several in vitro and in vivo reports confirming its beneficial effects on bone formation. However, the use of electrical stimulation on Ti implants to enhance osseointegration is less understood, in part because of the lack of in vitro models that truly represent the in vivo environment. In addition, an aspect that has not been thoroughly examined is the electrical implication of implant corrosion and its effect on the surrounding tissue. Implants are exposed to extreme conditions in the body such as high pH during inflammation, and cyclic loads. These circumstances may lead to corrosion events that generate large electrochemical currents and potentials, and may cause abnormal cell and tissue responses that could be partly responsible for complications such as aseptic loosening of implants. Consequently, Ti implants with tailored surface characteristics such as nanotopography and electrical polarization, could promote bone healing and osseointegration to ensure successful outcomes for patients by mimicking the biological environment of bone without the use of systemic drugs. The objective of this thesis is to understand how surface nanostructural and electrical characteristics of Ti and Ti alloy surfaces may affect osteoblast lineage cell response in vitro for normal tissue regeneration and repair. Our central hypothesis is that combined micro/nanostructured surfaces, as well as direct stimulation of Ti surfaces with fixed direct current (DC) potentials, can enhance osteoblast differentiation.

Cell adhesion to the extracellular matrix through cell-surface integrin receptors is essential to development, wound healing, and tissue remodeling and therefore represents a central theme in the design of bioactive surfaces that successfully interface with the body. This is especially significant in the areas of integrative implant coatings since adhesion triggers signals that regulate cell cycle progression and differentiation in multiple cellular systems. The interactions of osteoblasts with their surrounding extracellular matrix are essential for skeletal development and homeostasis and the maintenance of the mature osteoblastic phenotype. Our objective was to engineer integrin-specific bioactive surfaces that support osteoblastic differentiation and promote osseointegration by mimicking these interactions. We target two specific integrins essential to osteoblast differentiation the type I collagen receptor alpha2beta1 and the fibronectin receptor alpha5beta1. The central hypothesis of this project was that the controlled presentation of type I collagen and fibronectin binding domains onto well-defined substrates would result in integrin-specific bioadhesive surfaces that support osteoblastic differentiation, matrix mineralization, and osseointegration. We have demonstrated that these biomimetic peptides enhance bone formation and mechanical osseointegration on titanium implants in a rat tibia cortical bone model. We have also shown that the presentation of multiple integrin-binding ligands synergize to enhance intracellular signaling and proliferation. Finally, we demonstrate the advantage of the short biomimetic peptides over the native ECM proteins. This research is significant because it addresses current orthopaedic implant limitations by specifically targeting cellular responses that are critical to osteoblastic differentiation and bone formation. This biomolecular approach provides a versatile and robust strategy for developing bioactive surfaces that enhance bone repair and osseointegration of orthopaedic implants.

This doctoral thesis is devoted to studying the possibilities of using additive manufacturing (AM) and design based on computed tomography (CT), for the production of patient-specific implants within orthopedic surgery, initially in a broad perspective and, in the second part of the thesis focusing on customized clavicle osteosynthesis plates. The main AM method used in the studies is the Electron Beam Melting (EBM) technology. Using AM, the parts are built up directly from 3D computer models, by melting or in other ways joining thin layers of material, layer by layer, to build up the part. Over the last 20 years, this fundamentally new way of manufacturing and the rapid development of software for digital 3D reconstruction of anatomical models from medical imaging, have opened up entirely new opportunities for the design and manufacturing of patient-specific implants. Based on the information in a computed tomography (CT) scan, both digital and physical models of the anatomy can be created and of implants that are customized based on the anatomical models.   The main method used is a number of case studies performed, focusing on different parts of the production chain, from CT-scan to final implant, and with several aims: learning about the details of the different steps in the procedure, finding suitable applications, developing the method and trying it out. The first study was on customized hip stems, focusing on the EBM method and its special preconditions and possibilities. It was followed by a study of bone plates, designed to follow the patient-specific bone contour, in this case a tibia fracture including the whole production chain. Further, four cases of patient-specific plates for clavicle fracture fixation were performed in order to develop and evaluate the method. The plates fit towards the patient’s bone were tested in cooperation with an orthopedic surgeon at Östersund hospital. In parallel with the case studies, a method for finite element (FE) analysis of fixation plates placed on a clavicle bone was developed and used for the comparative strength analysis of different plates and plating methods. The loading on the clavicle bone in the FE model was defined on a muscle and ligament level using multibody musculoskeletal simulation for more realistic loading than in earlier similar studies.    The initial studies (papers I and II) showed that the EBM method has great potential, both for the application of customized hip stems and bone plates; in certain conditions EBM manufacturing can contribute to significant cost reductions compared to conventional manufacturing methods due to material savings and savings in file preparation time. However, further work was needed in both of the application areas before implementation. The studies on the fracture fixation using patient-specific clavicle plates indicated that the method can facilitate the work for the surgeon both in the planning and in the operating room, with the potential of a smoother plate with a better fit and screw positioning tailored to the specific fracture (paper VI). However, a large clinical trial is required to investigate the clinical benefit of using patient-specific plates. The FE simulations showed similar stress distributions and displacements in the patient-specific plates and the commercial plates (papers III to VI).   To summarize: the results of this thesis contribute to the area of digital design and AM in patient-specific implants with broad basis of knowledge regarding the technologies used and areas in which further work is needed for the implementation of the technology on a larger scale. Further, a method has been developed and initially evaluated for implementation in the area of clavicle fracture fixation, including an approach for comparing the strength of different clavicle plates.

Orientador: Rubens Caram Junior / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-23T09:33:56Z (GMT). No. of bitstreams: 1 Lopes_EderSocratesNajar_D.pdf: 9279894 bytes, checksum: a2ed77cd79f48134e7daf5bc705afb0e (MD5) Previous issue date: 2013 / Resumo: Ligas de Ti do tipo ? metaestável exibem comportamento singular no tocante à possibilidade de manipulação de seu comportamento mecânico. Nessas ligas, a rigidez pode ser alterada por meio do controle das fases presentes, o que permite que esses materiais sejam incluídos no seleto grupo dos materiais com gradientes funcionais (functionally graded materials - FGM). Neste trabalho, objetivou-se projetar, produzir, processar, caracterizar e aplicar ligas Ti-Nb com adições do elemento ? estabilizador de baixo custo Fe. As ligas foram produzidas por fusão a arco voltaico e submetidas a diversas condições de tratamento térmico, incluindo solubilização acima da temperatura ?-transus, resfriamento rápido até a temperatura ambiente e tratamentos térmicos de envelhecimento entre 260 °C e 400 °C. A caracterização envolveu calorimetria diferencial de varredura, difração de raios-X e dureza Vickers em alta temperatura, análises metalográficas e de módulo de elasticidade por técnicas acústicas, ensaios de tração e mapeamento de rigidez por meio de nanoindentação. Os resultados obtidos mostram a retenção completa da fase ? para a liga Ti-30Nb-3Fe solubilizada e resfriada rapidamente e permitem também, compreender a decomposição da fase martensita ?" e a nucleação das fases ? e ?. A adição do elemento Fe tornou a cinética de transformação de fases bem mais lenta, propiciando, sob algumas condições, a supressão da fase ?, que é conhecida por aumentar a dureza em detrimento da ductilidade. Tais resultados foram utilizados no estabelecimento de condições ideais de processamento que permitem obter componentes ortopédicos com rigidez gradual. Finalmente, o conhecimento adquiro foi usado na fabricação de placas e parafusos de osteossíntese a partir da liga Ti-30Nb-3Fe com gradientes de funcionalidade / Abstract: Metastable ? Ti alloys exhibit singular behavior regarding the possibility of manipulating their mechanical behavior. In these alloys, the stiffness can be changed by controlling phases, which allows these materials to be included in the select group of functionally graded materials (FGM). This study aimed to design, produce, process, characterize and apply Ti-Nb alloys with addition of Fe, an inexpensive ? stabilizing element. These alloys were produced by arc melting and subjected to different heat treatment conditions, including solution above the ?- transus temperature, quenching to room temperature and aging heat treatments between 260 °C and 400 °C. Characterization involved differential scanning calorimetry, X-ray diffraction and Vickers hardness at high temperature, metallographic analyzes, elastic modulus by acoustic techniques, tensile test and stiffness mapping via nanoindentation. The results obtained show complete retention of the ? phase in the Ti-30Nb-3Fe alloy after solution in the ? field and rapid cooling to room temperature and also allow understanding martensite ?" decomposition and nucleation of the ? and ? phases. It was found that Fe additions make the phase transformation kinetics much slower, providing, for some conditions, suppression of the ? phase precipitation, which is known to increase the hardness at the expense of ductility. These results were used to establish optimal processing conditions, resulting in orthopedic component with graded stiffness. Finally, the knowledge acquired was used in the manufacturing of osteosynthesis plates and screws with functionality graded from the Ti-30Nb-3Fe / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

Made available in DSpace on 2014-10-09T12:41:41Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:15Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Orientador: Cecilia A. C. Zavaglia / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica / Made available in DSpace on 2018-08-07T02:27:14Z (GMT). No. of bitstreams: 1 Uzumaki_EmiliaTieko_D.pdf: 44142340 bytes, checksum: e8db433907d2fd2f88b260ed4cd8a791 (MD5) Previous issue date: 2006 / Resumo: O carbono tipo diamante ("diamond-like carbon" - DLC) tem demonstrado características, como alta dureza, baixo atrito, resistência ao desgaste e à corrosão, e biocompatibilidade, que podem melhorar as propriedades de implantes sólidos e articulados. O processo de imersão em plasma vem sendo usado para depositar DLC em substratos tridimensionais, pois, com esta técnica, se consegue melhor adesão do que com as técnicas convencionais. Neste trabalho, filmes de DLC foram depositados, pelo processo de imersão em plasma, em lamínulas de vidro, silício e liga de titânio Ti-13Nb-13Zr. A caracterização da microestrutura, morfologia, dureza e adesão dos filmes de DLC foi feita por espectroscopia Raman, microscopia eletrônica de varredura (MEV), microscopia de força atômica (MFA), nanoindentação e ensaio de puxamento. Como exemplos de peças tridimensionais, filmes de DLC foram depositados em implantes osteoarticulares de quadril e joelho, titânio poroso (esponja de célula-aberta, semelhante à estrutura do osso esponjoso, expandida a vácuo), facas industriais, bisturi cirúrgico, engrenagem de motor, tubos de quartzo e de alumínio, e outros objetos. O filme obtido apresentou boas propriedades mecânicas, aumentando em 2 vezes a dureza da liga de Ti, alta adesão (filme sem interface definida e sem delaminação), resistência ao desgaste, baixa rugosidade e uniformidade de deposição em superfícies tridimensionais. Os resultados de corrosão (polarização de Tafel e espectroscopia de impedância eletroquímica em fluido corporal simulado) mostraram que o revestimento de DLC melhora a resistência da liga de Ti à corrosão. No ensaio de biocompatibilidade in vitro, com células fibroblásticas, foram estudados a citotoxicidade, adesão e morfologia celular (estudo citoquímico, microscopia de contraste de fase, MEV e MFA). No ensaio de biocompatibilidade in vivo, a liga de Ti-13Nb-13Zr, revestida com DLC, foi investigada em tecido muscular e ósseo de ratos após 4 e 12 semanas do procedimento cirúrgico. A interface formada entre o DLC e o tecido foi investigada por histologia convencional, e os implantes retirados por MEV. A interface entre o implante e o tecido ósseo, não descalcificado, foi estudada por MEV na modalidade retroespalhamento. Os resultados mostraram a biocompatibilidade in vitro e in vivo do filme de DLC, e foi verificado também que os implantes revestidos com DLC possuem resposta biológica mais favorável do que os implantes não revestidos / Abstract: Diamond-like carbon (DLC) films are often considered a suitable coating material for orthopaedic applications. It has proven characteristics, such as hardness, wear resistance, low friction coefficient and biocompatibility that improve the properties of solid and articulated implants. Recently, the plasma immersion process was used to deposit DLC films with superior adhesion properties to those prepared with conventional techniques. DLC coatings were deposited on glass coverslips, silicon (Si) and Ti-13Nb-13Zr substrates using the plasma immersion process. The microstructure, morphology, roughness, hardness and adhesion of DLC films were characterized using Raman spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), nanoindentation and pull-test. As examples, DLC films produced by plasma immersion were deposited on industrial knives, surgical knives, knee implants, femoral heads (of hip prostheses), titanium foams, transmission gears of motorcycles, aluminium pipes, quartz pipes, and others objects. The corrosion susceptibility of DLC coatings produced by plasma immersion was studied in a simulated body fluid environment (Hanks' solution) using polarization test and electrochemical impedance spectroscopy (EIS). Electrochemical results showed that DLC coating produced by plasma immersion could improve corrosion resistance, and no significant damage has been observed. Vero cells (fibroblasts) were utilized for the in vitro biocompatibility studies, by cytotoxicity, adhesion and cell morphology (phase contrast microscopy, SEM, AFM, and cytochemical study). DLC-coated Ti-13Nb-13Zr was investigated in an animal model using the muscular tissue and femoral condyles of rats for intervals of 4 and 12 weeks postoperatively. The interface between the implants and tissue were analysed by light microscopy, and the removed implants by SEM. The SEM by backscattering was used to access the interface between the implants the bone tissue without decalcifying. Our results indicate that DLC coatings are biocompatible in vitro and in vivo / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

Made available in DSpace on 2014-10-09T12:41:41Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:15Z (GMT). No. of bitstreams: 0 / A instalação de implantes odontológicos requer a presença de substrato ósseo adequado para garantir estabilidade e equilíbrio biomecânico. A deficiência óssea requer procedimentos de enxertia para adequar o volume para a instalação de implantes, porém a utilização de enxertos autógenos causa aumento de morbidade ao paciente e o uso de material homógeno e xenógeno apresenta dúvidas quanto à reação autoimune, transmissão de doenças e ao grau de reabsorção do enxerto. Com o grande desenvolvimento científico e tecnológico dos biomateriais, os materiais cerâmicos, tornaram-se alternativas promissoras para a recomposição da estrutura óssea perdida. As cerâmicas à base de fosfato de cálcio como a hidroxiapatita (HA) e o beta- fosfato tricálcido (beta-TCP), são materiais que apresentam qualidades desejáveis no processo de neoformação óssea como, por exemplo, a biocompatibilidade, bioatividade e osteocondutividade. A proposta deste trabalho é desenvolver e estudar corpos de prova na forma de cúpula oca de hidroxiapatita preenchidos por coágulo, beta- TCP e composto vitamínico, para estudar a osteogênese supracortical, a partir do potencial osteocondutor da cúpula de HA. As cúpulas foram obtidas por prensagem isostática a 200 MPa e sinterização ao ar a 1100°C por 60 minutos. As caracterizações físico-químicas das matérias-primas e da cúpula de HA foram realizadas por difração de raios X, microscopia eletrônica de varredura e determinação da densidade. Na caracterização biológica, foram realizados o teste de citotoxicidade in vitro e ensaio in vivo. Foram designados 9 coelhos (raça Nova Zelândia), sendo instaladas 18 cúpulas, divididas em três grupos, de acordo com o preenchimento: controle, composto vitamínico e &beta;-TCP em forma de pó. O período de reparação tecidual foi de 8 semanas, no qual foram aplicados marcadores de fluorescência. Após o período de cicatrização e eutanásia, as amostras foram incluídas em resina para a obtenção das lâminas e observadas em microscópio de fluorescência, para avaliar a quantidade de tecido ósseo neoformado, em microscópio de campo claro, para verificar as células presentes no tecido formado e por Espectroscopia de Energia Dispersiva, para análise química, da formação no interior das cúpulas. Como resultados, a cúpula de hidroxiapatita apresenta bom desempenho como arcabouço para neoformação óssea acima da cortical da tíbia de coelhos, pois manteve-se íntegra, com boa estabilidade e boa integração ao tecido ósseo, e principalmente pela neoformação óssea, demonstrando seu potencial osteocondutor. Em relação aos materiais de preenchimento, o beta-TCP apresenta maior valor de área de osso neoformado, em comparação com o coágulo. Nas cúpulas com preenchimento de composto vitamínico, não há formação de tecido ósseo pela não reabsorção do material. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

This thesis refers to Fe-based biodegradable materials and their potencial aplications in medicine, especially as temporary bone implants. This work generaly summaries aplications of biomaterial in medicine with more interest kept on biodegradable materials and their in-vivo corrosion. The experimental part refers to conduction of porous Fe-based materials with silica addition. The structure of prepared specimens is identified by EDX and XRD analysis. The imersion test and electrochemical studies were conducted to observe corrosion behaviour with respect to different concentration of silica. Potenciodynamic curves were obtained to determine corrosion potencial and corrosion current density of prepared samples.