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1.
Acta Biomater ; 184: 264-272, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38908419

RESUMO

The equine hoof wall has outstanding impact resistance, which enables high-velocity gallop over hard terrain with minimum damage. To better understand its viscoelastic behavior, complex moduli were determined using two complementary techniques: conventional (∼5 mm length scale) and nano (∼1 µm length scale) dynamic mechanical analysis (DMA). The evolution of their magnitudes was measured for two hydration conditions: fully hydrated and ambient. The storage modulus of the ambient hoof wall was approximately 400 MPa in macro-scale experiments, decreasing to ∼250 MPa with hydration. In contrast, the loss tangent decreased for both hydrated (∼0.1-0.07) and ambient (∼0.04-0.01) conditions, over the frequency range of 1-10 Hz. Nano-DMA indentation tests conducted up to 200 Hz showed little frequency dependence beyond 10 Hz. The loss tangent of tubular regions showed more hydration sensitivity than in intertubular regions, but no significant difference in storage modulus was observed. Loss tangent and effective stiffness were higher in indentations for both hydration levels. This behavior is attributed to the hoof wall's hierarchical structure, which has porosity, functionally graded aspects, and material interfaces that are not captured at the scale of indentation. The hoof wall's viscoelasticity characterized in this work has implications for the design of bioinspired impact-resistant materials and structures. STATEMENT OF SIGNIFICANCE: The outer wall of horse hooves evolved to withstand heavy impacts during gallop. While previous studies have measured the properties of the hoof wall in slowly changing conditions, we wanted to quantify its behavior using experiments that replicate the quickly changing forces of impact. Since the hoof wall's structure is complex and contributes to its overall performance, smaller scale experiments were also performed. The behavior of the hoof wall was within the range of other biological materials and polymers. When hydrated, it becomes softer and can dissipate more energy. This work improves our understanding of the hoof's function and allows for more accurate simulations that can account for different impact speeds.


Assuntos
Elasticidade , Casco e Garras , Viscosidade , Animais , Cavalos/anatomia & histologia , Módulo de Elasticidade , Casco e Garras/fisiologia
2.
Materials (Basel) ; 17(11)2024 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-38893943

RESUMO

Additive manufacturing (AM) is often used to create designs inspired by topology optimization and biological structures, yielding unique cross-sectional geometries spanning across scales. However, manufacturing defects intrinsic to AM can affect material properties, limiting the applicability of a uniform material model across diverse cross-sections. To examine this phenomenon, this paper explores the influence of specimen size and layer height on the compressive modulus of polycarbonate (PC) and thermoplastic polyurethane (TPU) specimens fabricated using fused filament fabrication (FFF). Micro-computed tomography imaging and compression testing were conducted on the printed samples. The results indicate that while variations in the modulus were statistically significant due to both layer height and size of the specimen in TPU, variations in PC were only statistically significant due to layer height. The highest elastic modulus was observed at a 0.2 mm layer height for both materials across different sizes. These findings offer valuable insights into design components for FFF, emphasizing the importance of considering mechanical property variations due to feature size, especially in TPU. Furthermore, locations with a higher probability of failure are recommended to be printed closer to the print bed, especially for TPU, because of the lower void volume fraction observed near the heated print bed.

4.
Rev Sci Instrum ; 94(8)2023 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-38065188

RESUMO

Reference point indentation (RPI) is a novel experimental technique designed to evaluate bone quality. This study utilizes two RPI instruments, BioDent and Osteoprobe, to investigate the mechanical responses of several 3D-printed polymers. We correlated the mechanical properties from a tensile test with the RPI parameters obtained from the BioDent and OsteoProbe. In addition, we tested the same polymers five years later (Age 5). The results show that for Age 0 polymers, the elastic modulus is highly correlated with average unloading slope (r = 0.87), first unloading slope (r = 0.85), bone material strength index (BMSi) (r = 0.85), average loading slope (r = 0.82), first indentation distance (r = 0.79), and total indentation distance (r = 0.76). The ultimate stress correlates significantly with first unloading slope (r = 0.85), average unloading slope (r = 0.83), BMSi (r = 0.81), first indentation distance (r = 0.73), average loading slope (r = 0.71), and total indentation distance (r = 0.70). The elongation has no significant correlation with the RPI parameters except with the average creep indentation distance (r = 0.60). For Age 5 polymers, correlations between mechanical properties and RPI parameters are low. This study illustrates the potential of RPI to assess the mechanical properties of polymers nondestructively with simple sample requirements. Furthermore, for the first time, 3D-printed polymers and aged polymers are investigated with RPI.

5.
J Ind Microbiol Biotechnol ; 50(1)2023 Feb 17.
Artigo em Inglês | MEDLINE | ID: mdl-37248049

RESUMO

Plastic waste is an outstanding environmental thread. Poly(ethylene terephthalate) (PET) is one of the most abundantly produced single-use plastics worldwide, but its recycling rates are low. In parallel, additive manufacturing is a rapidly evolving technology with wide-ranging applications. Thus, there is a need for a broad spectrum of polymers to meet the demands of this growing industry and address post-use waste materials. This perspective article highlights the potential of designing microbial cell factories to upcycle PET into functionalized chemical building blocks for additive manufacturing. We present the leveraging of PET hydrolyzing enzymes and rewiring the bacterial C2 and aromatic catabolic pathways to obtain high-value chemicals and polymers. Since PET mechanical recycling back to original materials is cost-prohibitive, the biochemical technology is a viable alternative to upcycle PET into novel 3D printing materials, such as replacements for acrylonitrile butadiene styrene. The presented hybrid chemo-bio approaches potentially enable the manufacturing of environmentally friendly degradable or higher-value high-performance polymers and composites and their reuse for a circular economy. ONE-SENTENCE SUMMARY: Biotransformation of waste PET to high-value platform chemicals for additive manufacturing.


Assuntos
Polímeros , Estireno , Polietilenotereftalatos , Bactérias , Reciclagem , Biotransformação , Plásticos
6.
J Mech Behav Biomed Mater ; 136: 105529, 2022 12.
Artigo em Inglês | MEDLINE | ID: mdl-36327663

RESUMO

This study predicts analytically effective elastic moduli of substructures within an equine hoof wall. The hoof wall is represented as a composite material with a hierarchical structure comprised of a sequence of length scales. A bottom-up approach is employed. Thus, the outputs from a lower spatial scale serve as the inputs for the following scale. The models include the Halpin-Tsai model, composite cylinders model, a sutured interface model, and classical laminate theory. The length scales span macroscale, mesoscale, sub-mesoscale, microscale, sub-microscale, and nanoscale. The macroscale represents the hoof wall, consisting of tubules within a matrix at the mesoscale. At the sub-mesoscale, a single hollow tubule is reinforced by a tubule wall made of lamellae; the surrounding intertubular material also has a lamellar structure. The lamellae contain sutured and layered cells at the microscale. A single cell is made of crystalline macrofibrils arranged in an amorphous matrix at the sub-microscale. A macrofibril contains aligned crystalline rod-like intermediate filaments at the nanoscale. Experimentally obtained parameters are used in the modeling as inputs for geometry and nanoscale properties. The predicted properties of the hoof wall material agree with experimental measurements at the mesoscale and macroscale. We observe that the hierarchical structure of the hoof wall leads to a decrease in the elastic modulus with increasing scale, from the nanoscale to the macroscale. Such behavior is an intrinsic characteristic of hierarchical biological materials. This study can serve as a framework for designing impact-resistant hoof-inspired materials and structures.


Assuntos
Casco e Garras , Animais , Cavalos , Módulo de Elasticidade
7.
Acta Biomater ; 151: 426-445, 2022 10 01.
Artigo em Inglês | MEDLINE | ID: mdl-35995409

RESUMO

The horse hoof wall exhibits exceptional impact resistance and fracture control due to its unique hierarchical structure which contains tubular, lamellar, and gradient configurations. In this study, structural characterization of the hoof wall was performed revealing features previously unknown. Prominent among them are tubule bridges, which are imaged and quantified. The hydration-dependent viscoelasticity of the hoof wall is described by a simplified Maxwell-Weichert model with two characteristic relaxation times corresponding to nanoscale and mesoscale features. Creep and relaxation tests reveal that the specific hydration gradient in the hoof keratin likely leads to reduced internal stresses that arise from spatial stiffness variations. To better understand realistic impact modes for the hoof wall in-vivo, drop tower tests were executed on hoof wall samples. Fractography revealed that the hoof wall's reinforced tubular structure dominates at lower impact energies, while the intertubular lamellae are dominant at higher impact energies. Broken fibers were observed on the surface of the tubules after failure, suggesting that the physically intertwined nature of the tubule reinforcement and intertubular matrix improves the toughness of this natural fiber reinforced composite. The augmented understanding of the structure-mechanical property relationship in dynamic loading led to the design of additively manufactured bioinspired structures, which were evaluated in quasistatic and dynamic loadings. The inclusion of gradient structures and lamellae significantly reduced the damage sustained in drop tower tests, while tubules increased the energy absorption of samples tested in compact tension. The samples most similar to the hoof wall displayed remarkably consistent fracture control properties. STATEMENT OF SIGNIFICANCE: The horse hoof wall, capable of withstanding large, repeated, dynamic loads, has been touted as a candidate for impact-resistant bioinspiration. However, our understanding of this biological material and its translation into engineered designs is incomplete. In this work, new features of the horse hoof wall are quantified and the hierarchical failure mechanisms of this remarkable material under near-natural loading conditions are uncovered. A model of the hoof wall's viscoelastic response, based on studies of other keratinous materials, was developed. The role of hydration, strain rate, and impact energy on the material's response were elucidated. Finally, multi-material 3D printed designs based on the hoof's meso/microstructure were fabricated and exhibited advantageous energy absorption and fracture control relative to control samples.


Assuntos
Fraturas Ósseas , Casco e Garras , Animais , Extremidades , Cavalos , Queratinas/química
8.
J Mech Behav Biomed Mater ; 134: 105370, 2022 10.
Artigo em Inglês | MEDLINE | ID: mdl-35872461

RESUMO

This computational study addresses new biomimetic load-bearing implants designed to treat long bone critical-sized defects in a proximal diaphysis region. The design encompasses two strategies: a Haversian bone-mimicking approach for cortical bone and lattices based on triply periodic minimal surfaces (TPMS) for trabecular bone. Compression tests are modeled computationally via a non-linear finite element analysis with Ti6Al4V alloy as a base material. Nine topologies resembling cortical bone are generated as hollow cylinders with different channel arrangements simulating Haversian (longitudinal) and Volkmann (transverse) canals to achieve properties like those of a human cortical bone (Strategy I). Then, the selected optimal structure from Strategy I is merged with the trabecular bone part represented by four types of TPMS-based lattices (Diamond, Primitive, Split-P, and Gyroid) with the same relative density to imitate the whole bone structure. The Strategy I resulted in finding a hollow cylinder including Haversian and Volkmann canals, optimized in canals number, shape, and orientation to achieve mechanical behavior close to human cortical bone. The surface area and volume created by such canals have the maximum values among all studied combinations of transverse and longitudinal channels. Strategy II reveals the effect of interior design on the load-bearing capacity of the whole component. Between four types of selected TPMS, Diamond-based lattice and Split-P have more uniform stress distribution, resulting in a superior load-bearing efficiency than Gyroid and Primitive-based design showing less uniformity. This work offers a new design of the bone-mimicking implant, with cortical and trabecular bone components, to repair long bone critical-sized defects.


Assuntos
Biomimética , Próteses e Implantes , Diamante , Análise de Elementos Finitos , Ósteon , Humanos , Porosidade
9.
iScience ; 24(8): 102798, 2021 Aug 20.
Artigo em Inglês | MEDLINE | ID: mdl-34355149

RESUMO

Keratin is a highly multifunctional biopolymer serving various roles in nature due to its diverse material properties, wide spectrum of structural designs, and impressive performance. Keratin-based materials are mechanically robust, thermally insulating, lightweight, capable of undergoing reversible adhesion through van der Waals forces, and exhibit structural coloration and hydrophobic surfaces. Thus, they have become templates for bioinspired designs and have even been applied as a functional material for biomedical applications and environmentally sustainable fiber-reinforced composites. This review aims to highlight keratin's remarkable capabilities as a biological component, a source of design inspiration, and an engineering material. We conclude with future directions for the exploration of keratinous materials.

10.
J Biomech ; 123: 110531, 2021 06 23.
Artigo em Inglês | MEDLINE | ID: mdl-34051614

RESUMO

Recent transmission electron microscopy images of transverse sections of human cortical bone showed that mineral lamellae (polycrystalline sheets of apatite crystals) form arcuate multi-radius patterns around collagen fibrils. The 3-6 nm thick mineral lamellae are arranged in stacks of 3-20 layers and curve around individual fibrils, few fibrils, and higher numbers of collagen fibrils. We evaluate the effect of these stacked mineral lamellae with various radius of curvature patterns on the elastic bending and torsional responses of bone at the sub-microscale using a finite element method. We find that the curved multi-radius stack patterns increased the bending and torsional stiffnesses by 7% and 23%, respectively, compared to when the stacks of mineral lamellae only encircle individual fibrils for the idealized geometric models considered. This study provides new insights into the structure-property relations for the bone ultrastructure.


Assuntos
Osso e Ossos , Colágeno , Apatitas , Humanos , Microscopia Eletrônica de Transmissão , Minerais
11.
Sci Rep ; 11(1): 7012, 2021 03 29.
Artigo em Inglês | MEDLINE | ID: mdl-33782429

RESUMO

Bone is a biological composite material consisting of two main components: collagen and mineral. Collagen is the most abundant protein in vertebrates, which makes it of high clinical and scientific interest. In this paper, we compare the composition and structure of cortical bone demineralized using several protocols: ethylene-diamine-tetraacetic acid (EDTA), formic acid (CH2O2), hydrochloric acid (HCl), and HCl/EDTA mixture. The efficiencies of these four agents were investigated by assessing the remaining mineral quantities and collagen integrity with various experimental techniques. Raman spectroscopy results show that the bone demineralized by the CH2O2 agent has highest collagen quality parameter. The HCl/EDTA mixture removes the most mineral, but it affects the collagen secondary structure as amide II bands are shifted as observed by Fourier transform infrared spectroscopy. Thermogravimetric analysis reveals that HCl and EDTA are most effective in removing the mineral with bulk measurements. In summary, we conclude that HCl best demineralizes bone, leaving the well-preserved collagen structure in the shortest time. These findings guide on the best demineralization protocol to obtain high-quality collagen from bone for clinical and scientific applications.


Assuntos
Técnica de Desmineralização Óssea/classificação , Técnica de Desmineralização Óssea/métodos , Colágeno/química , Osso Cortical/metabolismo , Animais , Suínos
12.
J Mech Behav Biomed Mater ; 113: 104132, 2021 01.
Artigo em Inglês | MEDLINE | ID: mdl-33049620

RESUMO

Bone is a composite material consisting principally of apatite mineral, collagen fibrils, non-collagenous proteins, and other organic species. Recent electron microscopy studies have shown that the mineral in bone occurs as stacks of thin polycrystalline sheets ("mineral lamellae," MLs) which surround and lie between the collagen fibrils. We focus on the effect of the interface between these mineral lamellae on the mechanical properties of bone. Previous studies on bone treated with sodium hypochlorite (NaClO) to remove all organic material showed a greatly weakened mineral framework. Here, we treated femoral cortical bone with ethylenediamine (EDA), which only removes collagen, to study the effect of its removal on bone properties. We tested the degree of completion of the treatment by Raman spectroscopy and thermogravimetric analysis. When only collagen is removed, a continuous mineral structure remains and is less weakened than by NaClO treatment. Transmission electron microscopy study of finely ground particles of the EDA treated bone shows that stacks of MLs remain joined, whereas in NaClO treated bone, only isolated crystals are present. Thus, we infer that the MLs in bone are held together in stacks by an organic glue, which is destroyed by NaClO, but which survives the EDA treatment. We show that this glue may contribute to the stiffness, strength, and energy absorption of bone. Further studies are needed to discover the chemical nature of this glue. This study provides a starting point for such investigations.


Assuntos
Osso e Ossos , Minerais , Apatitas , Osso Cortical , Microscopia Eletrônica de Transmissão
13.
Comput Methods Programs Biomed ; 200: 105870, 2021 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-33280935

RESUMO

BACKGROUND AND OBJECTIVE: Finite element models built from micro-computed tomography scans have become a powerful tool to investigate the mechanical properties of trabecular bone. There are two types of solving algorithms in the finite element method: implicit and explicit. Both of these methods have been utilized to study the trabecular bone. However, an investigation comparing the results obtained using the implicit and explicit solvers is lacking. Thus, in this paper, we contrast implicit and explicit procedures by analyzing trabecular bone samples as a case study. METHODS: Micro-computed tomography-based finite element analysis of trabecular bone under a direct quasi-static compression was done using implicit and explicit methods. The differences in the predictions of mechanical properties and computational time of the two methods were studied using high-performance computing. RESULTS: Our findings indicate that the results using implicit and explicit solvers are well comparable, given that similar problem set up is carefully utilized. Also, the parallel scalability of the two methods was similar, while the explicit solver performed about five times faster than the implicit method. Along with faster performance, the explicit method utilized significantly less memory for the analysis, which shows another benefit of using an explicit solver for this case study. CONCLUSIONS: The comparison of the implicit and explicit methods for the simulation of trabecular bone samples should be highly valuable to the bone modeling community and researchers studying complex cellular and architectured materials.


Assuntos
Osso Esponjoso , Osso Esponjoso/diagnóstico por imagem , Simulação por Computador , Análise de Elementos Finitos , Estresse Mecânico , Microtomografia por Raio-X
14.
Med Eng Phys ; 84: 60-67, 2020 10.
Artigo em Inglês | MEDLINE | ID: mdl-32977923

RESUMO

Titanium implants are widely used in dental and orthopedic surgeries. Osseointegration phenomena lead to direct contact between bone tissue and the implant surface. The quality of the bone-implant interface (BII), resulting from the properties of newly formed bone, determines the implant stability. This study investigates the BII properties using a dedicated in vivo implant model consisting of a coin-shaped Ti-6Al-4V implant inserted in a rabbit femur for 10 weeks. A gap created below the implant was filled with newly formed bone tissue after healing. The properties of mature and newly formed bone tissues were compared using: i) Raman spectroscopy to assess the nanoscale compositional bone properties and ii) nanoindentation to quantify microscale elastic properties in site-matched regions. The mineral-to-matrix ratio, crystallinity (mineral size and lattice order), and the collagen cross-link ratio were significantly lower in newly formed bone tissue (e.g., a mineral-to-matrix ratio of 9.3 ± 0.5 for proline 853 cm-1) compared to mature bone (15.6 ± 1). Nanoindentation measurements gave Young's modulus of 12.8 ± 1.8 GPa for newly formed bone and 15.7 ± 2.3 GPa for mature bone. This multimodal and multiscale approach leads to a better understanding of osseointegration phenomena.


Assuntos
Interface Osso-Implante , Implantes Dentários , Animais , Osseointegração , Coelhos , Análise Espectral Raman , Propriedades de Superfície , Titânio
15.
Soft Matter ; 16(6): 1389-1403, 2020 Feb 12.
Artigo em Inglês | MEDLINE | ID: mdl-31939988

RESUMO

The current trend in the global advanced material market is expeditiously shifting towards more lightweight, multifunctional configurations, considering very recent developments in electrical aircraft, biomedical devices, and autonomous automobiles. Hence, the development of novel polymer nanocomposite materials is critical to advancing the current state-of-the-art of structural material technologies to address the pressing performance demands. Aiming at expanding the existing material design space, we have investigated crosslinkable aromatic polyester matrix nanocomposites. Aromatic polyesters, in the thermosetting form, are a prospective high-performance/high-temperature polymer technology, which is on a par with conventional epoxy-derivative resins and high-performance engineering thermoplastics in the range of their potential applications. The aromatic matrix-based thermosetting nanocomposites manifest greatly enhanced physical properties enabled by a chemistry-favored robust interfacial covalent coupling mechanism developed during the in situ polymerization reaction with various nanofiller particle configurations. Here, we provide a summary review of our recent efforts in developing this novel polymer nanocomposite material system. We highlight the chemical strategy, fabrication approach, and processing techniques developed to obtain various nanocomposite representations for structural, electrical, optical, biomedical, and tribological applications. The unique characteristic features emerging in the nanocomposite morphologies, along with their physicochemical effects on the multifunctional macroscale properties, are demonstrated. This unique matrix configuration introduces superior performance elements to polymer nanocomposite applications towards designing advanced composite materials.

16.
J Mech Behav Biomed Mater ; 90: 365-373, 2019 02.
Artigo em Inglês | MEDLINE | ID: mdl-30399565

RESUMO

Osteoprobe (ActiveLife, Santa Barbara, CA) is a novel handheld microindentation instrument designed to test bone in vivo by measuring a Bone Material Strength index (BMSi). In this paper, the Osteoprobe indentation on a cortical bone is modeled computationally to gain insights into the physical interpretation of the BMSi output. The analysis is conducted using an axisymmetric finite element model with an isotropic viscoelastic-plastic constitutive law with continuum damage. The computational model is validated by comparing it with experimental data from the literature. Experimental factors (indenter tip radius and friction coefficient between the indenter and the bone) and four mechanical properties of bone (Young's modulus, compressive yield stress, and damage and viscosity constants) are varied to study their influence on the BMSi. We find that varying the friction coefficient can proportionally change the BMSi up to 3%. The indenter tip radius is proportional to the BMSi, with a more pronounced proportional relation when it is greater than 30 µm. Young's modulus has a proportional relation with the BMSi, where decreasing it by 73% reduces the BMSi by 41%. The damage constant has an inversely proportional relation to the BMSi, where increasing it from 0.5 to 0.96 reduces the BMSi by 29%. The compressive yield stress and the viscosity constant have a close proportional relation to the BMSi, where increasing the compressive yield stress from 50 MPa to 200 MPa increases the Osteoprobe BMSi by 21%. In summary, the friction coefficient and the indenter tip radius (when smaller than 30 µm) have a small effect on BMSi. Young's modulus and damage have stronger relations with the BMSi than compressive yield stress and viscosity constant. This fundamental study provides new insights into the BMSi measurement and serves as a basis for further computational and experimental investigations on the Osteoprobe technique. Such research is needed to facilitate the embrace of this technique by the clinical community.


Assuntos
Osso e Ossos , Análise de Elementos Finitos , Teste de Materiais/instrumentação , Fenômenos Mecânicos , Microtecnologia/instrumentação , Fenômenos Biomecânicos , Fricção , Estresse Mecânico
17.
Sci Rep ; 8(1): 14869, 2018 10 05.
Artigo em Inglês | MEDLINE | ID: mdl-30291259

RESUMO

Development of porous materials consisting of polymer host matrix enriched with bioactive ceramic particles that can initiate the reproduction of cellular organisms while maintaining in vivo mechanical reliability is a long-standing challenge for synthetic bone substitutes. We present hydroxyapatite (HA) reinforced aromatic thermosetting copolyester (ATSP) matrix bionanocomposite as a potential reconfigurable bone replacement material. The nanocomposite is fabricated by solid-state mixing a matching set of precursor oligomers with biocompatible pristine HA particles. During endothermic condensation polymerization reaction, the constituent oligomers form a mechanochemically robust crosslinked aromatic backbone while incorporating the HAs into a self-generated cellular structure. The morphological analysis demonstrates near-homogenous distributions of the pristine HAs within the matrix. The HAs behave as a crack-arrester which promotes a more deformation-tolerant formation with relatively enhanced material toughness. Chain relaxation dynamics of the nanocomposite matrix during glass transition is modified via HA-induced segmental immobilization. Chemical characterization of the polymer backbone composition reveals the presence of a hydrogen-advanced covalent interfacial coupling mechanism between the HAs and ATSP matrix. This report lays the groundwork for further studies on aromatic thermosetting copolyester matrix bionanocomposites which may find applications in various artificial bone needs.

18.
Calcif Tissue Int ; 103(5): 554-566, 2018 11.
Artigo em Inglês | MEDLINE | ID: mdl-30022228

RESUMO

Bone is a biological composite material having collagen and mineral as its main constituents. In order to better understand the arrangement of the mineral phase in bone, porcine cortical bone was deproteinized using different chemical treatments. This study aims to determine the best method to remove the protein constituent while preserving the mineral component. Chemicals used were H2O2, NaOCl, NaOH, and KOH, and the efficacy of deproteinization treatments was determined by thermogravimetric analysis and Raman spectroscopy. The structure of the residual mineral parts was examined using scanning electron microscopy. X-ray diffraction was used to confirm that the mineral component was not altered by the chemical treatments. NaOCl was found to be the most effective method for deproteinization and the mineral phase was self-standing, supporting the hypothesis that bone is an interpenetrating composite. Thermogravimetric analyses and Raman spectroscopy results showed the preservation of mineral crystallinity and presence of residual organic material after all chemical treatments. A defatting step, which has not previously been used in conjunction with deproteinization to isolate the mineral phase, was also used. Finally, Raman spectroscopy demonstrated that the inclusion of a defatting procedure resulted in the removal of some but not all residual protein in the bone.


Assuntos
Osso Cortical/ultraestrutura , Técnicas de Preparação Histocitológica/métodos , Minerais/análise , Animais , Microscopia Eletrônica de Varredura , Análise Espectral Raman , Suínos , Difração de Raios X
19.
RSC Adv ; 8(9): 4946-4954, 2018 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-35539540

RESUMO

Deliberately controlled interfacial interactions between incorporated nanofiller particles and host polymer backbone chains constitute a critical element in the realm of polymer nanocomposites with tailorable multifunctional properties. We demonstrate the physicochemical effects induced by graphene nanoplatelets (GNP) of different sizes on the condensation polymerization reaction of aromatic thermosetting copolyester (ATSP) through the formation of electrically conductive percolating networks as enabled by interfacial interactions. Carboxylic acid and acetoxy-capped precursor oligomers of ATSP are solid-state mixed with chemically pristine GNP particles at various loading levels. Upon in situ endothermic condensation polymerization reaction, crosslinked backbone of the ATSP foam matrix is formed while the carbonaceous nanofillers are incorporated into the polymer network via covalent conjugation with functional end-groups of the oligomers. The controlled GNP size promotes different electrical percolation thresholds and ultimate electrical conductivities. Microstructural analysis demonstrates GNP distributions in the matrix as well as morphological modifications induced by the formation of conductive percolating GNP networks. Cure characteristics reveal the thermochemical changes prompted in the polymerization processes for GNP content above the requirement for percolation formation. Chemical spectroscopy of the ATSP nanocomposite morphology exhibits the formation of a robust interfacial coupling mechanism between the GNPs and ATSP backbone. The findings here may guide the developmental efforts of nanocomposites through better identifying roles of the morphology and content of nanofillers in polymerization processes.

20.
J Vis Exp ; (127)2017 09 14.
Artigo em Inglês | MEDLINE | ID: mdl-28994795

RESUMO

This protocol describes the method using digital image correlation to estimate cortical strain from high speed video images of the cadaveric femoral surface obtained from mechanical testing. This optical method requires a texture of many contrasting fiduciary marks on a solid white background for accurate tracking of surface deformation as loading is applied to the specimen. Immediately prior to testing, the surface of interest in the camera view is painted with a water-based white primer and allowed to dry for several minutes. Then, a black paint is speckled carefully over the white background with special consideration for the even size and shape of the droplets. Illumination is carefully designed and set such that there is optimal contrast of these marks while minimizing reflections through the use of filters. Images were obtained through high speed video capture at up to 12,000 frames/s. The key images prior to and including the fracture event are extracted and deformations are estimated between successive frames in carefully sized interrogation windows over a specified region of interest. These deformations are then used to compute surface strain temporally during the fracture test. The strain data is very useful for identifying fracture initiation within the femur, and for eventual validation of proximal femur fracture strength models derived from Quantitative Computed Tomography-based Finite Element Analysis (QCT/FEA).


Assuntos
Fraturas do Fêmur/diagnóstico por imagem , Fêmur/diagnóstico por imagem , Fraturas do Fêmur/patologia , Fêmur/patologia , Humanos , Tomografia Computadorizada por Raios X/métodos
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