999 resultados para Método físico de controle


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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Neste trabalho é proposta uma metodologia de rastreamento de sinais e rejeição de distúrbios aplicada a sistemas não-lineares. Para o projeto do sistema de rastreamento, projeta-se os controladores fuzzy M(a) e N(a) que minimizam o limitante superior da norma H∞ entre o sinal de referência r(t) e o sinal de erro de rastreamento e(t), sendo e(t) a diferença entre a entrada de referência e a saída do sistema z(t). No método de rejeição de distúrbio utiliza-se a realimentação dinâmica da saída através de um controlador fuzzy Kc(a) que minimiza o limitante superior da norma H∞ entre o sinal de entrada exógena w(t) e o sinal de saída z(t). O procedimento de projeto proposto considera as não-linearidades da planta através dos modelos fuzzy Takagi-Sugeno. Os métodos são equacionados utilizando-se inequações matriciais lineares (LMIs), que quando factíveis, podem ser facilmente solucionados por algoritmos de convergência polinomial. Por fim, um exemplo ilustra a viabilidade da metodologia proposta.

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Hybrid systems formed from polymers and transition metals have now their physical and chemical properties extensively investigated for use in electronic devices. In this work, Titanium Dioxide (TiO2) from the precursor of titanium tetrabutoxide and the composite system Poly(Ethylene Glycol)-Titanium Dioxide (TiO2-PEG) were synthesized by sol-gel method. The PEG as acquired and TiO2 and composites powders were analyzed by X-Ray Diffraction (XRD), Spectroscopy in the Infrared region with Fourier transform (IRFT), Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and Electrochemical Impedance Spectroscopy (EIS). In the XRD analysis were observed in the TiO2 crystal faces of one of its polymorphs - anatase phase, crystal planes in Poly (Ethylene Glycol) with considerable intensity and in the composite systems the mixture of crystal faces of their precursors isolated and reduction of crystallinity. The TG / DTG suggested increasing the thermal instability of PEG in the composite powders as TiO2 is incorporated into the system. Spectral analysis presented in the infrared overlapping bands for the polymer and metal oxide, reducing the intensity of symmetric stretching of ligand groups in the main chain polymer and angular deformations; were observed using SEM micrographs of the morphological changes suffered by composite systems with the variation of the oxide concentration. Analyses by impedance spectroscopy indicated that the increased conductivity in composite occurs in line with the addition of the metal oxide concentration in the composite system

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Were synthesized systems Ni0,5Zn0,5Fe2O4, i0,2Zn0,5Mn0,3Fe2O4, Mn0,5Zn0,5Fe2O4, Ni0,5Mg0,5Fe2O4, Ni0,2Cu0,3Zn0,5Fe2O4 and Ni0,2Cu0,3Zn0,5Mg0,08Fe2O4, the precursors citrate method. The decomposition of the precursors was studied by thermogravimetric analysis and spectroscopy in the infrared region, the temperature of 350°C/3h. The evolution of the phases formed after calcinations at 350, 500, 900 and 1100ºC/3h was accompanied by X-ray diffraction using the Rietveld refinement to better identify the structures formed. The materials were also analyzed by scanning electron microscopy, magnetic measurements and analysis of the reflectivity of the material. The samples calcined at different temperatures showed an increase of crystallinity with increasing calcination temperature, verifying that for some compositions at temperatures above 500°C precipitates of second phase such as hematite and CuO. The compositions of manganese present in the structure diffusion processes slower due to the ionic radius of manganese is greater than for other ions substitutes, a fact that delays the stabilization of spinel structure and promotes the precipitation of second phase. The compositions presented with copper precipitation CuO phase at a temperature of 900 and 1100ºC/3h This occurs according to the literature because the concentration of copper in the structure is greater than 0.25 mol%. The magnetic measurements revealed features of a soft ferrimagnetic material, resulting in better magnetic properties for the NiZn ferrite and NiCuZnMg at high temperatures. The reflectivity measurements showed greater absorption of electromagnetic radiation in the microwave band for the samples calcined at 1100ºC/3h, which has higher crystallite size and consequently the formation of multi-domain, increasing the magnetization of the material. The results of absorption agreed with the magnetic measurements, indicating among the ferrites studied, those of NiZn and NiCuZnMg as better absorbing the incident radiation.

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The study of polymer blends has been an alternative method in the search field of new materials for obtaining materials with improved properties. In this work blends of poly(methyl methacrylate) (PMMA) and poly(ethylene oxide) (PEO) doped with titanium dioxide (TiO2) were studied. The PEO is a polymer semicrystalline structure varying between, 70 and 84% crystallinity, while the PMMA exhibits behavior amorphous in their structure. The use of TiO2 is related to corrosion-resistant of titanium as well as good heat transfer and other characteristics. The study of these polymer blends doped TiO2 gives the properties junction organic (polymer) and inorganic (oxide) which leads to modification of the properties of the resultant material. The blends were doped TiO2 (POE/PMMA/TiO2) in different proportions of the PMMA with the PEO and TiO2 fixed. The ratios were: 90/10/0,1; 85/15/0, 1; 80/20/0,1, 75/25/0,1 and 70/30/0,1. The resulting material was obtained in powder form and being characterized by Fourier Transformed Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Electrochemical Impedance Spectroscopy (EIS). The infrared spectra (IR) for the blends in different ratios showed a band at 1744 cm-1, characteristic of the C=O stretching, which increases in intensity with increasing PMMA composition, while in the spectrum of pure PEO this band is absent. This may suggest that the interaction is occurring between the polymers. In the micrographs of the blends also observed change in their surfaces with variation of the composition of PMMA, contributing to the change of the electrical properties of the material. The EIS data showed that the material exhibited conductivity of the order of 10-6 S.cm-1. The blend in the ratio B2(85/15/0, 1) showed better conductivity, σ = 1.56 x 10-6 S.cm-1. It was observed that the diffusion coefficient for the blends, B5(70/30/0, 1) was the largest, 1.07 x 10-6 m2.s-1. The XRD data showing that, with the variation in the composition of the PMMA blend crystallinity of the material is decreased reaching a minimum B3(80/20/0,1), and then increases again. Thermal analysis suggests that blends made from the material obtained can be applied at room temperature

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Different compositions of Ni0,5-xCuxZn0,5Fe2O4 and Ni0,5-xCoxZn0,5Fe2O4 0 ≤ x ≤ 0.3 were synthesized ferrite y the citrate precursor method. The stoichiometric compositions were calcined in air at 350°C and then pressed into pellets and toroids. The pressed samples were sintered at temperatures of 1000, 1050 and 1100°C/3h in air control at the speed of heating and cooling. The calcined powders were characterized by XRD, TGA / DTG, FTIR, SEM and vibrating sample magnetometry (VSM) and the sintered samples by XRD, SEM, MAV, density and measurements of permeability and magnetic losses. There was pure phase formation ferrimagnetism applied at all temperatures except for A-I composition at all sintering temperatures and A-II only at a temperature of 1100°C. Crystallite sizes were obtained by Rietveld analysis, nanometer size from 11 to 20 nm for the calcined powders. For SEM, the sintered samples showed grain size between 1 and 10 micrometers. Bulk density (ρ) of sintered material presented to the Families almost linear behavior with increasing temperature and a tendency to decrease with increasing concentration of copper, different behavior of the B Family, where the increase in temperature decreased the density. The magnetic measurements revealed the powder characteristics of a soft ferrimagnetic material. Two processes of magnetization were considered, the superparamagnetism at low temperatures (350°C) and the formation of magnetic domains at higher temperatures. Obtaining the best parameters for P and B-II magnetic ferrites at high temperatures. The sintered material at 1000°C showed a relative permeability (μ) from 50 to 800 for the A Family and from 10 to 600 for the B Family. The samples sintered at 1100°C, B Family showed a variation from 10 to 1000 and the magnetic loss (tan δ) of A and B Families, around of 1. The frequency response of the toroidal core is in the range of 0.3 kHz. Several factors contribute to the behavior of microstructure considering the quantities μ and tan δ, such as the grain size, inter-and intragranular porosity, amount of grain boundary and the aspects of the dynamics of domain walls at high frequencies.

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The pulps are products that add economic value enjoy the fruits of the surplus productions of the same. Have good market acceptance because of its practicality and diversity of flavors available year round. In order to assess the quality of the fruit pulp through the physical and chemical parameters and the characteristics of manufacturing industry, we analyzed 36 samples of frozen fruit pulp of three brands marketed in RIO Grande do Norte, 14 brand A, 12 of 10 brand B and brand C, which corresponded to 14 different flavors, of which 10 have identity Standards and Quality (ISQ S) established by the Ministério da Agricultura, Pecuária e Abastecimento (MAPA), totaling 27 samples with ISQ s. We conducted the following physicalchemical analyzes on samples of fruit pulp: Total solids, total soluble solids, pH, titratable acidity, total sugars and the determination of ascorbic acid. The percentage of failure for each parameter evaluated was 37, 04% in total soluble solids, 22,22% for total solids and titratable acidity, 7,40% in relation to pH. The total sugars were within the requirements demanded by the MAPA and ascorbic acid content, determined only in the pulp of acerola and cashew, presented a non compliance in the pulp of brand B. The percentage of failures of the pulps with ISQ S was 59% with brand A, B and C accounted for 3,70%, 33,33% and 22,22% respectively. The pulps which have no established atandards such as pineapple pulp, showed similar values between brands and literature data unlike the pulp of plum, jackfruit and tamarind which diverged greatly in parameters such as total solids and total soluble solids. The study demonstrates the need for greater quality control by the producers with respect to raw materials, processing, packing, stored and the importance of ISQ S to establish the flavors have not yet covered by existing legislation, but already highly commercialized

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A new self-sustainable film was prepared through the sol-gel modified method, previously employed in our research group; sodium alginate was used as the polymer matrix, along with plasticizer glycerol, doped with titanium dioxide (TiO2) and tungsten trioxide (WO3). By varying WO3 concentration (0,8, 1,6, 2,4 and 3,2 μmol) and keeping TiO2 concentration constant (059 mmol), it was possible to study the contribution of these oxides on the obtained films morphological and electrical properties. Self-sustainable films have analyzed by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XDR), Scanning Electron Microscope (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and Electrochemical Impedance Spectroscopy (EIS). By the IR specters, it was possible identify the TiO2, and posteriorly WO3, addition has provided dislocation of alginate characteristics bands to smaller vibrations frequencies indicating an electrostatic interaction between the oxides and the polymer matrix. Diffractograms show predominance of the amorphous phase in the films. SEM, along with EDX, analysis revealed self-sustainable films showed surface with no cracks and relative dispersion of the oxides throughout the polymer matrix. From Impedance analysis, it was observe increasing WO3 concentration to 2,4 μmol provided a reduction of films resistive properties and consequent improvement of conductive properties

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Catalytic processes are widely present in everyday life. This results in large number of studies seeking materials that may combine the low cost catalytic efficiency. Based on this assumption, the clays have long been used as catalysts, with its huge availability, diversity and possibility of improving their properties from structural changes, primarily responsible for this great use. Among the natural clays, vermiculite due to their characteristic properties (high cation exchange capacity and expansion), is suitable for various applications including as catalysts and catalyst supports. In this work, the acid leaching of clay vermiculite was performed, coming from Santa Luzia-PB, with nitric acid (2, 3 and 4 mol / L) and subsequent calcination of the materials obtained. The materials were named as Vx/400, where x is the acid concentration employed and 400 used in calcination temperature. The effectiveness of changes made was determined by XRD techniques, FT-IR, EDS, TG/DTG, nitrogen physisorption and DTP of n-butylamine. Acid leaching has improved some properties of the clay - specific area and acidity - but the control of the acid concentration used is of vital importance, since the highest concentration caused the partial destruction of vermiculite entailing a decline in their properties. For analysis of the catalytic activity of the modified clay was made a comparative study with the SBA -15 mesoporous materials, synthesized via hydrothermal method, using the pyrolysis of low density polyethylene (LDPE). The results showed that the acid plays a fundamental role in the conversion of the polymer into smaller molecules, the material V3/400 was more selective for the source monomer (ethylene) due to their increased acidity, which promotes more breaks bonds in the polymeric chain, while materials and V0/400 V2/400, lower acidity, showed higher selectivity to light hydrocarbons, the range of fuel (41.96 and 41.23%, respectively), due to less breakage and secondary condensation reactions chains; already V4/400 SBA-15/550 and resulted in lower percentages of light hydrocarbons and the partial destruction of the structure and low acidity, respectively, responsible for the inefficiency of materials

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In this study five compositions were synthesized zirconia doped with cerium and neodymium ions in the system Ce10-xNdx Zr90O2 with 0,5 ≤ x ≤ 4,0 using the Pechini method. The powders were characterized by thermogravimetric analysis, differential thermal analysis, infrared spectroscopy and X-ray diffraction, with application of Rietveld refinement of the calcination temperatures of 350ºC/3h and 30 minutes at 900ºC/3h. All compositions stabilized with a mixture of cubic and tetragonal phase zirconia. The samples were pressed into bars and sintered at 1500°C/3h and 1500°C/6h, being characterized by Xray diffraction, with application of the Rietveld refinement, density and porosity using Archimedes method, scanning electron microscopy and resistance the three point bending. It has been observed the increase in strength with increasing sintering temperature for the compositions x = 2,0 and x = 4,0. For x = 2,0 the main phase was the cubic with 92,56% with crystallite size of 0,56 μm, density and porosity of 96,82% from 1,36%. For x = 4,0 was a mixture of cubic and tetragonal phase with 21% and 37,98%, respectively. The crystallite size was 54,21 nm and 49,64 nm with a density porosity of 97,45% and 1,32% respectively. In the analysis of the fracture surface was observed a greater amount of grain fracture intragranular type, which contribute to increase the mechanical strength of the ceramic. Increased addition of the neodymium ion in the crystal lattice of the zirconium showed a nearly linear behavior with increasing mechanical strength of the zirconia ceramic. Was obtained a bending resistance of 537 ± 38 MPa for the composition x = 2,0 predominantly attributed to cubic phase with 92,56%

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Soil contamination by pesticides is an environmental problem that needs to be monitored and avoided. However, the lack of fast, accurate and low cost analytical methods for discovering residual pesticide in complex matrices, such as soil, is a problem still unresolved. This problem needs to be solved before we are able to assess the quality of environmental samples. The intensive use of pesticides has increased since the 60s, because the dependence of their use, causing biological imbalances and promoting resistance and recurrence of high populations of pests and pathogens (upwelling). This has contributed to the appearance of new pests that were previously under natural control. To develop analytical methods that are able to quantify residues pesticide in complex environment. It is still a challenge for many laboratories. The integration of two analytical methods one ecotoxicological and another chemical demonstrates the potential for environmental analysis of methamidophos. The aim of this study was to evaluate an ecotoxicological method as "screening" analytical methamidophos in the soil and perform analytical confirmation in the samples of the concentration of the analyte by chemical method LC-MS/MS In this work we tested two soils: a clayey and sandy, both in contact with the kinetic methamidophos model followed pseudo-second order. The clay soil showed higher absorption of methamidophos and followed the Freundlich model, while the sandy, the Langmuir model. The chemical method was validated LC-MS/MS satisfactory, showing all parameters of linearity, range, precision, accuracy, and sensitivity adequate. In chronic ecotoxicological tests with C. dubia, the NOEC was 4.93 and 3.24 for ng L-1 of methamidophos to elutriate assays of sandy and clay soils, respectively. The method for ecotoxicological levels was more sensitive than LC-MS/MS detection of methamidophos, loamy and sandy soils. However, decreasing the concentration of the standard for analytical methamidophos and adjusting for the validation conditions chemical acquires a limit of quantification (LOQ) in ng L-1, consistent with the provisions of ecotoxicological test. The methods described should be used as an analytical tool for methamidophos in soil, and the ecotoxicological analysis can be used as a "screening" and LC-MS/MS as confirmatory analysis of the analyte molecule, confirming the objectives of this work

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Chitosan is a biopolymer derived from the shells of crustaceans, biodegradable, inexpensive and renewable with important physical and chemical properties. Moreover, the different modifications possible in its chemical structure generate new properties, making it an attractive polysaccharide owing to its range of potential applications. Polymers have been used in oil production operations. However, growing concern over environmental constraints has prompted oil industry to search for environmentally sustainable materials. As such, this study sought to obtain chitosan derivatives grafted with hydrophilic (poly(ethylene glycol), mPEG) and/or hydrophobic groups (n-dodecyl) via a simple (one-pot) method and evaluate their physicochemical properties as a function of varying pH using rheology, small-angle Xray scattering (SAXS), dynamic light scattering (DLS) and zeta potential. The chitosan derivatives were prepared using reductive alkylation under mild reaction conditions and the chemical structure of the polymers was characterized by nuclear magnetic resonance (1H NMR) and CHN elemental analysis. Considering a constant mPEG/Chitosan molar ratio on modification of chitosan, the solubility of the polymer across a wide pH range (acidic, neutral and basic) could only be improved when some of the amino groups were submitted to reacetylation using the one-pot method. Under these conditions, solubility is maintained even with the simultaneous insertion of n-dodecyl. On the other hand, the solubility of derivatives obtained only through mPEG incorporation using the traditional methodology, or with the ndodecyl group, was similar to that of its precursor. The hydrophilic group promoted decreased viscosity of the polymer solutions at 10 g/L in acid medium. However, at basic pH, both viscosity and thermal stability increased, as well as exhibited a pronounced pseudoplastic behavior, suggesting strong intermolecular associations in the alkaline medium. The SAXS results showed a polyelectrolyte behavior with the decrease in pH for the polymer systems. DLS analyses revealed that although the dilute polymer solutions at 1 g/L and pH 3 exhibited a high density of protonated amino groups along the polymer chain, the high degree of charge contributed significantly to aggregation, promoting increased particle size with the decrease in pH. Furthermore, the hydrophobic group also contributed to increasing the size of aggregates in solution at pH 3, whereas the hydrophilic group helped reduce their size across the entire pH range. Nevertheless, the nature of aggregation was dependent on the pH of the medium. Zeta potential results indicated that its values do not depend solely on the surface charge of the particle, but are also dependent on the net charge of the medium. In this study, water soluble associative polymers exhibit properties that can be of great interest in the petroleum industry

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The development of more selective and sensitive analytical methods is of great importance in different areas of knowledge, covering, for example, food, biotechnological, environmental and pharmaceutical sectors. The study aimed to employ the technique electroanalytical differential pulse voltammetry (DPV) as an innovative and promising alternative for identification and quantification of organic compounds. The organic compounds were investigated in this study oxalic acid (OA) and folic acid (FA). The electrochemical oxidation of oxalic acid has been extensively studied as a model reaction in the boundary between the organic and inorganic electrochemistry. Since the AF, an essential vitamin for cell multiplication in all tissues, which is essential for DNA synthesis. The AF has been investigated using analytical techniques, liquid chromatography and molecular absorption spectrophotometry. The results obtained during the experimental procedure indicated that the process of electrochemical oxidation of oxalic acid is strongly dependent on the nature of the anode material and the oxidation mechanism, which affects their detection. Efficient removal was observed in Ti/PbO2 anodes, graphite, BDD and Pt 90, 85, 80 and 78% respectively. It was also shown that the DPV employing glassy carbon electrode offers a fast, simple, reliable and economical way to determine the AO during the process of electrochemical oxidation. Furthermore, electroanalytical methods are more expensive than commonly used chromatographic analysis and other instrumental methods involving toxic reagents and higher cost. Compared with the classical method of titration and DPV could be a good fit, confidence intervals and detection limits confirming the applicability of electroanalytical technique for monitoring the degradation of oxalic acid. For the study of AF was investigated the electrocatalytic activity of the carbon paste electrode for identification and quantification in pharmaceutical formulations by applying the DPV. The results obtained during the experimental procedure showed an irreversible oxidation peak at 9.1 V characteristic of FA. The carbon paste sensor showed low detection limit of 5.683×10−8 mol L-1 reducing matrix effects. The spectrophotometric analysis showed lower concentrations of HF compared with those obtained by HPLC and DPV. The levels of AF were obtained according to the methodology proposed by the Brazilian Pharmacopoeia. The electroanalytical method (DPV) proposed is cheaper than GC analysis commonly used by the pharmaceutical industry. The results demonstrated the potential of these electroanalytical techniques for future applications in environmental, chemical and biological sensors

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the institutionalized elderly presents for being more fragile a lot of body balance s changes, which can induce falls and health frailty. One of the consequences of it is the appearance of dizziness, vestibular or not. This study aims to identify the risk factors related to dizziness in institutionalized elderly, with and without vestibular disorders, in the city of Natal-RN. Method: a case-control study realized in 12 regulated by Health Surveillance Long Term Care Institutions for the elderly in Natal-RN. Elected seniors with good cognitive level and able to walk, totaling 115 individuals, and of these, 102 were selected according to the presence of dizziness in the last year (n = 51) and their controls (n = 51), paired by sex and age. The 51 elderly patients with dizziness were divided into 3 groups case: case one, for elderly with dizziness and without vestibulopathy (n=38); case two, for elderly with dizziness and vestibulopathy (n=13) and case three, for all the seniors with dizziness, or added to the case 1 case 2 (n=51). The 51 seniors who served as controls were also divided into three groups, according to the number of individuals of each case: control 1, n = 38, control 2, n = 13 control and 3 (sum of 1 control with control 2), n = 51. As possible risk factors were analyzed variables related to characteristics of the institution, to the habits of life of older people and those concerned with the health of the elderly. For statistical analysis, we used the chi-square or Fisher exact test for a significance level of 5% and calculating the association magnitude between variables by measuring the Odds Ratio. Results: as risk factors for dizziness without vestibular disorders were found the presence of hypertension and cardiovascular disease, as well as the presence of three or more disorders for elderly and use of gastric protector drugs. For the elderly group from case two were found no associated risk factor. For elderly patients with dizziness in the case group three, we observed the same risk factors found for the elderly in the case group one, plus the presence of osteoarthritis pathology, which was also significant for this group. Conclusion: dizziness in institutionalized elderly is associated with systemic common diseases in this age group and the vestibulopathy presents itself as pathology on an isolated way, not being possible, with our data, associate it with non-risk factors

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The objective of this research was to evaluate the passivity and strain induced in infrastructures screwed on abutments, made by CAD/CAM technology, and to compare these samples with parts manufactured by conventional casting. Using CAD/CAM technology, 4 samples were made from zirconia (Zircad) and 4 samples were manufactured from cobaltchrome (CoCrcad). The control groups were 4 specimens of cobalt-chrome, made by onepiece casting (CoCrci), for a total of 12 infrastructures. To evaluate the passivity, the infraestructures were installed on the abutments. One end was tightened and the vertical gap between the infrastructure and the prosthetic abutment was measured with scanning electron microscopy (250×). The mean strain in these infrastructures was analyzed via the photoelasticity test. A significant difference (p = 0.000) in passivity was observed between the control (CoCrci) and sample groups (CoCrcad and CoCrci). CoCrcad exhibited the best value of passivity (48.76 ± 13.45 μm) and CoCrci the worst (187.55 ± 103.63 μm), Zircad presented an intermediate value (103.81 ± 43.15 μm). When compared to the other groups, CoCrci showed the highest mean strain around the implants (17.19 ± 7.22 kPa). It was concluded that the zirconia infrastructure made by CAD / CAM showed a higher vertical marginal misfit than those made in cobalt-chromium alloy with the same methodology, however, the tension generated in the implants was similar. The CAD/CAM technology is more accurate for passivity and mean strain of infrastructure screwed on abutments than conventional manufacturing techniques