763 resultados para Tribological behaviour
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The present thesis focuses on characterisation of microstructure and the resulting mechanical and tribological properties of CVD and PVD coatings used in metal cutting applications. These thin and hard coatings are designed to improve the tribological performance of cutting tools which in metal cutting operations may result in improved cutting performance, lower energy consumption, lower production costs and lower impact on the environment. In order to increase the understanding of the tribological behaviour of the coating systems a number of friction and wear tests have been performed and evaluated by post-test microscopy and surface analysis. Much of the work has focused on coating cohesive and adhesive strength, surface fatigue resistance, abrasive wear resistance and friction and wear behaviour under sliding contact and metal cutting conditions. The results show that the CVD deposition of accurate crystallographic phases, e.g. α-Al2O3 rather than κ-Al2O3, textures and multilayer structures can increase the wear resistance of Al2O3. However, the characteristics of the interfaces, e.g. topography as well as interfacial porosity, have a strong impact on coating adhesion and consequently on the resulting properties. Through the deposition of well designed bonding and template layer structures the above problems may be eliminated. Also, the presence of macro-particles in PVD coatings may have a significant impact on the interfacial adhesive strength, increasing the tendency to coating spalling and lowering the surface fatigue resistance, as well as increasing the friction in sliding contacts. Finally, the CVD-Al2O3 coating topography influences the contact conditions in sliding as well as in metal cutting. In summary, the work illuminates the importance of understanding the relationships between deposition process parameters, composition and microstructure, resulting properties and tribological performance of CVD and PVD coatings and how this knowledge can be used to develop the coating materials of tomorrow.
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The main purpose of this work is to present and to interpret the change of structure and physical properties of tantalum oxynitride (TaNxOy) thin films, produced by dc reactive magnetron sputtering, by varying the processing parameters. A set of TaNxOy films was prepared by varying the reactive gases flow rate, using a N2/O2 gas mixture with a concentration ratio of 17:3. The different films, obtained by this process, exhibited significant differences. The obtained composition and the interpretation of X-ray diffraction results, shows that, depending on the partial pressure of the reactive gases, the films are: essentially dark grey metallic, when the atomic ratio (N + O)/Ta < 0.1, evidencing a tetragonal β-Ta structure; grey-brownish, when 0.1 < (N + O)/Ta < 1, exhibiting a face-centred cubic (fcc) TaN-like structure; and transparent oxide-type, when (N + O)/Ta > 1, evidencing the existence of Ta2O5, but with an amorphous structure. These transparent films exhibit refractive indexes, in the visible region, always higher than 2.0. The wear resistance of the films is relatively good. The best behaviour was obtained for the films with (N + O)/Ta ≈ 0.5 and (N + O)/Ta ≈ 1.3.
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Dissertação de mestrado integrado em Engenharia de Materiais
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Dissertação de mestrado integrado em Engenharia Biomédica
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Dissertação de mestrado integrado em Engenharia de Materiais
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Los recubrimientos lubricantes sólidos son requeridos para reducir la fricción y prevenir el desgaste en componentes que operan a altas temperaturas o en vacío (vehículos espaciales, industria química, motores diésel, turbinas aeronáuticas y de generación de energía…). Los lubricantes líquidos pierden sus características cuando las condiciones de presión, temperatura o ambientales son severas (oxidación, inestabilidad térmica, volatilidad,…), por ejemplo los aceites minerales convencionales se descomponen a temperaturas próximas a 200 ºC. Por tanto, la única manera de poder conseguir una adecuada lubricación a temperaturas extremas es por medio de sólidos, que cada vez más, se aplican en forma de recubrimientos. Estos recubrimientos podrían ser empleados en componentes de vehículos espaciales reutilizables, donde se pueden alcanzar, en la reentrada en la atmósfera, temperaturas de 700 ºC (bisagras, rodamientos, articulaciones y zonas de sellado en las superficies de control, y rodamientos de las turbobombas y las cajas de engranajes). Dichos recubrimientos también deberían ser capaces de proporcionar una lubricación efectiva a bajas temperaturas para las operaciones en tierra, para las operaciones de arranque en frío, incluso en el espacio. El conjunto de requisitos que tendrían que satisfacer las capas tribológicas relacionadas con estas condiciones extremas es muy diverso, lo que hace que el concepto de capas tipo composite (aquéllas constituidas por varios componentes) sea, en principio, muy adecuado para estas aplicaciones. Recubrimientos composite proyectados térmicamente constituidos por una matriz dura y conteniendo lubricantes sólidos pueden ser una buena solución desde el punto de vista tribológico. El “Lewis Research Centre” de la NASA ha estado desarrollando recubrimientos autolubricantes tipo composite, constituidos por la combinación de materiales duros como el carburo de cromo, junto con lubricantes sólidos como plata o la eutéctica de fluoruros de calcio y bario, en una matriz de NiCr, para su uso en aplicaciones terrestres a alta temperatura. Estos recubrimientos han sido aplicados mediante proyección térmica, siendo denominados como series PS100, PS200, PS300 y PS400, reduciendo de forma significativa el coeficiente de fricción y mejorando la resistencia al desgaste en un amplio margen de temperaturas. Otra nueva familia de materiales con comportamiento tribológico prometedor son las aleaciones cuasicristalinas (QC). Presentan características muy atractivas: alta dureza, baja fricción, alto límite elástico de compresión... Son muy frágiles como materiales másicos, por lo que se intentan aplicar en forma de recubrimientos. Se pueden depositar mediante proyección térmica. Algunos de estos materiales cuasicristalinos, como AlCoFeCr, poseen coeficientes de dilatación próximos al de los materiales metálicos, alta estabilidad térmica, baja conductividad térmica y una elevada resistencia a la oxidación y a la corrosión en caliente. En esta tesis se han desarrollado recubrimientos tipo composite conteniendo cuasicristales como componente antidesgaste, NiCr como componente tenaz, y Ag y la eutéctica de BaF2-CaF2, como lubricantes sólidos. Estos recubrimientos han sido depositados con diferentes composiciones (denominadas TH100, TH103, TH200, TH400, TH600…) mediante distintos procesos de proyección térmica: plasma en aire (PS), plasma en baja presión (LPPS) y combustión a alta velocidad (HVOF). Los recubrimientos se han generado sobre el sustrato X-750, una superaleación base níquel, endurecible por precipitación, con muy buena resistencia mecánica y a la oxidación hasta temperaturas de 870 ºC y, además, es empleada en aplicaciones aeroespaciales e industriales. Los recubrimientos han sido caracterizados microestructuralmente en INTA (Instituto Nacional de Técnica Aeroespacial), mediante SEM-EDS (Scanning Electronic Microscopy-Energy Dispersive Spectroscopy) y XRD (X-Ray Diffraction), y tribológicamente mediante medidas de microdureza y ensayos en tribómetro POD (Pin On Disc) para determinar los coeficientes de fricción y de desgaste. Los recubrimientos han sido ensayados tribológicamente a alta temperatura en INTA y en vacío en AMTTARC (Aerospace and Space Materials Technology Testhouse – Austrian Research Centres), en Seibersdorf (Austria). Se ha estudiado la influencia de la carga normal aplicada, la velocidad lineal y el material del pin. De entre las diferentes series de recubrimientos cuasicristalinos tipo composite desarrolladas, dos de ellas, TH100 y TH103 han presentado una excelente calidad microestructural (baja porosidad, distribución uniforme de fases…) y se han mostrado como excelentes recubrimientos antidesgaste. Sin embargo, estas capas presentan un pobre comportamiento como autolubricantes a temperatura ambiente, aunque mejoran mucho a alta temperatura o en vacío. Los resultados del trabajo presentado en esta tesis han proporcionado nuevo conocimiento respecto al comportamiento tribológico de recubrimientos autolubricantes cuasicristalinos tipo composite depositados por proyección térmica. Sin embargo, dichos resultados, aunque son muy prometedores, no han puesto de manifiesto el adecuado comportamiento autolubricante que se pretendía y, además, como ocurre en cualquier trabajo de investigación, durante el desarrollo del mismo siempre aparecen nuevas dudas por resolver. Se proponen nuevas líneas de trabajo futuro que complementen los resultados obtenidos y que puedan encaminar hacia la obtención de un recubrimiento que mejore su comportamiento autolubricante. ABSTRACT Solid lubricant coatings are required to reduce friction and prevent wear in components that operate at high temperatures or under vacuum (space vehicles, chemical industry, diesel engines, power generation turbines and aeronautical turbines, for instance). In these cases neither greases nor liquid lubricants can be employed and the only practicable approach to lubrication in such conditions is by means of solids. These are increasingly applied in the form of coatings which should exhibit low shear strength, whilst maintaining their chemical stability at extremes temperatures and in the space environment. In the space field, these coatings would be employed in re-usable space plane applications, such as elevon hinges, where temperatures of 700 ºC are reached during re-entry into the Earth’s atmosphere. These coatings should also be capable of providing effective lubrication at lower temperatures since “cold start” operation may be necessary, even in the space environment. The diverse and sometimes conflictive requirements in high temperature and space-related tribological coatings make the concept of composite coatings highly suitable for these applications. Thermal-sprayed composites containing solid lubricants in a hard matrix perform well tribologically. NASA‘s Lewis Research Centre had developed self-lubricating composite coatings for terrestrial use, comprising hard materials like chromium carbide as well as solid lubricant additives such as silver and BaF2-CaF2 eutectic on a Ni-Cr matrix. These coatings series, named PS100, PS200, PS300 and PS400, are applied by thermal spray and significantly reduce friction coefficients, improving wear resistance over a wide temperature range. Quasicrystalline alloys (QC) constitute a new family of materials with promising tribological behaviour. Some QC materials exhibit a combination of adequate antifriction properties: low friction coefficient, high hardness and high yield strength under compression, and can be easily produced as coatings on top of metallic and non-metallic materials. Among these QC alloys, AlCoFeCr has high hardness (700 HV0.1), a thermal expansion coefficient close to that of metals, high thermal stability, low thermal conductivity and good oxidation and hot corrosion resistance. However most QC materials have the disadvantage of being very brittle. In order to take advantage of the excellent tribological properties of QCs, thick composite lubricant coatings were prepared containing them as the hard phase for wear resistance, Ag and BaF2-CaF2 eutectic as lubricating materials and NiCr as the tough component. These coatings were deposited in different composition mixtures (named TH100, TH103, TH200, TH400, TH600…) by different thermal spray processes: air plasma spray (PS), low pressure plasma spray (LPPS) and high velocity oxy-fuel (HVOF), on X-750 substrates. X-750 is an age-hardenable nickel-base superalloy with very good strength and a good resistance to oxidising combustion gas environments at temperatures up to about 870 ºC and it is widely used in aerospace and industrial applications. Coatings have been characterized microstructurally, at INTA (National Institute for Aerospace Technology), by means of SEM-EDS (Scanning Electronic Microscopy- Energy Dispersive Spectroscopy) and XRD (X-Ray Diffraction), and tribologically by microhardness measurements and pin-on-disc testing to determine friction coefficients as well as wear resistance. The coatings were tested tribologically at high temperature at INTA and under vacuum at AMTT-ARC (Aerospace and Space Materials Technology Testhouse – Austrian Research Centres), in Seibersdorf (Austria). Different loads, linear speeds and pin materials were studied. TH100 and TH103 QC alloy matrix composite coatings were deposited by HVOF with excellent microstructural quality (low porosity, uniform phase distribution) and showed to be excellent wear resistant coatings. However these QC alloy matrix composite coatings are poor as a self-lubricant at room temperature but much better at high temperature or in vacuum. The results from the work performed within the scope of this thesis have provided new knowledge concerning the tribological behavior of self-lubricating quasicrystalline composite coatings deposited by thermal spraying. Although these results are very promising, they have not shown an adequate self-lubricating behavior as was intended, and also, as in any research, the results have in addition raised new questions. Future work is suggested to complement the results of this thesis in order to improve the selflubricating behaviour of the coatings.
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Thin hard coatings on components and tools are used increasingly due to the rapid development in deposition techniques, tribological performance and application skills. The residual stresses in a coated surface are crucial for its tribological performance. Compressive residual stresses in PVD deposited TiN and DLC coatings were measured to be in the range of 0.03-4 GPa on steel substrate and 0.1-1.3 GPa on silicon. MoS(2) coatings had tensional stresses in the range of 0.8-1.3 on steel and 0.16 GPa compressive stresses on silicon. The fracture pattern of coatings deposited on steel substrate were analysed both in bend testing and scratch testing. A micro-scale finite element method (FEM) modelling and stress simulation of a 2 mu m TiN-coated steel surface was carried out and showed a reduction of the generated tensile buckling stresses in front of the sliding tip when compressive residual stresses of 1 GPa were included in the model. However, this reduction is not similarly observed in the scratch groove behind the tip, possibly due to sliding contact-induced stress relaxation. Scratch and bending tests allowed calculation of the fracture toughness of the three coated surfaces, based on both empirical crack pattern observations and FEM stress calculation, which resulted in highest values for TiN coating followed by MoS(2) and DLC coatings, being K(C) = 4-11, about 2, and 1-2 MPa M(1/2), respectively. Higher compressive residual stresses in the coating and higher elastic modulus of the coating correlated to increased fracture toughness of the coated surface. (C) 2009 Elsevier B.V. All rights reserved.
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The tribological response of multilayer micro/nanocrystalline diamond coatings grown by the hot filament CVD technique is investigated. These multigrade systems were tailored to comprise a starting microcrystalline diamond (MCD) layer with high adhesion to a silicon nitride (Si3N4) ceramic substrate, and a top nanocrystalline diamond (NCD) layer with reduced surface roughness. Tribological tests were carried out with a reciprocating sliding configuration without lubrication. Such composite coatings exhibit a superior critical load before delamination (130–200 N), when compared to the mono- (60–100 N) and bilayer coatings (110 N), considering ∼10 µm thick films. Regarding the friction behaviour, a short-lived initial high friction coefficient was followed by low friction regimes (friction coefficients between 0.02 and 0.09) as a result of the polished surfaces tailored by the tribological solicitation. Very mild to mild wear regimes (wear coefficient values between 4.1×10−8 and 7.7×10−7 mm3 N−1 m−1) governed the wear performance of the self-mated multilayer coatings when subjected to high-load short-term tests (60–200 N; 2 h; 86 m) and medium-load endurance tests (60 N; 16 h; 691 m).
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Nanocrystalline diamond (NCD) coatings offer an excellent alternative for tribological applications, preserving most of the intrinsic mechanical properties of polycrystalline CVD diamond and adding to it an extreme surface smoothness. Silicon nitride (Si3N4) ceramics are reported to guarantee high adhesion levels to CVD microcrystalline diamond coatings, but the NCD adhesion to Si3N4 is not yet well established. Micro-abrasion tests are appropriate for evaluating the abrasive wear resistance of a given surface, but they also provide information on thin film/substrate interfacial resistance, i.e., film adhesion. In this study, a comparison is made between the behaviour of NCD films deposited by hot-filament chemical vapour deposition (HFCVD) and microwave plasma assisted chemical vapour deposition (MPCVD) techniques. Silicon nitride (Si3N4) ceramic discs were selected as substrates. The NCD depositions by HFCVD and MPCVD were carried out using H2–CH4 and H2–CH4–N2 gas mixtures, respectively. An adequate set of growth parameters was chosen for each CVD technique, resulting in NCD films having a final thickness of 5 m. A micro-abrasion tribometer was used, with 3 m diamond grit as the abrasive slurry element. Experiments were carried out at a constant rotational speed (80 r.p.m.) and by varying the applied load in the range of 0.25–0.75 N. The wear rate for MPCVD NCD (3.7±0.8 × 10−5 m3N−1m−1) is compatible with those reported for microcrystalline CVD diamond. The HFCVD films displayed poorer adhesion to the Si3N4 ceramic substrates than the MPCVD ones. However, the HFCVD films show better wear resistance as a result of their higher crystallinity according to the UV Raman data, despite evidencing premature adhesion failure.
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The main reasons for the attention focused on ceramics as possible structural materials are their wear resistance and the ability to operate with limited oxidation and ablation at temperatures above 2000°C. Hence, this work is devoted to the study of two classes of materials which can satisfy these requirements: silicon carbide -based ceramics (SiC) for wear applications and borides and carbides of transition metals for ultra-high temperatures applications (UHTCs). SiC-based materials: Silicon carbide is a hard ceramic, which finds applications in many industrial sectors, from heat production, to automotive engineering and metals processing. In view of new fields of uses, SiC-based ceramics were produced with addition of 10-30 vol% of MoSi2, in order to obtain electro conductive ceramics. MoSi2, indeed, is an intermetallic compound which possesses high temperature oxidation resistance, high electrical conductivity (21·10-6 Ω·cm), relatively low density (6.31 g/cm3), high melting point (2030°C) and high stiffness (440 GPa). The SiC-based ceramics were hot pressed at 1900°C with addition of Al2O3-Y2O3 or Y2O3-AlN as sintering additives. The microstructure of the composites and of the reference materials, SiC and MoSi2, were studied by means of conventional analytical techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (SEM-EDS). The composites showed a homogeneous microstructure, with good dispersion of the secondary phases and low residual porosity. The following thermo-mechanical properties of the SiC-based materials were measured: Vickers hardness (HV), Young’s modulus (E), fracture toughness (KIc) and room to high temperature flexural strength (σ). The mechanical properties of the composites were compared to those of two monolithic SiC and MoSi2 materials and resulted in a higher stiffness, fracture toughness and slightly higher flexural resistance. Tribological tests were also performed in two configurations disco-on-pin and slideron cylinder, aiming at studying the wear behaviour of SiC-MoSi2 composites with Al2O3 as counterfacing materials. The tests pointed out that the addition of MoSi2 was detrimental owing to a lower hardness in comparison with the pure SiC matrix. On the contrary, electrical measurements revealed that the addition of 30 vol% of MoSi2, rendered the composite electroconductive, lowering the electrical resistance of three orders of magnitude. Ultra High Temperature Ceramics: Carbides, borides and nitrides of transition metals (Ti, Zr, Hf, Ta, Nb, Mo) possess very high melting points and interesting engineering properties, such as high hardness (20-25 GPa), high stiffness (400-500 GPa), flexural strengths which remain unaltered from room temperature to 1500°C and excellent corrosion resistance in aggressive environment. All these properties place the UHTCs as potential candidates for the development of manoeuvrable hypersonic flight vehicles with sharp leading edges. To this scope Zr- and Hf- carbide and boride materials were produced with addition of 5-20 vol% of MoSi2. This secondary phase enabled the achievement of full dense composites at temperature lower than 2000°C and without the application of pressure. Besides the conventional microstructure analyses XRD and SEM-EDS, transmission electron microscopy (TEM) was employed to explore the microstructure on a small length scale to disclose the effective densification mechanisms. A thorough literature analysis revealed that neither detailed TEM work nor reports on densification mechanisms are available for this class of materials, which however are essential to optimize the sintering aids utilized and the processing parameters applied. Microstructural analyses, along with thermodynamics and crystallographic considerations, led to disclose of the effective role of MoSi2 during sintering of Zrand Hf- carbides and borides. Among the investigated mechanical properties (HV, E, KIc, σ from room temperature to 1500°C), the high temperature flexural strength was improved due to the protective and sealing effect of a silica-based glassy phase, especially for the borides. Nanoindentation tests were also performed on HfC-MoSi2 composites in order to extract hardness and elastic modulus of the single phases. Finally, arc jet tests on HfC- and HfB2-based composites confirmed the excellent oxidation behaviour of these materials under temperature exceeding 2000°C; no cracking or spallation occurred and the modified layer was only 80-90 μm thick.
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Novel poly(phenylene sulphide) (PPS) nanocomposites reinforced with an aminated derivative (PPS-NH2) covalently attached to acid-treated single-walled carbon nanotubes (SWCNTs) were prepared via simple melt-blending technique. Their morphology, viscoelastic behaviour, electrical conductivity, mechanical and tribological properties were investigated. Scanning electron microscopy revealed that the grafting process was effective in uniformly dispersing the SWCNTs within the matrix. The storage and loss moduli as a function of frequency increased with the SWCNT content, tending to a plateau in the low-frequency regime. The electrical conductivity of the nanocomposites was considerably enhanced in the range 0.1?0.5 wt% SWCNTs; electrical and rheological percolation thresholds occurred at similar nanotube concentrations. Mechanical tests demonstrated that with only 1.0 wt% SWCNTs the Young's modulus and tensile strength of the matrix improved by 51 and 37%, respectively, without decrement in toughness, ascribed to a very efficient load transfer. A moderate decrease in the friction coefficient and a 75% reduction in wear rate were found for the abovementioned nanotube loading, indicating that PPS-NH2-g-SWCNTs are good tribological additives for thermoplastic polymers. Based on the promising results obtained in this work, it is expected that these nanofillers will be used to develop high-performance thermoplastic/CNT nanocomposites for structural applications.
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TiSiC-Cr coatings, with Cr and Si as additional elements, were deposited on Si, C 45 and 316 L steel substrates via cathodic arc evaporation. Two series of coatings with thicknesses in the range of 3.6–3.9 μm were produced, using either CH4 or C2H2 as carbon containing gas. For each series, different coatings were prepared by varying the carbon rich gas flow rate between 90 and 130 sccm, while maintaining constant cathode currents (110 and 100 A at TiSi and Cr cathodes, respectively), substrate bias (–200 V) and substrate temperature (∼320 °C). The coatings were analyzed for their mechanical characteristics (hardness, adhesion) and tribological performance (friction, wear), along with their elemental and phase composition, chemical bonds, crystalline structure and cross-sectional morphology. The coatings were found to be formed with nano-scale composite structures consisting of carbide crystallites (grain size of 3.1–8.2 nm) and amorphous hydrogenated carbon. The experimental results showed significant differences between the two coating series, where the films formed from C2H2 exhibited markedly superior characteristics in terms of microstructure, morphology, hardness, friction behaviour and wear resistance. For the coatings prepared using CH4, the measured values of crystallite size, hardness, friction coefficient and wear rate were in the ranges of 7.2–8.2 nm, 26–30 GPa, 0.3–0.4 and 2.1–4.8 × 10−6 mm3 N−1 m−1, respectively, while for the coatings grown in C2H2, the values of these characteristics were found to be in the ranges of 3.1–3.7 nm, 41–45 GPa, 0.1–0.2 and 1.4–3.0 × 10−6 mm3 N−1 m−1, respectively. Among the investigated coatings, the one produced using C2H2 at the highest flow rate (130 sccm) exhibited the highest hardness (45.1 GPa), the lowest friction coefficient (0.10) and the best wear resistance (wear rate of 1.4 × 10−6 mm3 N−1 m−1).
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Oligodendrocytes and Schwann cells are engaged in myelin production, maintenance and repairing respectively in the central nervous system (CNS) and the peripheral nervous system (PNS). Whereas oligodendrocytes act only within the CNS, Schwann cells are able to invade the CNS in order to make new myelin sheaths around demyelinated axons. Both cells have some limitations in their activities, i.e. oligodendrocytes are post-mitotic cells and Schwann cells only get into the CNS in the absence of astrocytes. Ethidium bromide (EB) is a gliotoxic chemical that when injected locally within the CNS, induce demyelination. In the EB model of demyelination, glial cells are destroyed early after intoxication and Schwann cells are free to approach the naked central axons. In normal Wistar rats, regeneration of lost myelin sheaths can be achieved as early as thirteen days after intoxication; in Wistar rats immunosuppressed with cyclophosphamide the process is delayed and in rats administered cyclosporine it may be accelerated. Aiming the enlightening of those complex processes, all events concerning the myelinating cells in an experimental model are herein presented and discussed.
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The behaviour of the albino and melanic variants of Biomphalaria glabrata of Belo Horizonte (MG. Brazil) was studied comparatively, in terms of their respective susceptibilities to infection by Schistosoma mansoni of the same origin, through observation of the elimination of cercariae for a three-month period and the calculation of mortality and infection rates, in control and in infected snails. The number of amoebocytes, granulocytes and hyalinocytes in the circulating hemolymph during different periods of infection was analyzed. The evolution of the infection in the tissues was observed by means of histological cross-sections. The melanic variant showed greater susceptibility to infection and a higher mortality rate. The albino variant showed a higher number of circulating amoebocytes, both granulocytes and hyalinocytes. A higher number of degenerated sporocysts were seen in the histological cross-sections of the albino variant. The results suggest that the melanic variant of B. glabrata was more susceptible to infection by S. mansoni than was the albino variant.