The thesis is focused on the theoretical description of the technology of anodizing of aluminium, magnesium, zinc and their alloys. In this work, methods for formation of oxide layers and the used chemical processes are described in detail. The experimental part of this work deals with formation of oxide layers on aluminium, magnesium and zinc of high purity under different conditions. Oxide layers of different thicknesses were created on all three experimental materials. Aluminium was anodized in a bath of 10% H2SO4, magnesium in the bath of 1 mol/dm3 NaOH, and zinc in the bath of 0.5 mol/dm3 NaOH. Processes were carried out at laboratory temperature. On the aluminium, continuous oxide layer was formed. Furthermore rule "312" was verified, that can indicatively be used for calculating the thickness of the resulting oxide layer on the aluminium. When using lower current of 0.08 and 0.2 A for magnesium anodizing, dark colored layer was created comparing to higher current of 0.5 A. More rough appearance of the oxide layer was produced with increasing voltage. Further, it was observed for magnesium that the resulting layer comprises of two sublayers. For zinc, black colored layer was created when the voltage 20 V and current from 0.4 to 0.5 A were used. In the layer, two sublayers were also observed. For lower voltage and current (0.05 A, 0.17 V), formation of the oxide layer on the zinc does not occur, but the crystallographic etching was observed.

A process with aim to prepare an oxidically and thermal resistant layer was performed on the samples from clear aluminium (99,99+ %, VÚK čisté kovy, s. r. o.) and on the samples from clear titanium (99,95 % Goodfellow) with a layer from sputtered aluminium (99,99 %, VÚK čisté kovy, s. r. o.), An oxidic layer was prepared on the samples by anodization in the oxalic acid. The layer had fine, hexagonally organized pores with the diameter of 30 nm. During the following processing was the structure prepared for the electrochemical deposition of copper to the pores. The aim of the electrodeposition was preparation of copper nanowires deposited into the pores of the oxidic layer. The process was performed in the solution of copper sulfate and sulfuric acid in water. The controlling parameter of the deposition was voltage which had a very asymmetric period. The period had to be optimized for a successful preparation of the wires. The result of the whole process was structure with oxidic matrix whose most of the pores were filled with copper.

No description available.

Submitted by Caio Santos (c.dehly@gmail.com) on 2017-10-26T20:56:53Z No. of bitstreams: 2 Dissertação_Caio.pdf: 6450967 bytes, checksum: 9c0ad5f1b63e4ef97562046030ba0696 (MD5) Carta_Comprovante.pdf: 679811 bytes, checksum: b230eed541e4ff4ea1205d79507474d1 (MD5) / Approved for entry into archive by Milena Rubi ( ri.bso@ufscar.br) on 2017-11-10T12:12:33Z (GMT) No. of bitstreams: 2 Dissertação_Caio.pdf: 6450967 bytes, checksum: 9c0ad5f1b63e4ef97562046030ba0696 (MD5) Carta_Comprovante.pdf: 679811 bytes, checksum: b230eed541e4ff4ea1205d79507474d1 (MD5) / Approved for entry into archive by Milena Rubi ( ri.bso@ufscar.br) on 2017-11-10T12:12:54Z (GMT) No. of bitstreams: 2 Dissertação_Caio.pdf: 6450967 bytes, checksum: 9c0ad5f1b63e4ef97562046030ba0696 (MD5) Carta_Comprovante.pdf: 679811 bytes, checksum: b230eed541e4ff4ea1205d79507474d1 (MD5) / Made available in DSpace on 2017-11-10T12:13:12Z (GMT). No. of bitstreams: 2 Dissertação_Caio.pdf: 6450967 bytes, checksum: 9c0ad5f1b63e4ef97562046030ba0696 (MD5) Carta_Comprovante.pdf: 679811 bytes, checksum: b230eed541e4ff4ea1205d79507474d1 (MD5) Previous issue date: 2017-04-27 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Porous anodic alumina can be obtained, in addition to conventional methods such as potentiostatic and galvanostatic, or by pulsed method. Among these are the methods of discontinuous pulse, hybrid pulse and polarized pulse methods. The structures formed by these methods can be applied to sensors and photonic materials. In this work the influences of the pulse parameters for the porous anodic alumina were investigated by polarized pulse potentiostatic anodization. Data analysis was presented from the duty cycle seen in the literature, which provides important information about the structure formed for the applied conditions and, in addition, new ways of analyzing the data related to the pulse, such as the analysis of the potential difference and the pulse frequency, this latter complementing the analysis of the duty cycle. As a result it was possible to observe that the porous anodic alumina thickness obtained is proportional to the duty cycle applied, where the higher duty cycle, the greater the thickness obtained. From the potential difference, the differences in the morphological and optical parameters could be analyzed by the influence of the negative minimum voltage applied during the pulsed anodization. The pulse frequency, also discussed in this work, was used to analyze different pulse periods for the same duty cycle, demonstrating that can be obtained structures with different values by varying the value of the pulse frequency. For the porosity calculation, an application was developed that helped to obtain the pore distance, which is one of the variables used to calculate the porosity. With the porosity values, the effective refractive index of each sample was calculated to find the effective optical thickness (EOT) and, finally, the thickness of the obtained anodic alumina film. / A alumina anódica porosa pode ser obtida, além dos métodos convencionais como potenciostático e galvanostático, ou por métodos pulsados. Dentre estes destacam-se os métodos de pulso descontínuo, pulso híbrido e pulso polarizado. As estruturas formadas por estes métodos podem ser aplicadas em sensores e materiais fotônicos. Neste trabalho foram investigadas as influências dos parâmetros de pulso para a obtenção da alumina anódica porosa pelo método de anodização potenciostática com pulso polarizado. Foram apresentadas análises de dados a partir do ciclo de trabalho visto na literatura, onde traz importantes informações sobre a estrutura formada para as condições aplicadas e, além disto, novas formas de analisar os dados referentes aos pulsos, como a análise a partir da diferença de potencial e a frequência de pulso, este último complementando a análise do ciclo de trabalho. Como resultado foi possível observar que a espessura de alumina anódica porosa obtida é proporcional ao ciclo de trabalho aplicado, onde quanto maior o ciclo de trabalho, maior será a espessura obtida. A partir da diferença de potencial pôde-se analisar as diferenças nos parâmetros morfológicos e ópticos pela influência da tensão mínima negativa aplicada durante a anodização pulsada. A frequência de pulso, também abordada neste trabalho, foi utilizada para analisar diferentes períodos de pulsos para o mesmo ciclo de trabalho, demonstrando que variando o valor da frequência de pulso pode-se obter estruturas com valores distintos. Para o cálculo da porosidade foi desenvolvido um aplicativo que auxiliou na obtenção da distância entre poros, que é uma das variáveis utilizadas para o cálculo da porosidade. E com os valores de porosidade foi calculado o índice de refração efetivo de cada amostra para encontrar a sua espessura óptico efetivo (EOT, do inglês Effective Optical Thickness) e, por fim, a espessura do filme de alumina anódica obtido.

L'étude du comportement électrochimique des phases intermétalliques Al2Cu, Al2CuMg, Al7Cu2Fe, (Al,Cu)16Mn4Si3 et MgZn2, caractéristiques des alliages d'aluminium 2214-T6 et 7050-T74 et réalisée à partir d'échantillons massifs synthétisés, a montré que la formation de défauts majeurs dans la couche d'oxyde, obtenue par anodisation des alliages en milieu H2SO4 200 g/l, était directement due à la présence de ces particules au sein des alliages. L'important dégagement gazeux d'oxygène qui se produit à la surface de ces particules lors de l'étape d'anodisation explique la formation de trous et de fractures dans la couche d'oxyde. En milieu marin, ces défauts facilitent la migration des ions chlorures à la surface de l'alliage mise à nu localement et favorisent par conséquent le développement de la corrosion localisée. Les résultats obtenus en milieu NaCl 35g/l ont permis de mieux comprendre le mécanisme de corrosion des phases intermétalliques ainsi que leur rôle sur la propagation des piqûres. L'élimination des particules intermétalliques de la surface des alliages lors de l'étape de décapage (avant anodisation) permet de favoriser une croissance plus régulière de la couche d'oxyde lors de l'anodisation. Par conséquent, la résistance à la corrosion des alliages 2214 et 7050 augmente considérablement, permettant d'atteindre les objectifs fixés lors de ce projet / The electrochemical behaviour of the bulk intermetallic particles such as Al2Cu, Al2CuMg, Al7Cu2Fe, (Al,Cu)16(Mn,Fe)4Si3 and MgZn2 showed that the formation of wide defects in the oxide layer during the 2214-T6 and 7050-T74 alloys anodization was directly due to the presence of these kind of particles in the microstructure which are able to sustain both high dissolution rate and high water oxidation kinetics in acidic electrolyte. In marine environment, these defects facilitate the migration of aggressive ions like chloride on the locally bare alloys and are the onset of the pitting corrosion. The results obtained in 3.5 wt.% sodium chloride electrolyte permit to understand the corrosion mechanism of the intermetallic phases and their influence on the pits propagation. The optimization of the alloys pickling conditions in order to remove this kind of particles (prior to the anodization step) has been investigated in this work. Consequence of removing intermetallic particles, the aluminium enrichment of the surface facilitates the oxide growth and the formation of regular layer. The corrosion tests on treated aluminium alloys have clearly showed the influence of the pickling step on the resistance corrosion of 2214 and 7050 alloys, reaching the objectives fixed in this project

Cette étude avait pour objectif de développer un nouveau support photocatalytique pour des applications potentielles dans le domaine du traitement des eaux. Le choix s'est porté sur les nanotubes d'oxyde de titane (TiO2) et l'étude a plus particulièrement porté sur l'optimisation de leurs propriétés photocatalytiques vis-à-vis de la l'oxydation de solution aqueuse de composés azotés. Les nanotubes de TiO2 ont été préparés par anodisation électrochimique en faisant varier le potentiel appliqué, la durée d'anodisation, le pH et la viscosité du milieu électrolytique (milieu aqueux ou milieu glycérol), ainsi que la nature du substrat sur lequel étaient déposés ces nanotubes. Une fois anodisés, ces nanotubes amorphes et se présentant sous forme sous-stœchiométrique (O/Ti <2) ont été recuits à différentes températures afin d'obtenir des phases de TiO2 variées (anatase, anatase/rutile). Au cours de ces différentes étapes, les différents nanotubes obtenus ont été caractérisés morphologiquement et structurellement par analyses par diffraction des rayons X (DRX) et par microscopie électronique à balayage (MEB).L'activité photocatalytique de ces différents matériaux a été déterminée à partir des rendements de photodégradation d'un composé modèle, la 4-nitroaniline. Là aussi, différents facteurs ont été étudiés, à savoir le pH du milieu réactionnel, le type de lampe UV et les durées d'irradiation.Les résultats montrent que les performances photocatalytiques des nanotubes de TiO2 les meilleures sont obtenues lorsqu'ils sont déposés sur substrat de Ti massif, anodisés en solution aqueuse à 20 V et pendant 20 minutes, et recuits à 450 °C (structure anatase). / This study aimed to design a new photocatalytic support for potential uses in the field of water treatment. Titanium dioxide (TiO2) nanotubes were chosen and studied as a function of their photocatalytic properties towards nitrogenous compounds.TiO2 nanotubes were prepared by electrochemical anodization by varying the applied potential, anodization duration, pH and viscosity of the electrolytic medium (aqueous or glycerol medium), and by the nature of substrates where these nanotubes were deposited (titanium foil (Ti) or deposited on silicon (Ti / Si)). Once anodized, these amorphous and under-stoechiometric (O/Ti <2) were calcined at various temperatures in order to obtain different TiO2 phases (anatase or anatase/rutile). During these different steps, the whole nanotubes obtained were morphologically and structurally characterized par X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic activity of the different materials was determined from the photodegradation yields of a model compound, namely 4-nitroaniline. Here again, different factors were studied, such as pH of reaction medium, kind of UV lamps and irradiation durations. The results show that the best photocatalytic performances of TiO2 nanotubes were obtained when deposited on Ti foils, anodized in aqueous medium at 20 V and for 20 minutes, and calcined at 450 °C (anatase phase).

Neste trabalho foram estudadas diferentes modificações superficiais do titânio (Ti) como método de preparação de superfícies de eletrodos para baterias de íons lítio (Li+) Inicialmente, as modificações foram produzidas pelas micro-indentações, com posterior corrosão eletroquímica por pites em soluções de brometo. As superfícies polidas, tratadas termicamente e modificadas através de micro-indentações foram avaliadas em diferentes parâmetros, tais como o potencial aplicado, concentração dos íons agressivos no eletrólito, temperatura, tempo dos testes e principalmente, sobre o impacto das deformações causadas pela força indentações para localização de orifícios produzidos por pites. Filmes porosos de titânia (TiO2) crescidos sobre o Ti puro, foram produzidos por anodização a plasma (anodização por centelhamento ou sparking) em 1M H3PO4 e em 1M Na2SO4 e por anodização nanotubular em 1M H3PO4 + 1M NaOH + 0,4 %(peso) HF. Os resultados mostraram, em óxidos tipo “esponja” formados na anodização a plasma em 1M H3PO4 e 1M Na2SO4, a incorporação de elementos do eletrólito contendo, respectivamente, P e S, numa relação de P/O > S/O e em óxidos nanotulares, a predominante incorporação de elemento de F. Posteriormente, as superfícies corroídas por pites e as superfícies de óxidos crescidos por anodização a plasma foram convertidas por sulfetação em diferentes materiais micro e nanoestruturados compostos por sulfetos e oxisulfetos de titânio, ajustando-se as condições de processo. O desenvolvimento proposto mostrou que é possível modificar a composição química do óxido formado por anodização a plasma para nanocristais de TiS2, nanofitas de TiS3 e TiOxSy, sem danificar a morfologia original dos nanoporos de TiO2. Os compostos formados podem ser usados como eletrodos nanoarquiteturados tridimensionais (3D) para microbaterias de íons lítio (Li+) com alta densidade de potência. A síntese desses compostos é realmente promissora, porque eles têm a capacidade de inserir mais íons lítio do que TiO2 puro, resultando em uma melhoria na capacidade das microbaterias. / In this study, different surface modifications of titanium (Ti) were studied as a method of surface preparation of electrodes for ion lithium batteries (Li+). Initially, the modifications were produced by micro-indentation with subsequent electrochemical pitting corrosion in solutions of bromide. The polished surfaces, heat treated and modified through micro indentations were evaluated for different values of parameters, such as applied potential, concentration of aggressive ions in the electrolyte, temperature, polarization time, and mainly intensity of the deformation caused by indentations for localizing holes produced by pitting. It was expected the adjust of location of these parameter settings promotes nucleation of pits, according to the pattern of indentations and growth of pitting depth for increased surface area. Porous films of titania (TiO2) were produced on pure Ti by plasma anodization (or sparking) in 1M H3PO4 and 1M Na2SO4. Nanotubes were synthesized by porous anodization in 1M NaOH + 1M H3PO4 + 0.4 (wt%) HF. The results showed oxide "sponge" like formed by plasma anodization, incorporating elements of the electrolyte containing respectively, P and S in a ratio P/O> S/O and, in nanotubular oxides, with predominant incorporation of F. Subsequently, the pitted surfaces and the surfaces of oxides grown by plasma anodization were converted by sulfidation into different micro and nanostructured materials consisting of titanium sulfide and oxisulfides by adjusting the process conditions. The proposed development has shown that it is possible to modify the chemical composition of the oxide formed by plasma anodizing to nanocrystals of TiS2 and nanobelts of TiS3 and TiOxSy without damaging the original morphology of the nanoporous TiO2. The formed compounds can be used as three-dimensional (3D) nanoarchitectured electrodes for ion lithium batteries (Li+) with high power density. The synthesis of these compounds is promising due to a higher ability to intercalate more ions lithium than pure TiO2, resulting in an improvement in the capacity of microbatteries.

Ces travaux de thèse portent sur le développement d’une périphérie innovante de TRIAC exploitant le caractère semiisolant du silicium poreux (PS). L’intégration de caissons PS type P à partir des profils de dopage du TRIAC est en effet accessible. Une revue des propriétés électriques du PS type P réalisée à partir de nos propres échantillons méso voire micro-poreux a donc été entreprise. Des mesures de capacités et des relevés I-V ont ainsi permis de déterminer l’évolution de la constante diélectrique relative du PS ainsi que sa résistivité en fonction de la porosité. Plus cette dernière est élevée et plus les propriétés diélectriques du PS se rapprochent de celles d’un isolant. L’analyse des résultats a également permis de clarifier les mécanismes de transport des porteurs au sein de la couche de PS. Des prototypes de TRIACs avec une terminaison de jonction à base de PS ont ensuite été conçus, fabriqués et étudiés. La localisation du PS et la gestion des contraintes mécaniques résultant de la formation du PS sont apparus comme les principaux verrous technologiques à surmonter. Des solutions ont été proposées, néanmoins les tenues en blocage atteintes se sont avérées insuffisantes. Des courants de fuite supérieurs à la dizaine de milliampères ont en effet été mesurés et ce pour des tensions de polarisation de l’ordre de 100 V. La géométrie des caissons PS et/ou la présence de charges fixes à l’interface PS / Silicium sont jugées responsables des résultats. Enfin, en s’appuyant sur un modèle macroscopique du PS, une nouvelle structure plus optimisée a été suggérée. / This PhD thesis deals with the development of a novel TRIAC periphery, exploiting the semi-insulating nature of porous silicon (PS). It is namely accessible to integrate P type PS wells through the doping profiles encountered in the TRIAC. Thus, a review of the P type PS electrical properties was achieved through dedicated samples. In this context, capacitance measurements and I-V plots were used to determine the evolution of the PS relative dielectric constant and its resistivity with the porosity. Higher the latter is, more insulating the PS is. By analyzing all the results, it was also possible to clarify the carrier transport mechanisms in the PS. Some TRIAC prototypes with a PS based junction termination were then designed, processed and studied. The stress coming from the PS formation and the PS masking were the main technological steps to solve. First solutions were proposed, nevertheless insufficient blocking performances were reached. Leakage currents higher than 10 mA were demonstrated while the bias voltage was only 100 V. The presence of fixed charges at the PS / Silicon interface and/or the geometry of the PS wells may explain these results. Finally, with the help of a macroscopic PS model, a more optimized structure was proposed.

Neste trabalho foram estudadas diferentes modificações superficiais do titânio (Ti) como método de preparação de superfícies de eletrodos para baterias de íons lítio (Li+) Inicialmente, as modificações foram produzidas pelas micro-indentações, com posterior corrosão eletroquímica por pites em soluções de brometo. As superfícies polidas, tratadas termicamente e modificadas através de micro-indentações foram avaliadas em diferentes parâmetros, tais como o potencial aplicado, concentração dos íons agressivos no eletrólito, temperatura, tempo dos testes e principalmente, sobre o impacto das deformações causadas pela força indentações para localização de orifícios produzidos por pites. Filmes porosos de titânia (TiO2) crescidos sobre o Ti puro, foram produzidos por anodização a plasma (anodização por centelhamento ou sparking) em 1M H3PO4 e em 1M Na2SO4 e por anodização nanotubular em 1M H3PO4 + 1M NaOH + 0,4 %(peso) HF. Os resultados mostraram, em óxidos tipo “esponja” formados na anodização a plasma em 1M H3PO4 e 1M Na2SO4, a incorporação de elementos do eletrólito contendo, respectivamente, P e S, numa relação de P/O > S/O e em óxidos nanotulares, a predominante incorporação de elemento de F. Posteriormente, as superfícies corroídas por pites e as superfícies de óxidos crescidos por anodização a plasma foram convertidas por sulfetação em diferentes materiais micro e nanoestruturados compostos por sulfetos e oxisulfetos de titânio, ajustando-se as condições de processo. O desenvolvimento proposto mostrou que é possível modificar a composição química do óxido formado por anodização a plasma para nanocristais de TiS2, nanofitas de TiS3 e TiOxSy, sem danificar a morfologia original dos nanoporos de TiO2. Os compostos formados podem ser usados como eletrodos nanoarquiteturados tridimensionais (3D) para microbaterias de íons lítio (Li+) com alta densidade de potência. A síntese desses compostos é realmente promissora, porque eles têm a capacidade de inserir mais íons lítio do que TiO2 puro, resultando em uma melhoria na capacidade das microbaterias. / In this study, different surface modifications of titanium (Ti) were studied as a method of surface preparation of electrodes for ion lithium batteries (Li+). Initially, the modifications were produced by micro-indentation with subsequent electrochemical pitting corrosion in solutions of bromide. The polished surfaces, heat treated and modified through micro indentations were evaluated for different values of parameters, such as applied potential, concentration of aggressive ions in the electrolyte, temperature, polarization time, and mainly intensity of the deformation caused by indentations for localizing holes produced by pitting. It was expected the adjust of location of these parameter settings promotes nucleation of pits, according to the pattern of indentations and growth of pitting depth for increased surface area. Porous films of titania (TiO2) were produced on pure Ti by plasma anodization (or sparking) in 1M H3PO4 and 1M Na2SO4. Nanotubes were synthesized by porous anodization in 1M NaOH + 1M H3PO4 + 0.4 (wt%) HF. The results showed oxide "sponge" like formed by plasma anodization, incorporating elements of the electrolyte containing respectively, P and S in a ratio P/O> S/O and, in nanotubular oxides, with predominant incorporation of F. Subsequently, the pitted surfaces and the surfaces of oxides grown by plasma anodization were converted by sulfidation into different micro and nanostructured materials consisting of titanium sulfide and oxisulfides by adjusting the process conditions. The proposed development has shown that it is possible to modify the chemical composition of the oxide formed by plasma anodizing to nanocrystals of TiS2 and nanobelts of TiS3 and TiOxSy without damaging the original morphology of the nanoporous TiO2. The formed compounds can be used as three-dimensional (3D) nanoarchitectured electrodes for ion lithium batteries (Li+) with high power density. The synthesis of these compounds is promising due to a higher ability to intercalate more ions lithium than pure TiO2, resulting in an improvement in the capacity of microbatteries.

Neste trabalho foram estudadas diferentes modificações superficiais do titânio (Ti) como método de preparação de superfícies de eletrodos para baterias de íons lítio (Li+) Inicialmente, as modificações foram produzidas pelas micro-indentações, com posterior corrosão eletroquímica por pites em soluções de brometo. As superfícies polidas, tratadas termicamente e modificadas através de micro-indentações foram avaliadas em diferentes parâmetros, tais como o potencial aplicado, concentração dos íons agressivos no eletrólito, temperatura, tempo dos testes e principalmente, sobre o impacto das deformações causadas pela força indentações para localização de orifícios produzidos por pites. Filmes porosos de titânia (TiO2) crescidos sobre o Ti puro, foram produzidos por anodização a plasma (anodização por centelhamento ou sparking) em 1M H3PO4 e em 1M Na2SO4 e por anodização nanotubular em 1M H3PO4 + 1M NaOH + 0,4 %(peso) HF. Os resultados mostraram, em óxidos tipo “esponja” formados na anodização a plasma em 1M H3PO4 e 1M Na2SO4, a incorporação de elementos do eletrólito contendo, respectivamente, P e S, numa relação de P/O > S/O e em óxidos nanotulares, a predominante incorporação de elemento de F. Posteriormente, as superfícies corroídas por pites e as superfícies de óxidos crescidos por anodização a plasma foram convertidas por sulfetação em diferentes materiais micro e nanoestruturados compostos por sulfetos e oxisulfetos de titânio, ajustando-se as condições de processo. O desenvolvimento proposto mostrou que é possível modificar a composição química do óxido formado por anodização a plasma para nanocristais de TiS2, nanofitas de TiS3 e TiOxSy, sem danificar a morfologia original dos nanoporos de TiO2. Os compostos formados podem ser usados como eletrodos nanoarquiteturados tridimensionais (3D) para microbaterias de íons lítio (Li+) com alta densidade de potência. A síntese desses compostos é realmente promissora, porque eles têm a capacidade de inserir mais íons lítio do que TiO2 puro, resultando em uma melhoria na capacidade das microbaterias. / In this study, different surface modifications of titanium (Ti) were studied as a method of surface preparation of electrodes for ion lithium batteries (Li+). Initially, the modifications were produced by micro-indentation with subsequent electrochemical pitting corrosion in solutions of bromide. The polished surfaces, heat treated and modified through micro indentations were evaluated for different values of parameters, such as applied potential, concentration of aggressive ions in the electrolyte, temperature, polarization time, and mainly intensity of the deformation caused by indentations for localizing holes produced by pitting. It was expected the adjust of location of these parameter settings promotes nucleation of pits, according to the pattern of indentations and growth of pitting depth for increased surface area. Porous films of titania (TiO2) were produced on pure Ti by plasma anodization (or sparking) in 1M H3PO4 and 1M Na2SO4. Nanotubes were synthesized by porous anodization in 1M NaOH + 1M H3PO4 + 0.4 (wt%) HF. The results showed oxide "sponge" like formed by plasma anodization, incorporating elements of the electrolyte containing respectively, P and S in a ratio P/O> S/O and, in nanotubular oxides, with predominant incorporation of F. Subsequently, the pitted surfaces and the surfaces of oxides grown by plasma anodization were converted by sulfidation into different micro and nanostructured materials consisting of titanium sulfide and oxisulfides by adjusting the process conditions. The proposed development has shown that it is possible to modify the chemical composition of the oxide formed by plasma anodizing to nanocrystals of TiS2 and nanobelts of TiS3 and TiOxSy without damaging the original morphology of the nanoporous TiO2. The formed compounds can be used as three-dimensional (3D) nanoarchitectured electrodes for ion lithium batteries (Li+) with high power density. The synthesis of these compounds is promising due to a higher ability to intercalate more ions lithium than pure TiO2, resulting in an improvement in the capacity of microbatteries.