Chan, Mui. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2009. / Includes bibliographical references. / Abstract also in Chinese. / Abstract --- p.i / Abstract (Chinese) --- p.iii / Declaration --- p.v / Acknowledgement --- p.vi / Table of Contents --- p.viii / List of Tables --- p.xiv / List of Figures --- p.xv / Chapter Chapter 1: --- Introduction / Chapter 1.1 --- Overview --- p.1 / Chapter 1.2 --- Soft-Chemistry --- p.7 / Chapter 1.2.1 --- Sol-Gel Method --- p.7 / Chapter 1.2.2 --- Co-precipitation --- p.9 / Chapter 1.2.3 --- Microemulsion --- p.10 / Chapter 1.3 --- Application of Hydrothermal/Solvothermal Methods in Materials Synthesis --- p.12 / Chapter 1.3.1 --- Fundamentals of Hydrothermal and Solvothermal Methods --- p.12 / Chapter 1.3.2 --- Advantages of Hydrothermal/Solvothermal Methods in contrast to Conventional Synthetic Approaches --- p.13 / Chapter 1.3.3 --- Hydrothermal and Solvothermal Preparation of Materials --- p.14 / Chapter 1.4 --- Application of Transition Metal Oxides As Functional Materials --- p.15 / Chapter 1.5 --- Aim and Scope of Work --- p.16 / Chapter 1.6 --- References --- p.17 / Chapter Chapter 2: --- Solvothermal and Hydrothermal Template Free Synthesis of ZnO Microspheres / Chapter 2.1 --- Introduction --- p.23 / Chapter 2.2 --- Experimental Section --- p.25 / Chapter 2.2.1 --- Synthesis of ZnO Microspheres by Solvothermal Method --- p.25 / Chapter 2.2.2 --- Synthesis of ZnO Microspheres by Hydrothermal Method --- p.26 / Chapter 2.2.3 --- Doping ZnO Microspheres with Silver or Gallium by Solvothermal Method --- p.26 / Chapter 2.2.4 --- Characterization --- p.27 / Chapter 2.2.5 --- Measurement of Photocatalytic Activity --- p.29 / Chapter 2.3 --- Results and Discussion --- p.30 / Chapter 2.3.1 --- X-Ray Diffraction Analysis --- p.30 / Chapter 2.3.1.1 --- ZnO-HT and ZnO-ST --- p.30 / Chapter 2.3.1.2 --- ZnO-ST: Effect of Different Concentrations of Zinc Acetate --- p.33 / Chapter 2.3.1.3 --- Doping ZnO-ST with Silver or Gallium --- p.34 / Chapter 2.3.2 --- SEM study --- p.36 / Chapter 2.3.2.1 --- ZnO-HT and ZnO-ST --- p.36 / Chapter 2.3.2.2 --- ZnO-HT-Different Volume Ratios of Ethylene Glycol to Water --- p.37 / Chapter 2.3.2.3 --- ZnO-ST --- p.39 / Chapter 2.3.2.3.1 --- Different Volume Ratios of Benzyl Alcohol to Ethylene Glycol --- p.40 / Chapter 2.3.2.3.2 --- Different Concentrations of Zinc Acetate --- p.41 / Chapter 2.3.2.3.3 --- Different Concentrations of Urea --- p.42 / Chapter 2.3.3 --- TEM Study --- p.44 / Chapter 2.3.3.1 --- TEM and HRTEM of ZnO-HT --- p.44 / Chapter 2.3.3.2 --- TEM and HRTEM of ZnO-ST --- p.45 / Chapter 2.3.3.3 --- TEM Images of Ga-Doped ZnO-ST --- p.47 / Chapter 2.3.3.4 --- TEM Images of Ag-Doped ZnO-ST --- p.49 / Chapter 2.3.4 --- Nitrogen Adsorption and Desorption --- p.50 / Chapter 2.3.5 --- X-Ray Photoelectron Spectroscopy --- p.52 / Chapter 2.3.5.1 --- XPS Study of ZnO-ST --- p.52 / Chapter 2.3.5.2 --- XPS Study of ZnO-HT --- p.54 / Chapter 2.3.5.3 --- XPS Study of Silver Doped ZnO-ST --- p.56 / Chapter 2.3.5.4 --- XPS Study of Gallium Doped ZnO-ST --- p.58 / Chapter 2.3.6 --- FR-IR Spectra --- p.60 / Chapter 2.3.7 --- Photocatalytic Activity on Degradation of Methylene Blue --- p.61 / Chapter 2.3.8 --- Proposed Formation Mechanism for ZnO-ST --- p.64 / Chapter 2.3.9 --- Proposed Formation Mechanism for ZnO-HT --- p.68 / Chapter 2.3.10 --- Optical Property of ZnO Microspheres --- p.69 / Chapter 2.4 --- Conclusion --- p.73 / Chapter 2.5 --- References --- p.74 / Chapter Chapter 3: --- Synthesis of Hierarchical Porous Lithium Niobate Submicrometer Rods / Chapter 3.1 --- Introduction --- p.79 / Chapter 3.2 --- Experimental Section --- p.81 / Chapter 3.2.1 --- Characterization --- p.82 / Chapter 3.3 --- Results and Discussion --- p.83 / Chapter 3.3.1 --- X-Ray Diffraction Analysis --- p.83 / Chapter 3.3.2 --- SEM Study --- p.86 / Chapter 3.3.2.1 --- Surfactants Dependent Morphologies Change --- p.86 / Chapter 3.3.2.2 --- Concentrations of CTAB --- p.87 / Chapter 3.3.2.3 --- Time Dependent Morphologies Change --- p.88 / Chapter 3.3.3 --- TEM Study --- p.91 / Chapter 3.3.5 --- XPS Analysis --- p.93 / Chapter 3.3.6 --- BET Analysis --- p.96 / Chapter 3.3.7 --- Proposed Formation Mechanism --- p.97 / Chapter 3.3.7.1 --- Effect of Microemulsion --- p.97 / Chapter 3.3.7.2 --- Effect of CTAB --- p.98 / Chapter 3.3.7.3 --- Ostwald Ripening --- p.99 / Chapter 3.3.7.4 --- Formation of LiNi3O8 --- p.101 / Chapter 3.4 --- Conclusion --- p.102 / Chapter 3.5 --- References --- p.103 / Chapter Chapter 4: --- Flower-Like α-Nickel Hydroxide synthesized by hydrothermal method / Chapter 4.1 --- Introduction --- p.106 / Chapter 4.2 --- Experimental Section --- p.108 / Chapter 4.2.1 --- Synthesis of Nickel Hydroxide by Hydrothermal Method --- p.108 / Chapter 4.2.2 --- Characterization --- p.109 / Chapter 4.3 --- Results and Discussion --- p.111 / Chapter 4.3.1 --- X-Ray Diffraction Analysis --- p.111 / Chapter 4.3.2 --- SEM Study --- p.115 / Chapter 4.3.3 --- TEM and HRTEM Study --- p.116 / Chapter 4.3.4 --- XPS Analysis --- p.117 / Chapter 4.3.5 --- FT-IR Analysis --- p.119 / Chapter 4.3.6 --- BET analysis --- p.120 / Chapter 4.3.7 --- Proposed Formation Mechanism of the Flower like α-Ni(OH)2 --- p.122 / Chapter 4.4 --- Conclusion --- p.123 / Chapter 4.5 --- References --- p.124 / Chapter Chapter 5: --- Conclusions and Future Work / Chapter 5.1 --- Conclusions --- p.127 / Chapter 5.2 --- Future work --- p.129

SILVA, Eder Nascimento. Propriedades Vibracionais de Perovskitas Complexas Ordenadas. 2008. 181 f. Tese (Doutorado em Física) - Programa de Pós-Graduação em Física, Departamento de Física, Centro de Ciências, Universidade Federal do Ceará, Fortaleza, 2008. / Submitted by Edvander Pires (edvanderpires@gmail.com) on 2015-05-04T19:23:25Z No. of bitstreams: 1 2008_tese_ensilva.pdf: 7886254 bytes, checksum: baaeb81edf0f9b9bff1c7ee1c5ae7c79 (MD5) / Approved for entry into archive by Edvander Pires(edvanderpires@gmail.com) on 2015-05-07T16:52:15Z (GMT) No. of bitstreams: 1 2008_tese_ensilva.pdf: 7886254 bytes, checksum: baaeb81edf0f9b9bff1c7ee1c5ae7c79 (MD5) / Made available in DSpace on 2015-05-07T16:52:15Z (GMT). No. of bitstreams: 1 2008_tese_ensilva.pdf: 7886254 bytes, checksum: baaeb81edf0f9b9bff1c7ee1c5ae7c79 (MD5) Previous issue date: 2008 / The A2B0B00O6 double perovskites can crystallize in at least 12 different space groups, where the B0O6 and B00O6 octahedra (1:1 order) alternate along the three crystallographic axis. Four perovskites with this order are studied in this work, to know: Sr2CoWO6 (I4/m), Ca2CoWO6, Ca2CoTeO6 and Sr2CoTeO6 (P21/n). In many cases, total or partial disorder due to the random distribution of the B0 and B00 cations in the B sites of the ABO3 perovskites can be observed. An example of compound with total disorder is Pb(Fe1/2Nb1/2)O3 (Cm), where the Fe3+ and Nb5+ cations possess an occupation factor 1/2 in the octahedral sites of the perovskite structure. The compounds: (i) Ba2In(In1/3U2/3)O6, Ba2In(In1/3W2/3)O6 (Fm¯ 3m), Sr2In(In1/3U2/3)O6, Sr2(In0,87W0,13)(In0,46W0,54)O6 (P21/n) and (ii) a2(Fe0,73W0,27)(Fe0,60W0,40)O6 (P21/n) and Sr2(Fe0,79W0,21)(Fe0,54W0,46)O6, Sr2(Fe0.90Te0.10)(Fe0.57Te0.43)O6 (I4/m) possess partial disorder in the sites of the B0 and/or B00 cations, but nevertheless they exhibit 1: 1 order. In the present work, the phonon spectra of the above-mentioned perovskites are studied through the Raman scattering and infrared transmittance and/or diffuse reflectance. To analyze the phonon spectra of these compounds, theory group methods are used based on three ion sub-lattices, to know: A, B0 and B00O6. The vibrational freedom degrees of the 12 ordered perovskites are described in terms of the internal vibrations of the B00O6 octahedron and of the translational modes of the A and B0 cations. This model is valid when the vibrations of the B0O6 octahedron are negligible compared with the one of the B00O6 octahedron. We used crystallographic information to discuss the processes behind the changes in the phonon energies based on the internal modes of the octahedra. Besides, our results of Raman scattering of low temperature in Pb(Fe1/2Nb1/2)O3 ceramic, reveal pronounced anomalies in the phonon spectra around N´eel temperature TN∼150 K. We attributed these anomalies to the magnetoelectric effect in this compound.

Disorder in materials often brings in new and exotic physical properties along with it. It is thus very important to study different kinds of disorder and their implications on various material properties. In this thesis, we study selected transition metal oxide families of compounds, each being associated with a specific kind of disorder and investigate effects of that disorder on their dielectric and magnetic properties. In Chapter1, we have given brief introductions on the origin of magnetic and dielectric properties in materials and have also discussed various mechanism which give rise to multiferroism in materials which exhibit both spontaneous magnetic ordering and spontaneous electric ordering in the same phase of the material. In Chapter2,we describe the various methodologies adopted in this thesis. In Chapter3,we mainly study the effect of cationic size-disorder in deciding un-usually robust dielectric properties of Ln2CuTiO6(Ln=Y,Dy,Ho,Er,Yb) family of compounds. We discover that these materials, in addition to possessing large dielectric constant values, also exhibit exceptional stabilities of their dielectric constants with respect to large changes in temperature and frequency. We further find that this class of materials are non-ferroelectrics though its hares the same non-centrosymmetric space group, P63cm,with the well-known multiferroic YMnO3 that undergoes a ferroelectric transition at 940K. Using first principles calculations, we establish that exceptional dielectric properties result from a combination of two separate effects. Extensive size disorders at the Cu/Ti B-site suppress the expected ferroelectric transition, leading to relatively large values of the dielectric constant for every compound investigated in this series. Additionally, it is shown that the majority contribution to the dielectric constant arises from intermediate-frequency polar vibrational modes, making it relatively stable against temperature variations. In Chapter4, we study the effect of cation anti-site disorder on the magnetic, electric and dielectric properties of the solid solution series of (x)Fe2O3-(1-x)FeTiO3 for several values of x. For intermediate values of x, these solid solution members are found to be strong ferrimagnets. Anti-site cation disorder, between Fe and Ti, however strongly reduces the magnetic moment values. By tuning the degree of cation anti-site disorder, we attain multi-functionality in these samples. We have performed detailed characterizations of valence states of Fe and Ti across the solid solution series using x-ray photoelectron spectroscopy and x-ray absorption spectroscopy. Using x-ray magnetic circular dichroism, we validate the microscopic model of magnetism and suggest a microscopic picture of the anti-site cation disorder for these samples. In Chapter5,we study the effects of controlled chemical disorder in SrTiO3 lattice, by performing site-specific doping of Mn in SrTiO3. We find that site specific Mn doping has decisive influence on their dielectric properties with qualitatively and quantitatively different behaviors between these doped samples .Using electron paramagnetic resonance experiments, we establish the site specific doping of Mn in SrTiO3 lattice. We find that while Mn doping at Ti site continues to remain paraelectric, Mn doping at the Sr site becomes a relaxor ferroelectric. We find samples having Mn substituted at both Sr and Ti sites simultaneously to be also relaxor ferroelectrics. Combining experiments with first principles calculations, we understand the origin for the high temperature dielectric properties of various Mn doped SrTiO3 samples. We show that Mn ions doped at the Sr sites off-centers and gives a significant dipolar contribution to their dielectric constants. While demonstrating the superior dielectric properties of Mn doped SrTiO3 ceramics ,we also elucidate their magnetic properties in details. In Chapter6,we study the effect of cation anti-site disorder on the magnetic and dielectric properties of undoped and Lu doped La2NiMnO6 samples. Using detailed spectroscopic characterizations of these samples with x-ray absorption experiments, coupled with d.c.magnetization and a.c.susceptibility measurements, we demonstrate that while the doped samples are ferromagnetic, the undoped samples exhibit re-entrant spin-glass magnetism. We also show that the dielectric properties of undoped La2NiMnO6,crys-tallizing in monoclinic and rhombohedral phases are distinctly different and we study their dielectric relaxations in details. We also demonstrate multiferroism in Lu doped La2NiMnO6 samples. In Appendix A, we study the electronic origin of ferroelectric polarization in the spin spiral compound ,MnWO4. Using x-ray absorption spectroscopy on synthesized MnWO4 samples, coupled with configuration interaction calculations, we establish quantitatively a significant population of Mn 3d states beyond the expected half filling and provide a critical insight into the significant presence of spin-orbit coupling and consequent finite polarization in this system. In Appendix B, we study charge-transfer doping in few-layer grapheme covered with electron acceptor (Tetracyanoethylene) and donor (Tetrathiafulvalene) molecules using x-ray photoelectron spectroscopy. We give quantitative estimates of the extent of doping in these samples and thereby elucidate the origin of unusual shifts of their Raman G bands in contrast to electrochemically doping schemes. In conclusion, we investigate, in this thesis, properties of different classes of compounds in presence of distinctly different kinds of disorder and establish the critical role of disorder in each case in tuning their desirable physical properties.

Le sujet de la topologie dans les oxydes, en particulier à la surface des oxydes de pérovskite comme SrTiO₃, ou à l'interface de LaA1O₃ / SrTiO₃ sera étudié dans cette thèse. Les deux matériaux, à leurs surfaces orientées (001), contiennent un état métallique limité à quelques nanomètres de la surface. De plus, nous montrerons qu'il existe certains croisements de trois bandes autour desquelles des perturbations vont provoquer l'apparition d'un spectre de bandes inversées et gappées. Ceux-ci conduiront à des états de bord topologiques qui peuvent être détectés via la supraconductivité induite comme dans le cas des puits quantiques topologiques ou des nanofils des supraconducteurs-semi-conducteurs. Ensuite, la surface orientée (111) de LaA1O₃ / SrTiO₃ sera étudiée lorsque les mesures de transport de Hall révèlent une transition de un à deux porteurs par dopage électrostatique. Une explication basée sur un modèle de liaisons fortes incluant des corrélations U de Hubbard sera proposée, ce qui donnera lieu à des croisements de bandes entre les sous-bandes favorisant les états topologiques. Enfin, une étude ab-initio de CaTiO₃ sera effectuée pour expliquer l'état métallique qui existe à sa surface (001) orientée et pour prédire le magnétisme dans le système. CaTiO₃ est différent des autres composés étudiés précédemment, en raison de la grande rotation et de l'inclinaison des octaèdres d'oxygène entourant le Ti, ce qui complique les faits. La structure avec et sans lacunes d'oxygène sera étudiée en profondeur pour fournir des détails sur la bande de conduction et leurs caractères orbitaux. / The subject of topology in oxides, in particular at the surfaces of perovskite oxides like SrTiO₃, or at the interface of LaA1O₃/SrTiO₃ will be investigated in this thesis. Both compounds, at their (001) oriented surfaces, contain a metallic state confined to a few nanometers at the surface. In addition, we will show that there exist certain three band crossings around which perturbations will cause an inverted and gapped band spectrum to appear. These will lead to topological edge states which can be detected via induced superconductivity as in the case of topological quantum wells or superconductor-semiconductor nanowires. Next, the (111) oriented surface of LaA1O₃/SrTiO₃ will be studied where Hall transport measurements reveal a one to two carrier transition via electrostatic doping. An explanation based on a tight binding modelling including Hubbard U correlations, will be proposed which will give rise to band crossings between sub-bands promoting topological states. Finally, an ab-initio study of CaTiO₃ will be performed to explain the metallic state which exists at its (001) oriented surface and to predict magnetism in the system. CaTiO₃ is different from the other compounds studied previously, due to the large rotation and tilting of the oxygen octahedra surrounding the Ti, which complicates the picture. The structure with and without oxygen vacancies will be studied in-depth to provide details about the conduction band and their orbital characters.

<p>Various transition metal oxides with interesting magnetic properties (often based on the perovskite structure) were prepared using conventional solid-state methodologies and fully characterized using a variety of techniques such as powder X-ray diffraction, variable temperature neutron diffraction, SEM-EDS, TEM-EDS, SQUID magnetometry and heat capacity measurements.</p> <p>One family of compounds that was investigated intensively were the 'pillared perovskites'. In this structure type, perovskite-like layers of comer shared octahedra are separated. by about 10 A by diamagnetic edge-shared octahedral dimer 'pillars'. Despite this long distance between layers, long-range order is present in both the La5Re3Co016 and La5Re3Ni016 members. In fact, a new magnetic structure was discovered for the Ni compound consisting of ferromagnetically ordered layers, coupled antiferromagnetically.</p> <p>In addition, for the first time, substitution of the 5+ ion within the layer was successful, yielding compounds with general formula, La5Re3-xTaxB016 (B =Mn, Fe, Co, Ni; x ~ 0.5). Surprisingly, despite replacing about half of the magnetic ions within the perovskite layers with non-magnetic tantalum, the materials had the same ordering temperatures and magnetic structures as their unsubstituted analogues. This observation is evidence that the longer interlayer coupling pathway is the key to long-range ordering in this structure type.</p> <p>The lanthanum rhenium oxide, La3Re20 10, involves the edge-shared octahedral dimer 'pillar' unit from the pillared perovskite structure, but with one unpaired electron per dimer unit. Prepared for the first time by solid-state synthesis, and studied magnetically in depth, long-range order was evident at 18 K. Theoretical investigations hinted that the magnetic structure consists of antiferromagnetically coupled chains of dimers, coupled antiferromagnetically.</p> <p>The magnetic properties of the double perovskite, SrLaRuNi06, were also explored for the first time. This study demonstrates the power of neutron diffraction at elucidating magnetic information, such as the ordering temperature and magnetic structure, despite the presence of a ferromagnetic impurity that dominated much of the measurements.</p> <p>The candidate's examination of the magnetism of the rock-salt oxides, Na2Cu2Te06 and Na3Cu2Sb06 has raised some controversy in the literature, as the exact nature of the one-dimensional order (either antiferromagnetic-antiferromagnetic or antiferromagnetic-ferromagnetic alternating linear chains) is uncertain. Again, theoretical calculations and comparison with other magnetic data can aide in the ultimate understanding of the overriding magnetism.</p> <p>This thesis has focused on the synthesis and study of transition metal oxides with interesting or unusual magnetic properties. In many cases, the compounds exhibited long-range magnetic order despite convoluted or non-existent magnetic superexchange pathways.</p> / Thesis / Doctor of Philosophy (PhD)

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The commercialization of lithium-ion batteries has played a pivotal role in the development of consumer electronics and electric vehicles. In recent years, much research has focused on the development and modification of the active materials of electrodes to obtain higher energies for a broader range of applications. High voltage spinel materials including LiNi_0.5Mn_1.5O_4-δ (LNMO) have been considered as promising cathode materials to address the increasing demands for improved battery performance due to their high operating potential, high energy density, and stable cycling lifetimes. In an effort to elucidate fundamental structure-property relationships, this thesis explores the tunable properties of single-crystal LNMO. Utilizing facile molten salt synthesis methods, the structural and electronic properties of LNMO can be well controlled. Chapter 2 of this thesis focuses on uncovering the effect of molten salt synthesis parameters including molten salt composition and synthetic temperature on the materials properties. A range of imaging, microscopic, and spectroscopic techniques are used to characterize structural and electronic properties which are investigated in tandem with electrochemical performance. Results indicate the Mn oxidation state is highly dependent on synthesis temperature and can dictate performance, while the molten salt composition strongly influences the particle morphology. In Chapter 3, we explore the concept of utilizing LNMO as a tunable support for heterogeneous metal nanocatalysts, where alteration of the support structure and electronics can have an influence on catalytic properties due to unique support effects. Ultimately, this work illustrates the tunable nature of single-crystal LNMO and can inform the rational design of LNMO materials for energy applications. / M.S. / The development of lithium-ion batteries has been fundamental to the expansion and prevalence of consumer electronics and electric vehicles in the twenty-first century. Despite their ubiquity, there is an ongoing drive by researchers to address the limitations and improve the quality and performance of lithium ion batteries. Much research has focused on altering the composition, structure, or properties of electrodes at the materials level to design higher achieving batteries. A fundamental understanding of how composition and structure effect battery performance is necessary to progress toward better materials. This thesis focuses on investigating the properties of LiNi_0.5Mn_1.5O_4-δ (LNMO). LNMO material is considered a promising cathode material to meet the increasing consumer demands for improved battery performance. Through the synthesis methods, the shape of individual particles and the global electronic properties of LNMO can be tuned. In this work, specific synthesis parameters are systematically tuned and the properties of the resultant LNMO materials are explored. Electrochemical testing also evaluates the performance of the materials and offers insights into how they may fair in real battery systems. In an effort to potentially recycle spent battery materials, LNMO is also utilized as a catalyst support. Alteration of shape and electronic properties of the LNMO support can influence the catalytic properties, or the ability of the material to enhance the rate of a chemical reaction. Overall, this thesis explores how LNMO can be tuned and utilized for different applications. This work provides insights for understanding LNMO properties and direction for the development of future battery materials.

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L'objectif de ce travail de thèse vise à étudier la conversion de la lignine dans des conditions oxydantes hydrothermales, par catalyse hétérogène. La lignine est l'une des principales constituantes des matériaux ligno-cellulosiques. Considérée comme déchet des procédés de valorisation de la cellulose, elle est majoritairement brûlée pour produire de l'énergie. De par sa structure de polymère phénolique, la lignine peut être considérée comme la principale source de noyaux aromatiques. Une méthodologie analytique complexe a, dans un premier temps, été mise en place pour permettre une caractérisation poussée des lignines et produits d'oxydation. Les lignines étudiées ont été extraites à partir de la paille par un procédé organosolv. Le procédé d'extraction influe sur les rendements mais aussi sur les structures et propriétés des différents produits. Les catalyseurs d'oxydation sont des oxydes divisés des métaux de transition, synthétisés par voie alginate. L'oxydation de la vanilline, composé modèle de la lignine, met en évidence des phénomènes d'oligomérisation des produits formés. Lors de l'oxydation des lignines, l'utilisation d'un catalyseur augmente les rendements et modifie les équilibres de dépolymérisation – oligomérisation. / The objective of this thesis is to study the conversion of lignin in oxidizing hydrothermal conditions, by heterogeneous catalysis. Lignin is among the main constituents of lignocellulose materials. Being considered like a waste of the cellulose valorization procedures, it is mostly burned to produce the energy. Taking into account its phenolic polymer structure, lignin can be considered as the main source of aromatic rings. Complex analytical methodology has initially been set up to allow a thorough characterization of lignins and oxidation products. Lignins were extracted from the straw by the organosolv procedure. The extraction process affects not only yields but also the structures and properties of products. The oxidation catalysts are transition metal oxides, synthesized by an alginate route. The oxidation of vanillin (lignin's model compound) shows the oligomerization phenomena of obtained products. In the oxidation of lignin, the use of a catalyst increases the yield and modifies the equilibrium of depolymerization - oligomerization.