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Hydrothermal Synthesis of Solid State Materials and Crystallography

Hydrothermal Synthesis of Solid State Materials and Crystallography PDF Author: Bahar Özmen
Publisher:
ISBN:
Category : Crystal growth
Languages : en
Pages : 154

Book Description
The structure solution of the new polyoxovanadate compound ([V16O31(OH)7]Cl.15H2O), has been done by the SHELX crystal solution software. The compound was synthesized solvothermally at 170 C in the Northwestern University.The compound crystallizes in the space group C2/c of the monoclinic system with eight formula units in a cell of dimensions a = 18.070 (2) A, b = 17.414 (2) A, c = 15.1154 (18) A, .= 97.696 (2), V= 4713.8 (10) A3 (T = 153 K). The structure is composed of vanadium-oxygen clusters encapsulating Cl anion. Each of the V centers has square pyramidal geometry coordinated by five O atoms. The 16 (VO5) units are fused together through common edges to form (V16O38) cage with Cl anion in the middle.The single crystals of the [Ni(en)3(VO3)2] compound was synthesized by hydrothermal method. [Ni(en)3(VO3)2] compound is in the crystal system of hexagonal and in the space group P61. The unit cell parameters are a = 8.9940 (13) A, b = 8.9940 (13) A, c = 34.001 (7) A and alpha = 90 , B = 90 , y = 120 . The structure is composed of VO4 tetrahedras which are joined with others by sharing corners into infinite chains running along the c axis. The complex cation [Ni(en)3]2+ are located between the chains The chain in the compound has a repetitive sequence of 12-nuclear corner-sharing tetrahedras. The compound was synthesized at 160 C for 3 days in the steel reaction autoclaves which have PTFE (Polytetrafluoroethylene) cups in them.By the reaction of the reactants NH4VO3, Ni(NO3)2.6H2O, H3BO3 with H2O the orange crystals of NH4(V3O8) and the green unknown crystals were obtained at 160 C in 3 days..By the reaction of the reactants NaVO3, Ni(NO3)2.6H2O, H3BO3, NH2CH2CH2NH2, with the solvents H3PO4 and H2O the green bulk unknown crystals were obtained at 160 C in 3 days.the reaction of the reactants B4K2O7.H2O, KVO3 with H2O and NH2CH2CH2NH2 brown unknown crystals were obtained at 170 C in 5 days.We have also done some crystal growth studies in our laboratory. There are several known compounds as CoV2O6(H2O)2, Co(VO)2(PO4)2(H2O)4, which were also synthesized in our laboratory with good yields. These crystals were synthesized with other methods and characterized. However we were able to grow their crystals in good shape and size by using hydrothermal method. CoV2O6(H2O)2 was obtained from the reaction of NH4VO3, Co(NO3)2.6H2O and H3BO3. The compound crystallizes in the space group Pnma (62) of the orthorhombic system in a cell of dimensions, a = 5.572 A,b = 10.70 A, c = 11.860 A, alpha = Beta = y = 90 , V = 707.69 A3. CoV2O6(H2O)2 was prepared in a steel autoclave by using ultra pure water as the solvent and heated at 160 C for 3 days. Red prism shaped crystals of the reported materials were obtained with the orange plates in a red-orange crystalline powder. The single crystal XRD results showed that the orange plates have the formula of NH4(V3O8) which crystallizes in the space group P21/m (11) of the monoclinic system in a cell of dimensions a = 4.999 A, b = 8.423 A, c = 7.849 A, B = 96.426 , V = 328.44 A3. It has been shown that CoV2O6(H2O)2 compound can also be synthesized by the reaction of NaVO3, GeO2, H3BO3, CoCl2.6H2O with H2O as the solvent.The green crystals of the compound Co(VO)2(PO4)2(H2O)4 were synthesized from the reaction of V2O5, H2C2O4.2H2O, CoCl2.6H2O with the solvents H3PO4 and H2O at 160 0C for 3 days. The compound crystallizes in the space group I4/mmm (139) of the tetragonal system in a cell of dimensions a = 6.264 A, c = 13.428 A, alpha = B = y = 90 , V = 526.88 A3.

Hydrothermal Synthesis of Solid State Materials and Crystallography

Hydrothermal Synthesis of Solid State Materials and Crystallography PDF Author: Bahar Özmen
Publisher:
ISBN:
Category : Crystal growth
Languages : en
Pages : 154

Book Description
The structure solution of the new polyoxovanadate compound ([V16O31(OH)7]Cl.15H2O), has been done by the SHELX crystal solution software. The compound was synthesized solvothermally at 170 C in the Northwestern University.The compound crystallizes in the space group C2/c of the monoclinic system with eight formula units in a cell of dimensions a = 18.070 (2) A, b = 17.414 (2) A, c = 15.1154 (18) A, .= 97.696 (2), V= 4713.8 (10) A3 (T = 153 K). The structure is composed of vanadium-oxygen clusters encapsulating Cl anion. Each of the V centers has square pyramidal geometry coordinated by five O atoms. The 16 (VO5) units are fused together through common edges to form (V16O38) cage with Cl anion in the middle.The single crystals of the [Ni(en)3(VO3)2] compound was synthesized by hydrothermal method. [Ni(en)3(VO3)2] compound is in the crystal system of hexagonal and in the space group P61. The unit cell parameters are a = 8.9940 (13) A, b = 8.9940 (13) A, c = 34.001 (7) A and alpha = 90 , B = 90 , y = 120 . The structure is composed of VO4 tetrahedras which are joined with others by sharing corners into infinite chains running along the c axis. The complex cation [Ni(en)3]2+ are located between the chains The chain in the compound has a repetitive sequence of 12-nuclear corner-sharing tetrahedras. The compound was synthesized at 160 C for 3 days in the steel reaction autoclaves which have PTFE (Polytetrafluoroethylene) cups in them.By the reaction of the reactants NH4VO3, Ni(NO3)2.6H2O, H3BO3 with H2O the orange crystals of NH4(V3O8) and the green unknown crystals were obtained at 160 C in 3 days..By the reaction of the reactants NaVO3, Ni(NO3)2.6H2O, H3BO3, NH2CH2CH2NH2, with the solvents H3PO4 and H2O the green bulk unknown crystals were obtained at 160 C in 3 days.the reaction of the reactants B4K2O7.H2O, KVO3 with H2O and NH2CH2CH2NH2 brown unknown crystals were obtained at 170 C in 5 days.We have also done some crystal growth studies in our laboratory. There are several known compounds as CoV2O6(H2O)2, Co(VO)2(PO4)2(H2O)4, which were also synthesized in our laboratory with good yields. These crystals were synthesized with other methods and characterized. However we were able to grow their crystals in good shape and size by using hydrothermal method. CoV2O6(H2O)2 was obtained from the reaction of NH4VO3, Co(NO3)2.6H2O and H3BO3. The compound crystallizes in the space group Pnma (62) of the orthorhombic system in a cell of dimensions, a = 5.572 A,b = 10.70 A, c = 11.860 A, alpha = Beta = y = 90 , V = 707.69 A3. CoV2O6(H2O)2 was prepared in a steel autoclave by using ultra pure water as the solvent and heated at 160 C for 3 days. Red prism shaped crystals of the reported materials were obtained with the orange plates in a red-orange crystalline powder. The single crystal XRD results showed that the orange plates have the formula of NH4(V3O8) which crystallizes in the space group P21/m (11) of the monoclinic system in a cell of dimensions a = 4.999 A, b = 8.423 A, c = 7.849 A, B = 96.426 , V = 328.44 A3. It has been shown that CoV2O6(H2O)2 compound can also be synthesized by the reaction of NaVO3, GeO2, H3BO3, CoCl2.6H2O with H2O as the solvent.The green crystals of the compound Co(VO)2(PO4)2(H2O)4 were synthesized from the reaction of V2O5, H2C2O4.2H2O, CoCl2.6H2O with the solvents H3PO4 and H2O at 160 0C for 3 days. The compound crystallizes in the space group I4/mmm (139) of the tetragonal system in a cell of dimensions a = 6.264 A, c = 13.428 A, alpha = B = y = 90 , V = 526.88 A3.

Preparative Methods in Solid State Chemistry

Preparative Methods in Solid State Chemistry PDF Author: Paul Hagenmuller
Publisher: Elsevier
ISBN: 0323144365
Category : Science
Languages : en
Pages : 621

Book Description
Preparative Methods in Solid State Chemistry deals with the preparative methods used in solid state chemistry and highlights the importance of the chemist's role in preparing materials of desired quality as well as obtaining materials according to the requirements of the user such as the physicist. Topics covered range from high-pressure techniques in preparative chemistry to methods of growing single crystals of high-melting-point oxides. This book is comprised of 14 chapters and begins with an overview of possibilities for high-pressure synthesis, as well as the methods used to obtain high pressures, including transmission by gaseous or liquid fluids or in the solid state. The method of shock waves is then considered both from the point of view of thermodynamics and thermoelasticity, along with the possibility of using superpressures for evidently revolutionary applications. Subsequent chapters focus on the synthesis of single crystals of refractory oxides either at high temperatures (essentially liquid-solid transformations) or at lower temperatures in the presence of a solvent or a chemical reagent. The production of single crystals by electrolytic reduction in molten salts is also described. Numerous examples of vapor transport reactions in a temperature gradient are presented. This monograph should be of interest to chemists and students of solid state chemistry.

Synthesis, Structural and Spectroscopic Characterization of New Polychalcogenide Complexes of Indium and Thallium, and Their Applicaton as Precursors to Solid State Materials

Synthesis, Structural and Spectroscopic Characterization of New Polychalcogenide Complexes of Indium and Thallium, and Their Applicaton as Precursors to Solid State Materials PDF Author: Sandeep S. Dhingra
Publisher:
ISBN:
Category : Chalcogenides
Languages : en
Pages : 352

Book Description


Perovskite Materials

Perovskite Materials PDF Author: Likun Pan
Publisher: BoD – Books on Demand
ISBN: 9535122452
Category : Technology & Engineering
Languages : en
Pages : 652

Book Description
The book summarizes the current state of the know-how in the field of perovskite materials: synthesis, characterization, properties, and applications. Most chapters include a review on the actual knowledge and cutting-edge research results. Thus, this book is an essential source of reference for scientists with research fields in energy, physics, chemistry and materials. It is also a suitable reading material for graduate students.

Hydrothermal Synthesis of Crystals

Hydrothermal Synthesis of Crystals PDF Author: A. N. Lobachev
Publisher: Springer
ISBN:
Category : Science
Languages : en
Pages : 182

Book Description


Crystallization Processes under Hydrothermal Conditions

Crystallization Processes under Hydrothermal Conditions PDF Author: A. N. Lobachev
Publisher: Springer Science & Business Media
ISBN: 1468475231
Category : Science
Languages : en
Pages : 256

Book Description
This collection conta ins the results of a number of investiga tions which have been carried out in the Hydrothermal Synthesis Laboratory of the Institute of Crystallography, Academy of Sciences of the USSR; it constitutes a continuation of an earlier collection which appeared in 1968: Hydrothermal Synthesis of Crystals. Problems associated with the synthesis of oxides, simple and complex sulfides, carbonates, silicates, and germanates are consid ered, and a great deal of factual material relating to the growth of single crystals of some of these compounds on a seed is presented. Some of the articles pay special attention to the kinetic asp ect of the growth of crystals; the conditions of growth are relat ed to the morphological characteristics of the growing faces, and the relationship between the habit of the crystals and the oomposi tion and constitution of the solutions is considered. A fair number of articles are concerned with the crystalliza tion of new compounds, most of which have now been synthesized under hydrothermal conditions for the very first time; these in clude ternary chalcohalides of composition AVBvIVVII. zirconates, lithium silicates, and germanates. The collection also contains a description of the apparatus used for precision measurements at high temperatures and pres sures. We hope that this publication will present a better idea of the special characteristics of the hydrothermal method of synthes izing and .growing crystals, and will prove useful to all those in terested in this field of knowledge.

Crystals for Magnetic Applications

Crystals for Magnetic Applications PDF Author: C.J.M. Rooijmans
Publisher: Springer Science & Business Media
ISBN: 364267061X
Category : Science
Languages : en
Pages : 146

Book Description
Springer-Verlag, Berlin Heidelberg, in conjunction with Springer-Verlag New York, is pleased to announce a new series: CRYSTALS Growth, Properties, and Applications The series will present critical reviews of recent developments in the field of crystal growth, properties, and applications. A substantial portion of the new series will be devoted to the theory, mechanisms, and techniques of crystal growth. Occasionally, clear, concise, complete, and tested instructions fqr growing crystals will be published, particularly in the case of methods and procedures that promise to have general applicability. Responding· to the ever-increasing need for crystal substances in research and industry, appropriate space will be devoted to methods of crystal characterization and analysis in the broadest sense, even though reproducible results may be expected only when structures, microstructures, and composition are really known. Relations among procedures, properties, and the morphology of crystals will also be treated with reference to specific aspects of their practical application. In this way, the series will bridge the gaps between the needs of research and industry, the pos sibilities and limitations of crystal growth, and the properties of crystals. Reports on the broad spectrum of new applications - in electronics, laser tech nology, and nonlinear optics, to name only a few - will be of interest not only to industry and technology, but to wider areas of applied physics as well and to solid state physics in particular. In response to the growing interest in and importance of organic crystals and polymers, they will also be treated.

Frontiers Of Solid State Chemistry, Proceedings Of The International Symposium On Solid State Chemistry In China

Frontiers Of Solid State Chemistry, Proceedings Of The International Symposium On Solid State Chemistry In China PDF Author: Jiesheng Chen
Publisher: World Scientific
ISBN: 981448783X
Category : Science
Languages : en
Pages : 606

Book Description
Solid state chemistry is a multidisciplinary field that deals with the synthesis, structural characterization and properties of various solids, and it has been playing a more and more important role in the design and preparation of advanced materials. This book includes the excellent research results recently obtained by a wide spectrum of solid state chemists both from China and from abroad. Among the distinguished contributors are C N R Rao, M Greenblatt and Y T Qian, to name a few. A variety of subjects representing the frontiers of solid state chemistry — which are categorized into solids with electrical, optical and magnetic properties; porous solids and catalysts; hybrid inorganic-organic solids; solid nanomaterials; and new synthetic methods and theory — are presented. This book will benefit readers who are interested in the chemistry and physics of solids, as well as materials scientists and engineers.The proceedings have been selected for coverage in:• Chemistry Citation IndexTM• Index to Scientific & Technical Proceedings (ISTP CDROM version / ISI Proceedings)

Crystallography of Modular Materials

Crystallography of Modular Materials PDF Author: Giovanni Ferraris
Publisher: OUP Oxford
ISBN: 0191545872
Category : Science
Languages : en
Pages : 384

Book Description
This is the first book to provide a comprehensive treatment of theories and applications in the rapidly expanding field of the crystallography of modular materials. Molecules are the natural modules from which molecular crystalline structures are built. Most inorganic structures, however, are infinite arrays of atoms and some kinds of surrogate modules, e.g. co-ordination polyhedra, are usually used to describe them. In recent years the attention has been focused on complex modules as the basis for a systematic description of polytypes and homologous/polysomatic series (modular structures). This representation is applied to the modelling of unknown structures and understanding nanoscale defects and intergrowths in materials. The Order/Disorder (OD) theory is fundamental to developing a systematic theory of polytypism, dealing with those structures based on both ordered and disordered stacking of one or more layers. Twinning at both unit-cell and micro-scale, together with disorder, causes many problems, "demons", for computer-based methods of crystal structure determination. This book develops the theory of twinning with the inclusion of worked examples, converting the "demons" into useful indicators for unravelling crystal structure. In spite of the increasing use of the concepts of modular crystallography for characterising, understanding and tailoring technological crystalline materials, this is the first book to offer a unified treatment of the results, which are spread across many different journals and original papers published over the last twenty years.

Synthesis Methods in Solid-State Chemistry

Synthesis Methods in Solid-State Chemistry PDF Author: Riadh Marzouki
Publisher:
ISBN:
Category : Electronic books
Languages : en
Pages : 0

Book Description
The synthesis of single crystal is an area of intense activity in the materials science. The obtaining of the single crystal with sufficient dimension for X-ray diffraction depends on several factors including the chemical composition, crystal structure of the reagents, and physical parameters (temperature and pressure). In this context, this chapter is dedicated to the description of the most common synthesis methods of single crystal in the solid-state chemistry: solid-state method, hydrothermal, and slow evaporation at room temperature. Same other materials can be obtained at high pressure. There are also some physical techniques to grow single crystal, each technique is specific for specific materials.