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Synthesis and Characterization of Multifunctional Organic/ inorganic Hybrid Materials obtained by the "wet chemistry" approachKammoe, Astride Lorette 31 July 2015 (has links) (PDF)
Die vorliegende Arbeit fokussiert auf die Synthese von organisch/anorganischen Hybridmaterialien mit multifunktionalen Eigenschaften unter ausschliesslicher Darstellung dieser Materialen mit Hilfe des „wet chemistry“ Zugangs. Ausgehend von der Darstellung und Charakterisierung von isomorphen bzw. isostrukturellen Hybridmaterialien der allgemeinen Zusammensetzung catena-{[Me3NH][MCl3·2H2O]}n (Mtac) (MII = Mn, Co, Ni, Cu, tac = [Me3NH]Cl3·2H2O]) speziell mittels IR und UV/vis Spektroskopie ist beschrieben, wie sich aus diesen entsprechende bi-, tri-, und auch tetra-heterometallische Koordinationspolymere der allgemeinen Zusammenseztung {MxM´ytac}n, {MxM´yM´´ztac}n, {MxM´yM´´zM´´´ttac}n (MII = M ≠ M´≠ M´´≠ M´´´≠ M´´´´ und x, y, z, t als prozentualer Metallgehalt) herstellen lassen und welche limitierende Faktoren zu berücksichtigen sind. Leifähigkeitsmessungen an Einkristallen ausgewählter Koordinationspolymere werden vorgestellt. Zusätzlich werden die durch Rekristallisation von Nitac erhaltenen zwei verschiedenen Koordinationspolymere der Formel {[Me3NH]3{NiCl4}{NiCl3}}n und {[(Me3NH]{NiCl3}}n in Bezug auf ihre ungewöhnlichen strukturellen und magnetischen Eigenschaften vorgestellt und beschrieben.
Die durch Austausch von [Me3NH]+ Kationen gegen [Et3NH]+ bzw. protonierten aromatischen N-haltigen Kationen wie [2,2’-bipyH2]2+, [4,4’-bipyH2]2+ and [1,10-phenH2]2+ erhaltenen Reaktionsprodukte aus Umsetzungen mit Hilfe des “wet chemistry” Zugangs werden im Hinblick auf ihre Festkörperstrukturen beschrieben.
Die erfolgreiche Darstellung einer neuen Familie von perylentetracarboxylato-basierenden Komplexen, die teilweise hervorragende Löslichkeiten besitzen, wird beschrieben sowie die strukturellen, magnetischen und lumineszierenden Eigenschaften ausgewählter Vetreter. / The thesis presented here is focused on the synthesis of organic/ inorganic hybrid materials with multifunctional properties by means of the “wet chemistry” approach. The synthesis and characterization of hybrid materials with the general composition catena-{[Me3NH][MCl3·2H2O]}n (Mtac) (MII = Mn, Co, Ni, Cu, tac = [Me3NH]Cl3·2H2O]) is described. Due to their isomorphic and/ or isostructural character, bi-, tri-, and even tetra-heterometallic chains of the general formula {MxM´ytac}n, {MxM´yM´´ztac}n, {MxM´yM´´zM´´´ttac}n (MII = M ≠ M´≠ M´´≠ M´´´≠ M´´´´ and x, y, z, t is the percentage of each metal content) were synthesized and characterized. Limitating factors of the synthesis of these types of heterometallic coordination polymers are discussed. Furthermore, the conductive properties of selected representatives were investigated. Additionally, the products obtained from recrystallization of Nitac, two different novel 1D coordination polymers of the formula {[Me3NH]3{NiCl4}{NiCl3}}n and {[(Me3NH]{NiCl3}}n are described with respect to their structural and magnetic properties.
Efforts to replace the [Me3NH]+ cations of Mtac compounds by [Et3NH]+ cations as well as by protonated aromatic amines as [2,2’-bipyH2]2+, [4,4’-bipyH2]2+ and [1,10-phenH2]2+ are reported next with respect to the structural exploration of obtained hybrid materials by the “wet chemistry” approach.
Finally, the synthesis of a new family of perylene tetracarboxylate (ptc) based soluble complexes is reported. Structural, magnetic and luminescence properties of selected representatives of this new series of soluble ptc derivatives are reported.
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Magnetic superexchange interactions: trinuclear bis(oxamidato) versus bis(oxamato) type complexesAbdulmalic, Mohammad A., Aliabadi, Azar, Petr, Andreas, Krupskaya, Yulia, Kataev, Vladislav, Büchner, Bernd, Zaripov, Ruslan, Vavilova, Evgeniya, Voronkova, Violeta, Salikov, Kev, Hahn, Torsten, Kortus, Jens, Meva, Francois Eya'ane, Schaarschmidt, Dieter, Rüffer, Tobias 09 June 2015 (has links) (PDF)
The diethyl ester of o-phenylenebis(oxamic acid) (opbaH2Et2) was treated with an excess of RNH2 in MeOH to cause the exclusive formation of the respective o-phenylenebis(N(R)-oxamides) (opboH4R2, R = Me 1, Et 2, nPr 3) in good yields. Treatment of 1–3 with half an equivalent of [Cu2(AcO)4(H2O)2] or one equivalent of [Ni(AcO)2(H2O)4] followed by the addition of four equivalents of [nBu4N]OH resulted in the formation of mononuclear bis(oxamidato) type complexes [nBu4N]2[M(opboR2)] (M = Ni, R = Me 4, Et 5, nPr 6; M = Cu, R = Me 7, Et 8, nPr 9). By addition of two equivalents of [Cu(pmdta)(NO3)2] to MeCN solutions of 7–9, novel trinuclear complexes [Cu3(opboR2)(L)2](NO3)2 (L = pmdta, R = Me 10, Et 11, nPr 12) could be obtained. Compounds 4–12 have been characterized by elemental analysis and NMR/IR spectroscopy. Furthermore, the solid state structures of 4–10 and 12 have been determined by single-crystal X-ray diffraction studies. By controlled cocrystallization, diamagnetically diluted 8 and 9 (1%) in the host lattice of 5 and 6 (99%) (8@5 and 9@6), respectively, in the form of single crystals have been made available, allowing single crystal ESR studies to extract all components of the g-factor and the tensors of onsite CuA and transferred NA hyperfine (HF) interaction. From these studies, the spin density distribution of the [Cu(opboEt2)]2− and [Cu(opbonPr2)]2− complex fragments of 8 and 9, respectively, could be determined. Additionally, as a single crystal ENDOR measurement of 8@5 revealed the individual HF tensors of the N donor atoms to be unequal, individual estimates of the spin densities on each N donor atom were made. The magnetic properties of 10–12 were studied by susceptibility measurements versus temperature to give J values varying from −96 cm−1 (10) over −104 cm−1 (11) to −132 cm−1 (12). These three trinuclear CuII-containing bis(oxamidato) type complexes exhibit J values which are comparable to and slightly larger in magnitude than those of related bis(oxamato) type complexes. In a summarizing discussion involving experimentally obtained ESR results (spin density distribution) of 8 and 9, the geometries of the terminal [Cu(pmdta)]2+ fragments of 12 determined by crystallographic studies, together with accompanying quantum chemical calculations, an approach is derived to explain these phenomena and to conclude if the spin density distribution of mononuclear bis(oxamato)/bis(oxamidato) type complexes could be a measure of the J couplings of corresponding trinuclear complexes. / Dieser Beitrag ist aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.
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Χημεία, οπτικές και μαγνητικές ιδιότητες ετερομεταλλικών 3d/4f- μεταλλικών πλειάδωνΠολύζου, Χριστίνα 19 July 2012 (has links)
Τα ετερομεταλλικά σύμπλοκα μεταβατικών μετάλλων-λανθανιδίων (Ln) έχουν μεγάλη σημασία εξαιτίας των σημαντικών φυσικών (μαγνητικών και οπτικών) ιδιοτήτων τους. Μόνο λίγες πλειάδες ΝiII/LnIII και πολυμερή ένταξης έχουν αναφερθεί μέχρι σήμερα. Δύο γενικές προσεγγίσεις για τη σύνθεση συμπλόκων ΝiII/LnIII είναι: η στρατηγική που βασίζεται στη χρησιμοποίηση «μεταλλικών συμπλόκων ως υποκαταστατών» και η στρατηγική που βασίζεται στην «απλή ανάμιξη των συστατικών». Στην παρούσα Διπλωματική Εργασία εφαρμόζεται η δεύτερη κατά σειρά προσέγγιση για την παρασκευή των ακόλουθων ετερομεταλλικών συμπλόκων:
[Ni8Tb8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (1.xMeOH.yH2O)
[Ni8Ηο8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (2.xMeOH.yH2O)
[Ni8Υ8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (3.xMeOH.yH2O)
[Ni8Eu8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (4.xMeOH.yH2O)
[Ni8Sm8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (5.xMeOH.yH2O)
[Ni8Gd8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (6.xMeOH.yH2O)
[Ni4Er4(OH)2(Pao)14(PaoH)2](ClO4)4.4MeOH.2H2O (7.4MeOH.2H2O)
[Ni4Yb4(OH)2(Pao)14(PaoH)2](ClO4)4.4MeOH.2H2O (8.4MeOH.2H2O)
[NiDy(OH)2(Phpao)3(NO3)2(MeOH)].xMeOH (9.xMeOH)
{[NiDy(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (10.xMeOH.yH2O)
{[NiCe(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (11.xMeOH.yH2O)
{[NiPr(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (12.xMeOH.yH2O)
{[NiNd(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (13.xMeOH.yH2O)
{[NiSm(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (14.xMeOH.yH2O)
{[NiEu(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (15.xMeOH.yH2O)
{[NiTb(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (16.xMeOH.yH2O)
{[NiHo(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (17.xMeOH.yH2O)
{[NiEr(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (18.xMeOH.yH2O)
{[NiGd(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (19.xMeOH.yH2O)
όπου PaoH = 2-πυριδυλοαλδοξίμη, MepaoH = μέθυλο 2-πυριδυλοκετονοξίμη και PhpaoH = φαίνυλο 2-πυριδυλοκετονοξίμη.
Οι μοριακές και κρυσταλλικές δομές των συμπλόκων προσδιορίστηκαν με κρυσταλλογραφία ακτίνων-Χ επί μονοκρυστάλλου. Eπίσης μελετήθηκαν οι μαγνητικές και οι οπτικές ιδιότητες επιλεγμένων συμπλόκων. / Heterometallic transition metal-lanthanide (Ln) complexes are of great importance because of their interesting physical (magnetic and optical) properties. Only few ΝiII/LnIII clusters and coordination polymers have been reported to date. Two general approaches for the synthesis of ΝiII/LnIII complexes are: the «metal complexes as ligands» strategy and the «one pot procedure» strategy. Here, the second approach has been applied for the preparation of the following complexes:
[Ni8Tb8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (1.xMeOH.yH2O)
[Ni8Ηο8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (2.xMeOH.yH2O)
[Ni8Υ8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (3.xMeOH.yH2O)
[Ni8Eu8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (4.xMeOH.yH2O)
[Ni8Sm8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (5.xMeOH.yH2O)
[Ni8Gd8O(OH)4(Pao)28](ClO4)5(NO3).xMeOH.yH2O (6.xMeOH.yH2O)
[Ni4Er4(OH)2(Pao)14(PaoH)2](ClO4)4.4MeOH.2H2O (7.4MeOH.2H2O)
[Ni4Yb4(OH)2(Pao)14(PaoH)2](ClO4)4.4MeOH.2H2O (8.4MeOH.2H2O)
[NiDy(OH)2(Phpao)3(NO3)2(MeOH)].xMeOH (9.xMeOH)
{[NiDy(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (10.xMeOH.yH2O)
{[NiCe(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (11.xMeOH.yH2O)
{[NiPr(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (12.xMeOH.yH2O)
{[NiNd(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (13.xMeOH.yH2O)
{[NiSm(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (14.xMeOH.yH2O)
{[NiEu(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (15.xMeOH.yH2O)
{[NiTb(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (16.xMeOH.yH2O)
{[NiHo(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (17.xMeOH.yH2O)
{[NiEr(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (18.xMeOH.yH2O)
{[NiGd(Mepao)3(MepaoH)3](ClO4)2}2.xMeOH.yH2O (19.xMeOH.yH2O)
where PaoH = 2-pyridylaldoxime, MepaoH = methyl 2-pyridylketoxime and PhpaoH = phenyl 2-pyridylketoxime.
The molecular and crystal structures of the complexes have been determined by single-crystal X-ray crystallography. The magnetic and optical properties of selected complexes have also been studied.
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Síntese, caracterização e avaliação da atividade antimicrobiana de uma hidrazona e seus complexos metálicos / Synthesis, characterization and evaluation of the antimicrobial activity of a hydrazone and its metallic complexesReis, Jéssika Vieira dos 24 July 2018 (has links)
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Previous issue date: 2018-07-24 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / With the increasing resistance of microrganisms to available drugs, mainly in hospital
environments, the pharmaceutical industries have concentrated efforts in the research of new
versatility of their molecular structures and their biological effects achieved. The hydrazones
belong to an important class as they present a broad pharmacological profile whose properties have
been extensively studied in medicinal chemistry because of their chelating capacity and the role of
coordination in their biochemical mechanism of action. In this work a chemical ligand called J3
was synthesized which was complexed with copper nitrate (II), nickel nitrate, cadmium nitrate,
cobalt perchlorate and diphenyltin dichloride, being called: J3Cu, J3Ni, J3Cd, J3Co and J3Sn,
respectively. From the formation of the crystals, they were subjected to spectroscopic analysis of
single crystal X-ray diffraction and infrared spectroscopy, which confirmed the chemical structures
obtained from the ligand and its complexes. The biological activity of the six synthesized
compounds was evaluated through the microdilution method on 96 wells plates, and the
determination of the minimum inhibitory concentration (MIC) was determined by the density
measurement in ELISA reader after incubations of 24, 48, 72 and 96 hours in bacteria of the
species Escherichia coli and Staphylococcus aureus. The J3Cu, J3Cd and J3Sn compounds
presented moderate activity for the tested bacteria, whereas the J3 ligand and its J3Co and J3Ni
complexes did not inhibit 100% of the microrganisms in the tested concentrations. Through the
tests of determination of the minimum bactericidal concentration (MBC), it was concluded that the
complexes J3Sn and J3Cd presented bacteriostatic and bactericidal activity and J3Cu complex
presented activity bacteriostatic. / Com o crescente aumento da resistência de microrganismos aos fármacos disponíveis,
principalmente em ambiente hospitalar, as indústrias farmacêuticas têm concentrado esforços
na pesquisa de novos fármacos. Diversas classes de compostos orgânicos despertam o
interesse de pesquisadores devido à versatilidade de suas estruturas moleculares e seus
efeitos biológicos alcançados. As hidrazonas pertencem a uma classe importante pois
apresentam um amplo perfil farmacológico cujas propriedades têm sido extensivamente
estudadas na Química Medicinal em razão de sua capacidade quelante e do papel da
coordenação no seu mecanismo bioquímico de ação. Neste trabalho foi sintetizado um ligante
químico denominado J3 o qual foi complexado com Nitrato de Cobre (II), Nitrato de Níquel,
Nitrato de Cádmio, Perclorato de Cobalto e Dicloreto de difenilestanho, sendo denominados
de: J3Cu, J3Ni, J3Cd, J3Co e J3Sn, respectivamente. A partir da formação dos cristais, os
mesmos foram submetidos a análises espectroscópicas de difração de raios x em monocristal
e espectroscopia na região do infravermelho, que confirmaram as estruturas químicas obtidas
do ligante e seus complexos. Foi avaliada a atividade biológica dos seis compostos
sintetizados através do método de microdiluição em placas de 96 poços, e a determinação da
concentração inibitória mínima (CIM) foi determinada através da medida de densidade em
leitor de ELISA após incubações de 24, 48, 72 e 96 horas em bactérias das espécies
Escherichia coli e Staphylococcus aureus. Foi determinada a concentração bactericida mínima
para os compostos que apresentaram CIM contra as bactérias testadas. Os compostos J3Cu,
J3Cd e J3Sn apresentaram atividade moderada para as bactérias testadas, ao passo que o
ligante J3 e seus complexos J3Co e J3Ni não inibiram 100% dos microrganismos nas
concentrações testadas. Através dos testes de determinação da concentração bactericida
mínima, concluiu-se que os complexos J3Sn e J3Cd apresentaram atividade bacteriostática e
bactericida, o complexo J3Cu apresentou atividade bacteriostática.
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Extending the Search Space for Novel Physical Forms of Pharmaceuticals and Biomolecules using High-Pressure TechniquesSaouane, Sofiane 30 September 2015 (has links)
No description available.
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CHEMICAL AND STRUCTURAL CHARACTERIZATION OF FLUORAPATITE FROM THE POUDRETTE PEGMATITE, MONT SAINT-HILAIRE, QUEBEC, CANADAChappell, Joseph Caleb 14 January 2019 (has links)
No description available.
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Stabilization mechanism of molecular orbital crystals in IrTe2Ritschel, Tobias, Stahl, Quirin, Kusch, Maximilian, Trinckauf, Jan, Garbarino, Gaston, Svitlyk, Volodymyr, Mezouar, Mohamed, Yang, Junjie, Cheong, Sang-Wook, Geck, Jochen 19 March 2024 (has links)
Doped IrTe2 is considered a platform for topological superconductivity and therefore receives currently a lot of interest. In addition, the superconductivity in these materials exists in close vicinity to electronic order and the formation of molecular orbital crystals, which we explore here by means of high-pressure single crystal x-ray diffraction in combination with density functional theory. Our crystallographic refinements provide detailed information about the structural evolution as a function of applied pressure up to 42 GPa. Using this structural information for density functional theory calculations, we show that the local multicenter bonding in IrTe2 is driven by changes in the Ir-Te-Ir bond angle. When the electronic order sets in, this bond angle decreases drastically, leading to a stabilization of a multicenter molecular orbital bond. This unusual local mechanism of bond formation in an itinerant material provides a natural explanation for the different electronic orders in IrTe2. It further illustrates the strong coupling of the electrons with the lattice and is most likely relevant for the superconductivity in this material.
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Revealing the Magic in Silver Magic Number Clusters: The Development of Size-Evolutionary Patterns for Monolayer Coated Silver-Thiolate NanoclustersConn, Brian E. January 2016 (has links)
No description available.
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Intriguing High Z'' Cocrystals of EmtricitabinePalanisamy, V., Sanphui, P., Bolla, G., Narayan, Aditya, Seaton, Colin C., Vangala, Venu R. 12 August 2020 (has links)
Yes / Emtricitabine (ECB) afforded dimorphic cocrystals (Forms I, II) of benzoic acid (BA), whereas with p-hydroxybenzoic acid (PHBA), p-aminobenzoic acid (PABA) are resulted in as high Z'' cocrystals. Intriguingly, the Z'' of cocrystals are trends from two to fourteen based on the manipulation of functional groups on the para position of BA (where H atom is replaced with that of OH or NH2 group). ECB‒PABA cocrystal consists of six molecules each and two water molecules in the asymmetric unit (Z''=14) with 2D planar sheets represents the rare pharmaceutical cocrystal. The findings suggest that the increment of H bond donor(s) systematically via a suitable coformer are in correspondence with attaining high Z'' cocrystals. Further, solid state NMR spectroscopy in conjunction with single crystal X-ray diffraction are demonstrated as significant tools to enhance the understanding of the number of symmetry independent molecules in the crystalline lattice and provide insights to the mechanistic pathways of crystallization. / Department of Science and Technology (DST) Fund for improvement of S & T Infrastructure (FIST) with grant no. SR/FST/CST-266/2015(c) to PS and VP. AN and VV acknowledge the Government of India under National Overseas Scholarship (2012-13) and High Commission of India, London UK for PhD studentship.
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From molecular germanates to microporous Ge@C via twin polymerizationKitschke, Philipp, Walter, Marc, Rüffer, Tobias, Lang, Heinrich, Kovalenko, Maksym V., Mehring, Michael 31 March 2016 (has links) (PDF)
Four molecular germanates based on salicyl alcoholates, bis(dimethylammonium) tris[2-(oxidomethyl)phenolate(2-)]germanate (1), bis(dimethylammonium) tris[4-methyl-2-(oxidomethyl)phenolate(2-)]germanate (2), bis(dimethylammonium) tris[4-bromo-2-(oxidomethyl)phenolate(2-)]germanate (3) and dimethylammonium bis[2-tert-butyl-4-methyl-6-(oxidomethyl)phenolate(2-)][2-tert-butyl-4-methyl-6-(hydroxymethyl)phenolate(1-)]germanate (4), were synthesized and characterized including single crystal X-ray diffraction analysis. In the solid state, compounds 1 and 2 exhibit one-dimensional hydrogen bonded networks, whereas compound 4 forms separate ion pairs, which are connected by hydrogen bonds between the dimethylammonium and the germanate moieties. The potential of these compounds for thermally induced twin polymerization (TP) was studied. Germanate 1 was converted by TP to give a hybrid material (HM-1) composed of phenolic resin and germanium dioxide. Subsequent reduction with hydrogen provided a microporous composite containing crystalline germanium and carbon (Ge@C – C-1, germanium content ∼20%). Studies on C-1 as an anode material for Li-ion batteries revealed reversible capacities of ∼370 mA h gGe@C−1 at a current density up to 1384 mA g−1 without apparent fading for 500 cycles. / Dieser Beitrag ist aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.
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