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Muhammad Ali, 2021, doktorska disertacija

Opis: In this thesis, we study the structure and optical transmission properties of the twist-bend nematic liquid crystalline phase, made of bent dimers, confined in thin planar cells. Confinement leads to the formation of a periodic modulated structure, the formation of which is explained as follows. The twist-bend nematic phase is characterized by a heliconical modulation of the molecular long axes. Due to a short pitch of modulation (approximately 10 nm), the twist-bend nematic phase behaves as a pseudo-layered medium. At temperatures below the nematic – twist-bend nematic phase transition, the heliconical pitch and thus the thickness of the pseudo-layers reduces, which leads to a two-dimensional undulation of pseudo-layers in the direction perpendicular to the cell surfaces and along the surfaces. The undulated structure is responsible for a stripe texture observed under a polarizing microscope and acts as a diffraction grating. We constructed theoretical models to predict the pseudo-layer structure of a confined twist-bend nematic phase and to describe the properties of light diffracted on such cells. The free energy of the two-dimensional pseudo-layer structure of the twist-bend nematic phase is expressed in terms of the nematic director field, by which we describe the direction of the heliconical axis, and a complex smectic order parameter, the gradient of which gives the direction of the layer normal. At first, we assume that pseudo-layers are perpendicular to the surfaces (bookshelf geometry) and find a stable structure by assuming an ansatz for the pseudo-layer displacement from the bookshelf geometry and then minimizing the free energy at a very strong and very weak surface anchoring. In this way a threshold condition for the onset of the modulated structure is obtained, as well as the amplitude and period of modulation. Next, we assume that, at the onset of the twist-bend nematic phase, pseudo-layers are formed at some angle (pre-tilt) with respect to the surface. We find that in both cases, the bookshelf and pre-tilted one, the calculated period of modulation far from the phase transition is always approximately twice the cell thickness, which agrees with experimental observations. The properties of light diffracted by the spontaneously formed grating were studied both experimentally and theoretically. We measured the intensity and polarization properties of the first two orders of the diffracted light and the temperature dependence of the polarization of the second order diffraction peaks. To predict the observed properties of the diffracted light and to simplify the description of such gratings, we consider different preliminary models of a one-dimensional spatial variation of the optic axis, the direction of which is given by two angles. A transfer matrix method is used and a good agreement between the experimental and theoretical results is obtained. In a more comprehensive approach, we determine the spatial variation of the optic axis direction from the modeled structure. The electric field in the diffracted light is obtained by using the transfer matrix method and beam propagation method. In the case of a pre-tilt of the pseudo-layers and very strong surface anchoring both methods give good qualitative agreement with experimental results, only in the case of the temperature dependence of the second order diffraction peaks, a more complex beam propagation method is superior to the transfer matrix method. The thesis is divided into three parts. In the first part, we focus on the physical properties of the twist-bend nematic phase and its structure in thin planar cells. In the second part, a continuum model is proposed and finally, the properties of diffracted light are discussed and theoretically predicted by using the beam propagation method and transfer matrix method.
Ključne besede: Bent-dimer liquid crystals, twist-bend nematic phase, undulation of pseudo-layers, polarization, diffraction grating, beam propagation method, transfer matrix method.
Objavljeno: 21.10.2021; Ogledov: 6; Prenosov: 1
.pdf Celotno besedilo (10,65 MB)

Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrate
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Amalija Golobič, Marta Kasunič, Mihael Drofenik, 2012, izvirni znanstveni članek

Opis: This paper reports on the synthesis of a new hydroxylammonium fluoroferrate, with the formula $(NH_3OH)_3FeF_6$, obtained after dissolving iron powder in hydrofluoric acid and adding solid $NH_3OHF$. This new compound has been characterized by chemical and thermal analysis, single-crystal X-ray diffraction, and magnetic measurements. The title compound crystallizes trigonal, R3c, with cell parameters a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. The structure consists of $NH_3OH^+$ cations and isolated $FeF_6^{3–}$ octahedra in which the central ion lies on a threefold axis. The oxygen and nitrogen atoms of the hydroxylammonium cations are donors of hydrogen bonds to fluoride anions, resulting in a network of hydrogen bonds between counterions. The effective magnetic moment $µ_{eff}$ = 5.8 BM was calculated and perfectly matches the expected value of high-spin Fe(III) ions. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction.
Ključne besede: inorganic chemistry, crystallography, coordination compounds, synthesis, crystal structure, characterization of compounds, determination of the structure of compounds, X-ray diffraction, magnetic measurements, thermal analysis, TG, DSC, hydrogen bond, metal complexes, hydroxylammonium fluoromethalatehydroxylammonium, fluoroferrate
Objavljeno: 25.08.2017; Ogledov: 1163; Prenosov: 53
.pdf Celotno besedilo (198,42 KB)
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Synthesis and characterisation of hydroxylammonium fluorochromate
Matjaž Kristl, Mihael Drofenik, Ljubo Golič, Amalija Golobič, 2003, izvirni znanstveni članek

Opis: Reactions in the system $Cr – NH_3OHF – HF – H_2O$ were investigated. Green crystals of a new compound with the formula $(NH_3OH)_3CrF_6$ have been isolated from the water solution and characterized by chemical analysis. The compound crystallizes as triclinic, P-1, with cell parameters: a = 6.5461(2) Å, b = 6.9347(2) Å, c = 9.4072(3) Å, α = 86.772(1)°, β = 83.804(1)°, γ = 70.283(1)°. The effective magnetic moment, $µ_{eff}$ = 3.82 BM, was calculated from magnetic susceptibility measurements in the temperature range 80-290 K. The thermal decomposition of the compound was studied by TG and DSC analysis. $(NH_3OH)_3CrF_6$ decomposes above 125 °C in three steps and the residue has been identified by X-ray powder diffraction as $α – Cr_2O_3$.
Ključne besede: inorganic chemistry, structural chemistry, crystalline structure, coordination compounds, synthesis, inorganic reactions, thermal decomposition, characterization of compounds, TG, DSC, X-ray diffraction, chromium complexes, hydroxylammonium fluoro chromates, crystals
Objavljeno: 25.08.2017; Ogledov: 970; Prenosov: 83
.pdf Celotno besedilo (206,45 KB)
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Ammoniumbis(hydroxylammonium) pentafluoridooxidovanadate(IV)
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Mihael Drofenik, Anton Meden, 2008, izvirni znanstveni članek

Opis: Turquoise crystals of a new hydroxylammonium compound with the formula $NH_4(NH_3OH)_2[VOF_5]$ have been synthesized by the reaction of solid $NH_3OHF$ and the aqueous solution of vanadium in HF. The compound crystallizes monoclinic, $P2_1/n$, with cell parameters: a = 10.5658(2) Å, b = 6.6143(1) Å, c = 11.6618(2) Å, β = 96.282(1). Magnetic susceptibility was measured using a SQUID device over a temperature range 2–300 K at magnetic field $10^3 Oe$ giving the result $µ_{eff}$ = 1.65 BM. The thermal decomposition was studied by TG and DSC analysis. $NH_4(NH_3OH)_2[OF_5V]$ decomposes above 354 K in three steps, obtaining $NH_4VOF_3$ after the first step and $V_2O_5$ as the final residue.
Ključne besede: hydroxylammonium fluorovanadates, x-ray powder diffraction, x-ray structure determination, thermal analysis
Objavljeno: 17.08.2017; Ogledov: 890; Prenosov: 67
.pdf Celotno besedilo (218,95 KB)
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Measurement of strain caused by residual stresses in a welded joint using neutron diffraction
Nenad Gubeljak, Jelena Vojvodič-Tuma, Hans-Georg Preismeyer, 1999, izvirni znanstveni članek

Opis: The distribution and amount of residual stresses can significantly contrubute to the fatigue fracture behaviour of welded joints in structures. Interior residual stresses, which interact with the plane strain state, are more dangerous than residual stresses at the surface of the welded joint. If the surface of the welded joint is mechanically treated (e.g. shapering), then significant differences between the stress stated at the surface and within the volume occur. Hence, different non-destructive methods (e.g. gamma radiation, neutron diffraction) have been developed to determine strains caused by residual stresses in the volume of polycrystalline materials. However, the measurement of strains caused by residual stresses becomes difficult for large samples. In this paper the measurement procedure on a sample taken from the weld joint is presented and the effecet of residual stresses on fatigue crack propagation is assessed for low and high cycle loading fatigue.
Ključne besede: zaostale napetosti, zvarni spoj, neutronski lom žarkov, utrujenostno širjenje razpoke, neutron diffraction method, residual stresses, fatigue crack propagation, weld joint
Objavljeno: 10.07.2015; Ogledov: 710; Prenosov: 17
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Hydroxylammonium fluorogermanates
Irena Ban, Matjaž Kristl, Mihael Drofenik, Arkadije Popović, 2004, izvirni znanstveni članek

Opis: A new hydroxylammonium compound (NH3OH)2GeF6, has been synthesized by the addition of solid NH3OHF to a solution of GeO2 dissolved in 20% HF. The compound was characterized by chemical analysis and X-ray powder diffraction, the thermal decomposition was studied by thermal analysis and mass spectrometry. (NH3OH)2GeF6 crystallizes monoclinic. Two endothermic and two exothermic peaks have been observed on the DSC curve, the decomposition product at 500 °C is GeO2.
Ključne besede: inorganic chemistry, synthesis, characterisation, hydroxylammonium fluorogermanates, x-ray powder diffraction, mass spectroscopy, thermal analysis
Objavljeno: 01.06.2012; Ogledov: 1875; Prenosov: 79
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Crystal-structure and Mössbauer studies of Li[sub]1.746]Nd[sub]4.494FeO9[sub]9.493
Mihael Drofenik, Irena Ban, Darko Makovec, Darko Hanžel, Amalija Golobič, Ljubo Golič, 2007, izvirni znanstveni članek

Opis: The ▫$Li_1.746Nd_4.494FeO_9.493$▫ (LNF) ternary phase, located in the ▫$Li_2O$▫-rich part of the ▫$Li_2O-Nd_2O_3-Fe_2O_3$▫ system, crystallizes with a cubic unit cell of dimension and the space group Im3m. Refinement on F resulted in R=1.9%. The structure is comprised of a network of corners, edges and faces sharing the coordination polyhedra of neodymium. In between this skeleton the regular octahedra of oxygen-coordinated iron and trigonal prisms of lithium are located. The Mössbauer spectra revealed the presence of ▫$Fe^3+$▫, ▫$Fe^4+$▫ and ▫$Fe^5+$▫ ions distributed on two symmetry-independent lattice positions.
Ključne besede: crystal structure, ternary compounds, single-crystal X-ray diffraction, Mössbauer spectroscopy, iron oxidation state, kristalna struktura, ternarne spojine, rentgenska difrakcija, Mössbauerjeva spektroskopija, rentgenska strukturna analiza
Objavljeno: 01.06.2012; Ogledov: 1683; Prenosov: 38
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Subsolidus phase equilibria and the Li[sub]5Nd[sub]4FeO[sub]10 phase in the Li[sub]2O-Nd[sub]2O[sub]3-Fe[sub]2O[sub]3 system
Irena Ban, Mihael Drofenik, Danilo Suvorov, Darko Makovec, 2005, izvirni znanstveni članek

Opis: A survey of the subsolidus phase equilibria in the system Li2O-Nd2O3-Fe2O3 wasmade at subsolidus temperatures in the range 1000-1050 °C. A ternary phase was identified. The phase is centered on Li5Nd4FeO10, with a cubic lattice a =11.9494 A. The compound melts incongruently at 1105 °C. The magnetic susceptibility was measured in the temperature range 4-300 K. The compound is paramagnetic in the temperature range 150-300 K and follows the Curie-Weiss law. At about TN = 10 K, a long-range magnetic ordering is observed.
Ključne besede: lithium ferrites, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, magnetic properties, phase equilibrium
Objavljeno: 01.06.2012; Ogledov: 1655; Prenosov: 24
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Preparation of enantiomers using high pressure technologies
Paul Thorey, 2010, doktorska disertacija

Opis: The study of two different methods of obtaining chiral alcohols is proposed herein. The requirement of the relatively new paradigm of green chemistry associated with clean technologies such as biocatalysis or non-conventional solvents, dense gases, was focused at. Indeed, the two methods of production of chiral alcohols were: - the conversion of acetophenone into (R)-1-phenylethanol in dense gases catalysed by Lactobacillus brevis alcohol dehydrogenase and its coenzyme, NADP/H; - the resolution of (±)-trans-1,2-cyclohexanediol by cocrystal formation with tartaric acid followed by supercritical extraction. In both cases high enantiopurities were achieved (ee>99%).
Ključne besede: High-pressure technologies, enantiomers, green chemistry, R-1-phenylethanol, Lactobacillus brevis, alcohol dehydrogenase, NADP, liquid propane, enzyme deactivation, resolution, trans-1, 2-cyclohexanediol, tartaric acid, cocrystal, supercritical carbon dioxide, extraction, X-ray diffraction, differential scanning calorimetry
Objavljeno: 02.02.2011; Ogledov: 2409; Prenosov: 89
.pdf Celotno besedilo (6,25 MB)

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