Studium lokální struktury hexagonálních feritů metodami NMR

Title: Local structure of hexagonal ferrites studied by NMR Author: Karel Kouřil Department/Institute: Department of Low Temperature Physics Supervisor of the doctoral thesis: prof. RNDr. Helena Štěpánková, CSc. Abstract: Hexagonal ferrites of M, W, X and Y structure types were studied by means of NMR, electronic structure calculations and magnetoelectric experi- ments. Presented results deal with cation distribution, localization of ferrous ions, interpretation of NMR spectra of studied materials and effects of size reduction. In oriented layers M type strontium ferrite and submicron particles of M type barium ferrite pronounced effects of reduced size were observed on 57 Fe NMR spectra. Performance of magnetoelectric barium-strontium Y type hexaferrites with divalent zinc cations improved upon thermal treatment of samples while distribution of zinc was not significantly altered. In Sc sub- stituted BaM, Sc content was found to be uniform throughout TSSG grown crystal. In LaSrM systems electron localization in 2a sublattice was observed, co-substitution with La+Zn, La+Co and La+Cu was found to lead to partial charge compensation. In strontium ferrites of type W and X localization of ferrous ions in octahedral sites in SS block pair was observed. Keywords: NMR, hexagonal ferrites, structure,...Název Práce: Studium lokální struktury hexagonálních feritů metodami NMR Autor: Karel Kouřil Katedra/Ústav: Katedra fyziky nízkých teplot Vedoucí doktorské práce: prof. RNDr. Helena Štěpánková, CSc. Abstrakt: Práce je věnována hexagonálním feritům strukturních typů M, W, X a Y. Tyto materiály byly studovány pomocí NMR, výpočtů elektronové struktury a magnetoelektrických experimentů. Byly získány výsledky týkající se distribuce kationtů, lokalizace železnatých iontů, interpretace NMR spekter studovaných materiálů a důsledků redukce velikosti částic. V tenkých vrstvách strontnatého M feritu a v submikronových částicích barnatého M feritu byla 57 Fe NMR spektra ovlivněna efekty snížené velikosti částic. V magnetoelek- trických barnatostrontnatých Y hexaferitech s dvojmocnými ionty zinku mělo žíhání pozitivní vliv na jejich magnetoelektrické vlastnosti, zatímco distribuce zinku nebyla výrazně ovlivněna. Ve skandiem substituovaném barnatém M fe- ritu bylo pozorováno rovnoměrné rozložení substituce v krystalu připraveném TSSG technikou. V lantnatostrontnatém M feritu byla zjištěna lokalizace elektronů v podmříži 2a, dvojná substituce La+Zn, La+Co, a La+Cu vedla k částečné kompenzaci náboje. V strontnatých...Katedra fyziky nízkých teplotDepartment of Low Temperature PhysicsFaculty of Mathematics and PhysicsMatematicko-fyzikální fakult

Preiskava vpliva hitrosti rezanja na zdržljivost vložka za rezanje pri rezanju jekla DIN 1.4301

The main aim of this paper is to assess the tool life T = f(vc) during the dry turning of 1.4301 austenitic stainless steel with a CNMG 120408 coated carbide cutting insert. Experimental tests of the selected material were realized in an Aero Turn BT-380 CNC machine tool with a Fanuc 21i TB control system. The effect of the applied cutting parameters on the surface finish, tool wear, tool life and surface roughness were investigated during the realized experiments. The aim of the present paper is to focus scientific research on the impact of the various cutting speeds during the outer longitudinal turning. The presented approach and results will be helpful for understanding the machinability of 1.4301 austenitic stainless steel during dry turning. This paper, together with the achieved results, is a basis to optimize the performance of the machining (i.e., turning) of austenitic stainless steel 1.4301 used for special industrial applications with their dominant functional areas.Glavni namen članka je oceniti preiskovano zdržljivost orodja T = f(vc) pri struženju, brez mazanja avstenitnega nerjavnega jekla 1.4301, s karbidnim rezalnim vložkom CNMG 120408 s prevleko. Preizkusi izbranega materiala so bili izvršeni na CNC stroju Aero Turn BT-380 s Fanuc 21i TB kontrolnim sistemom. Med preizkusi je bil preiskovan vpliv uporabljenih parametrov pri rezanju na kvaliteto površine, obrabo orodja, zdržljivost orodja in hrapavost. Namen članka je usmeriti raziskavo na vpliv različnih uporabljenih vrednosti hitrosti rezanja pri zunanjem vzdolžnem struženju. Vsi predstavljeni približki in rezultati bodo pomagali pri razumevanju obdelovalnosti avstenitnega nerjavnega jekla 1.4301 pri struženju brez mazanja. Dobljeni rezultati so osnova za optimiranje struženja avstenitnega nerjavnega jekla 1.4301, ki se ga, na podlagi posebnih lastnosti, uporablja pri posebnih industrijskih namenih.Web of Science50344543

Scalable dissolution-dynamic nuclear polarization with rapid transfer of a polarized solid

In dissolution-dynamic nuclear polarization, nuclear spins are hyperpolarized at cryogenic temperatures using radicals and microwave irradiation. The hyperpolarized solid is dissolved with hot solvent and the solution is transferred to a secondary magnet where strongly enhanced magnetic resonance signals are observed. Here we present a method for transferring the hyperpolarized solid. A bullet containing the frozen, hyperpolarized sample is ejected using pressurized helium gas, and shot into a receiving structure in the secondary magnet, where the bullet is retained and the polarized solid is dissolved rapidly. The transfer takes approximately 70 ms. A solenoid, wound along the entire transfer path ensures adiabatic transfer and limits radical-induced low-field relaxation. The method is fast and scalable towards small volumes suitable for high-resolution nuclear magnetic resonance spectroscopy while maintaining high concentrations of the target molecule. Polarization levels of approximately 30% have been observed for 1-13C-labelled pyruvic acid in solution

PRODUCTION OF PROTOTYPE PARTS USING DIRECT METAL LASER SINTERING TECHNOLOGY

Unconventional methods of modern materials preparation include additive technologies which involve the sintering of powders of different chemical composition, granularity, physical, chemical and other utility properties. The technology called Rapid Prototyping, which uses different technological principles of producing components, belongs to this type of material preparation. The Rapid Prototyping technology facilities use photopolymers, thermoplastics, specially treated paper or metal powders. The advantage is the direct production of metal parts from input data and the fact that there is no need for the production of special tools (moulds, press tools, etc.). Unused powder from sintering technologies is re-used for production 98% of the time, which means that the process is economical, as well as ecological.The present paper discusses the technology of Direct Metal Laser Sintering (DMLS), which falls into the group of additive technologies of Rapid Prototyping (RP). The major objective is a detailed description of DMLS, pointing out the benefits it offers and its application in practice. The practical part describes the production and provides an economic comparison of several prototype parts that were designed for testing in the automotive industry

Radical-induced hetero-nuclear mixing and low-field 13^{13}C relaxation in solid pyruvic acid

Radicals serve as a source of polarization in dynamic nuclear polarization, but may also act as polarization sink, in particular at low field. Additionally, if the couplings between the electron spins and different nuclear reservoirs are stronger than any of the reservoirs’ couplings to the lattice, radicals can mediate hetero-nuclear polarization transfer. Here, we report radical-enhanced $^{13}$C relaxation in pyruvic acid doped with trityl. Up to 40 K, we find a linear carbon $T_{1}$ field dependence between 5 mT and 2 T. We model the dependence quantitatively, and find that the presence of trityl accelerates direct hetero-nuclear polarization transfer at low fields, while at higher fields $^{13}$C relaxation is diffusion limited. Measurements of hetero-nuclear polarization transfer up to 600 mT confirm the predicted radical-mediated proton–carbon mixing

Biphasic NMR of Hyperpolarized Suspensions─Real-Time Monitoring of Solute-to-Solid Conversion to Watch Materials Grow

Nuclear magnetic resonance (NMR) spectroscopy is a key method for the determination of molecular structures. Due to its intrinsically high (i.e., atomistic) resolution and versatility, it has found numerous applications for investigating gases, liquids, and solids. However, liquid-state NMR has found little application for suspensions of solid particles as the resonances of such systems are excessively broadened, typically beyond the detection threshold. Herein, we propose a route to overcoming this critical limitation by enhancing the signals of particle suspensions by >3.000-fold using dissolution dynamic nuclear polarization (d-DNP) coupled with rapid solid precipitation. For the proof-of-concept series of experiments, we employed calcium phosphate (CaP) as a model system. By d-DNP, we boosted the signals of phosphate $^{31}$P spins before rapid CaP precipitation inside the NMR spectrometer, leading to the inclusion of the hyperpolarized phosphate into CaP-nucleated solid particles within milliseconds. With our approach, within only 1 s of acquisition time, we obtained spectra of biphasic systems, i.e., micrometer-sized dilute solid CaP particles coexisting with their solution-state precursors. Thus, this work is a step toward real-time characterization of the solid–solution equilibrium. Finally, integrating the hyperpolarized data with molecular dynamics simulations and electron microscopy enabled us to shed light on the CaP formation mechanism in atomistic detail

Activated sintering of Cr2O3-based composites by hot pressing

The paper presents and discusses questions on structure formation during the sintering process of Cr2O3-based composites using the hot pressing method, when a chemical reaction between the components takes place. The task was difficult because Cr2O3 decomposes when sintered at temperatures above 1300 degrees C. The proposed novel method allowed for interaction between aluminum and chromia, thus avoiding the decomposition of the latter. Here, ultrafine aluminum powder played the role of the active agent forming a liquid phase and reacting with Cr2O3. The appearance of the solid solutions of (Cr,Al)(2)O-3 with different stoichiometry of Cr and Al depended on the aluminum content in the initial mixture. The solid solution significantly strengthened boundaries between composite phases, resulting in the composite material of high fracture toughness between 5 and 7 MPa m(1/2) and bending strength of ca. 500 MPa. The best mechanical properties exhibited the cermet with 22 wt.% of the restored chromium.Web of Science1517art. no. 596

Radical-Induced Low-Field 1H Relaxation in Solid Pyruvic Acid Doped with Trityl-OX063

In dynamic nuclear polarization (DNP), radicals such as trityl provide a source for high nuclear spin polarization. Conversely, during the low-field transfer of hyperpolarized solids, the radicals’ dipolar or Non-Zeeman reservoir may act as a powerful nuclear polarization sink. Here, we report the low-temperature proton spin relaxation in pyruvic acid doped with trityl, for fields from 5 mT to 2 T. We estimate the heat capacity of the radical Non-Zeeman reservoir experimentally and show that a recent formalism by Wenckebach yields a parameter-free, yet quantitative model for the entire field range

The dipolar endofullerene HF@C60

The cavity inside fullerenes provides a unique environment for the study of isolated atoms and molecules. We report encapsulation of hydrogen fluoride inside C60 using molecular surgery to give the endohedral fullerene HF@C60. The key synthetic step is the closure of the open fullerene cage while minimizing escape of HF. The encapsulated HF molecule moves freely inside the cage and exhibits quantization of its translational and rotational degrees of freedom, as revealed by inelastic neutron scattering and infrared spectroscopy. The rotational and vibrational constants of the encapsulated HF molecules were found to be redshifted relative to free HF. The NMR spectra display a large 1H-19F J coupling typical of an isolated species. The dipole moment of HF@C60 was estimated from the temperature-dependence of the dielectric constant at cryogenic temperatures and showed that the cage shields around 75% of the HF dipole

Návrh nové metodiky zkoušek řezivosti a stanovení aplikačních oblastí nově vyvíjených vyměnitelných břitových destiček

Import 20/04/2006Prezenční výpůjčkaVŠB - Technická univerzita Ostrava. Fakulta strojní. Katedra (344) výrobních strojů a konstruován