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1.
Superparamagnetni nanokompoziti na osnovi nanodelcev superparamagnetnega železovega oksida in polimetil metakrilata
Sašo Gyergyek, 2010, dissertation

Abstract: V pričujočem delu sem se ukvarjal s sintezo superparamagnetnih nanokompozitov na osnovi nanodelcev γ-Fe2O3 in PMMA. Nanodelce sem sintetiziral s koprecipitacijo Fe2+/Fe3+ ionov v vodni raztopini. Nanodelce prevlečene z oleinsko ali ricinolejsko kislino sem sintetiziral s koprecipitacijo Fe2+/Fe3+ ionov v vodni raztopini v prisotnosti oleinske oz. ricinolejske kisline. Preliminarne raziskave so jasno pokazale, da je nemogoče pripraviti superparamagnetne nanokompozite γ-Fe2O3 v PMMA matrici brez ustrezne funkcionalizacije površine magnetnih nanodelcev. Iz slik s presevnega elektronskega mikroskopa (TEM) sem zaključil, da je vzorec pripravljen z mešanje nanodelcev γ-Fe2O3 s PMMA v acetonu in kasnejšim obarjanjem polimera v vodi, fazno separiran. Vzorec je sestavljen iz aglomeratov nanodelcev γ-Fe2O3, ki niso vgrajeni v polimerno matrico. Nanokompozite sem pripravil z obarjalno polimerizacijo PMMA v prisotnosti nanodelcev prevlečenih z oleinsko kislino. Koloidno stabilni suspenziji nanodelcev prevlečenih z oleinsko kislino v n-dekanu sem dodal monomer metil metakrilat. Polimerizacijo monomera sem izvedel pri povišani temperaturi. Delež nanodelcev v nanokompozitu sem kontroliral preko razmerja nanodelci/monomer. S pomočjo TEM analize sem ugotovil, da so nanodelci homogeno porazdeljeni v polimerni matrici. Z višanjem razmerja prehaja mehanizem nastanka polimernih zrn preko homogene v heterogeno nukleacijo. Nanokompozit ohrani superparamagnetno naravo tudi ob vgradnji relativno velikega deleža vgrajenih nanodelcev, do 48 ut. %. Vgradnja velikega deleža magnetnih nanodelcev je razlog za visoko nasičeno magnetizacijo nanokompozitov, do 31 emu/g. Nanokompozitne delce sem pripravil s polimerizacijo monomera metil metakrilata v prisotnosti nanodelcev v miniemulziji. Koloidno stabilno suspenzijo sestavljeno iz nanodelcev prevlečenih z ricinolejsko kislino, ultrahidrofoba in iniciatorja v monomeru, sem dodal k vodni raztopini surfaktanta. Miniemulzijo sem pripravil s pomočjo ultrazvoka. Polimerizacijo sem izvajala pri povišani temperaturi. S spreminjanjem deleža surfaktanta sem prilagajal povprečni premer nanokompozitnih delcev v razponu med ~25 nm in ~50 nm. Zaradi visokega ζ-potenciala je suspenzija nanokompozitnih delcev v vodi koloidno stabilna. S TEM slik nanokompozitnih delcev sem ugotovil, da so nanokompozitni delci sestavljeni iz nanodelcev, ki tvorijo jedro delca in tankega sloja polimera okrog jedra. V nanokompozitne delce sem uspel vgraditi do 39 ut. % magnetnih nanodelcev, ne glede na velikost nanokompozitnih delcev. Nasičena magnetizacija nanokompozitnih delcev znaša 27 emu/g.
Keywords: Superparamagnetizem, magnetni nanodelci, nanokompoziti, koloidi, polimerizacija
Published: 07.04.2010; Views: 3048; Downloads: 312
.pdf Full text (5,18 MB)

2.
LESEN RAZGLEDNI STOLP NA GOLEKU PRI ZREČAH
Darko Makovec, 2010, undergraduate thesis

Abstract: Namen diploske naloge je računska analiza in dimenzioniranje novega lesenega razglednega stolpa na Goleku pri Zrečah po predpisih Eurocode. Razgledni stolp je skupne višine 25.29m, njegova tlorisna površina je 6.30 x 6.30 m. Stolp je temeljen na štirih točkovnih temeljih. Zgrajen iz bukovega lesa kvalitete D50 in zavetrovan z jeklenimi palicami kvalitete S355/510. Razdeljen je na šest segmentov. Pokrit z štirikapno streho prekrito iz skodel. Stopnišče se nahaja znotraj stolpa in je sestavljeno iz šestih stopniščnih ram. V prvem delu diplome smo se odločili o tipu in izgledu stolpa. Določili smo njegove dimnzije in ga izrisali. V drugem delu smo se lotili računske analize z pomočjo računalniškega orodja TOWER in ga z dimenzionirali v skladu z Eurocodi 1,3,5,8.
Keywords: gradbeništvo, lesene konstrukcije, leseni stolp, razgledni stolp, evropski standardi, analiza konstrukcij, dimenzioniranje
Published: 10.06.2010; Views: 3649; Downloads: 248
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3.
KONTROLA RASTI ZELO MAJHNIH NANODELCEV STRONCIJEVEGA HEKSAFERITA MED HIDROTERMALNO SINTEZO
Leon Stare, 2013, undergraduate thesis

Abstract: Znano je, da lahko hidrotermalno sintetiziramo zelo majhne nanodelce Sr heksaferita (SrFe12O19) velikosti približno 10 nm. Sinteza takih nanodelcev je mogoča le pri temperaturah malo nad temperaturo njihovega nastanka. Če se temperatura poveča, začnejo nastajati veliki, ploščati kristali heksaferita, ki so posledica Ostwaldove pogrobitve. To onemogoča sintezo nanodelcev, ki bi imeli velikost okoli 30 nm in bi po predvidevanjih izkazovali želene magnetne lastnosti. V diplomskem delu sem se posvetil preučevanju vpliva natrijeve soli karboksimetil celuloze (NaCMC) na rast nanodelcev Sr heksaferita med hidrotermalno sintezo. Predpostavili smo, da se bo NaCMC adsorbiral na površino nastalih nanodelcev in tako uravnaval njihovo rast. Hidrotermalna sinteza poteka z obarjanjem ionov Sr in Fe iz vodnih raztopin z velikim prebitkom hidroksida NaOH in hidrotermalno obdelavo suspenzije oborjenih ionov pri temperaturah nad 100 °C. Sinteza je potekala v eni stopnji ali v dveh stopnjah. Pri sintezi v eni stopnji sem NaCMC dodal v suspenzijo oborjenih ionov, suspenzijo zaprl v avtoklav in segreval pri različnih temperaturah med 180 °C in 300 °C. Pri sintezi v dveh stopnjah pa sem v prvi stopnji sintetiziral zelo majhne nanodelce Sr heksaferita in nato njihovo suspenzijo v drugi stopnji avtoklaviral v prisotnosti NaCMC pri različnih temperaturah. Produkte smo analizirali z rentgensko difraktometrijo in s presevno elektronsko mikroskopijo. Izkazalo se je, da s sintezo v eni stopnji ne dobimo monofaznega produkta. Dodatek primerne količine NaCMC pri sintezi v dveh stopnjah zavre Ostwaldovo pogrobitev, hkrati pa ne zavre popolnoma primarne rasti. Z dodajanjem NaCMC in naknadno hidrotermalno obdelavo sem lahko povečal srednjo velikost zelo majhnih nanodelcev Sr heksaferita na približno 15 nm pri temperaturi 200 °C.
Keywords: nanodelci, hidrotermalna sinteza, heksaferiti, Ostwaldova pogrobitev
Published: 26.03.2013; Views: 1108; Downloads: 62
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4.
SINTEZA KOMPOZITNIH NANODELCEV S PREVLEČENJEM JEDRNIH NANODELCEV S PLASTMI SPINELNIH FERITOV
Blaž Belec, 2013, undergraduate thesis

Abstract: Pri diplomskem delu smo raziskovali postopek sinteze kompozitnih nanodelcev, kjer smo različne jedrne nanodelce (silicijev dioksid – SiO2 in barijev heksaferit – BaFe12O19) prevlekli s plastjo spinelnega ferita. Plast spinelnega ferita je nastala s soobarjanjem Fe3+/M2+ ionov (M2+ = Fe2+, Co2+) ter heterogeno nukleacijo trdnega produkta na površino jedrnih nanodelcev. Sintezo kompozitnih nanodelcev prekritih s plastjo kobaltovega ferita smo naredili s stehiometričnim razmerjem Fe3+/Co2+ ionov in povečano koncentracijo Co2+ ionov. Z izbrano metodo smo na površino jedrnih nanodelcev nukleirali plast spinelnega ferita (maghemit ali kobaltov ferit). Plast kobaltovega ferita ni imela stehiometrične sestave. Pri sintezi kompozitnih nanodelcev, kjer smo kot jedrne nanodelce uporabili nanodelce barijevega heksaferita velikosti 5 − 70 nm, smo dobili nehomogen vzorec. Vzorec je vseboval majhne nanodelce (13 nm), pri katerih so oborjeni ioni zreagirali z jedrnimi nanodelci ter večje kompozitne nanodelce, kjer je bila spinelna plast heterogeno nukleirana na bazalnih površinah ploščatih heksaferitnih nanodelcev. Pri pripravi kompozitnih nanodelcev, kjer smo heksaferitne nanodelce prevlekli s plastjo kobaltovega ferita, smo v primeru stehiometrične in povečane koncetacije Co2+ ionov dobili nestehiometrično sestavo spinelne pasti na površini jedrnih nanodelcev. Magnetne meritve so pokazale, da se je nasičena magnetizacija v primeru kompozitov s spinelno plastjo maghemita povečala, kakor se je povečala tudi remanenca. Pri kompozitih s plastjo kobaltovega ferita na površini se je zmanjševala tako nasičena magnetizacija kot koercitivnost.
Keywords: kompozitni nanodelci, soobarjanje, spinel, ferit
Published: 06.09.2013; Views: 1084; Downloads: 98
.pdf Full text (85,36 MB)

5.
The synthesis of iron-nickel alloy nanoparticles using a reverse micelle technique
Irena Ban, Mihael Drofenik, Darko Makovec, 2006, original scientific article

Abstract: Nanosized Fe0.2Ni0.8 particles were prepared by reducing their salts with sodium borohydride (NaBH4) in cationic water-in-oil (w/o) microemulsions of water/cetyl-trimethyl-amonium bromide (CTAB) and n-butanol/isooctane at 25 °C.According to the TEM and X-ray diffraction analyses, the synthesized particles were around 4-12 nm in size. Due to their nanodimensions, the particles had a primitive cubic (pc) structure rather than the body-centered cubic (BCC) structure of the bulk material. An examination of the synthesis from the reverse micelle reveals that the morphology of the iron-nickel alloy nanoparticles depends mainly on the microemulsion`s composition. The magnetization of the nanoparticles was much lower than that of the bulk material, reflecting the influence of the nanodimensions on the particlesć magnetizations.
Keywords: magnetic materials, nickel/iron alloys, nanoparticles, synthesis, microemulsions, magnetic properties, reverse micelles
Published: 31.05.2012; Views: 1215; Downloads: 67
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6.
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, original scientific article

Abstract: 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.
Keywords: lithium ferrites, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, magnetic properties, phase equilibrium
Published: 01.06.2012; Views: 1272; Downloads: 16
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7.
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, original scientific article

Abstract: 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.
Keywords: 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
Published: 01.06.2012; Views: 1227; Downloads: 24
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8.
A facile route to the synthesis of coated maghemite nanocomposites for hyperthermia applications
Gregor Ferk, Irena Ban, Janja Stergar, Darko Makovec, Anton Hamler, Zvonko Jagličić, Mihael Drofenik, 2012, original scientific article

Abstract: CM-dextran-covered maghemite particles for applications in magnetic hyperthermia treatments were synthesized and their physical, magnetic and morphological properties were examined. Magnetic fluids were prepared and their heating proper ies in an alternating magnetic field were studied. The results reveal that the particle size and the thickness of the carboxy-methyl-dextran (CM-dextran) coatings have a decisive influence on the heating properties: specific absorption rate (SAR). The majority of the magnetic dissipation comes from the Neel relaxation, while the Brown contribution is small. A thermal steady state at the selected temperature (42 °C) can be achieved using synthesized maghemite particles with proper particle morphology and by controlling the magnetic field intensity or the frequency.
Keywords: magnetic nanoparticles, hyperthermia, magnetic properties
Published: 10.07.2015; Views: 925; Downloads: 42
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9.
Chemical reactions between $BaTiO_3$ ceramic and fluorine-containing atmosphere
Darko Makovec, Nina Ule, Mihael Drofenik, 2002, original scientific article

Abstract: ▫$BaTiO_3$▫ ceramics were exposed to fluorine-containing atmosphere prepared by introducing a fluorination agent (▫$CF_3CH_2OH$▫) into a hot alumina-tube furnace. The fluorinated samples were studied using SEM and TEM. The fluorination resulted in the formation of a surface-reaction layer with a complex structure. At the reaction front fluorine reacts with ▫$BaTIO_3$▫ to produce ▫$BaF_2$▫ and ▫$BaTi_2O_5$▫. During the course of the fluorination the ▫$BaTi_2O_5$▫ reacts further to produce ▫$BaF_2$▫ and then subsequently Ba-polytitanates with an increasing content of titanium, and then finally ▫$TiO_2$▫. Fluorine also diffuses along the grain boundaries towards the pellet's interior. The presence of the fluorine stabilises the ▫$BaTi_2O_5$▫ compound and consequently triggers its formation in the ceramic's interior in a reaction between ▫$BaTiO_3$▫ and the intergranular phase ▫$Ba_6Ti_{17}O_{40}$▫.
Keywords: ceramics, fluorinated ceramic samples, stabilising, electronic ceramics
Published: 10.07.2015; Views: 474; Downloads: 50
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10.
Synthesis of chromium-nickel nanoparticles prepared by a microemulsion method and mechanical milling
Irena Ban, Janja Stergar, Mihael Drofenik, Gregor Ferk, Darko Makovec, 2013, original scientific article

Abstract: A chemical and a physical method have been applied for the preparation of chromium-nickel alloy nanoparticles. These particles were designed to be used for controlled magnetic hyperthermia applications. Microemulsions with $Ni^{2+}$ and $Cr^{3+}$ and/or $NaBH_4$ as precursors were prepared using the isooctane/CTAB, n-butanol/$H_2O$ system. The samples of $Cr_xNi_{1-x}$ nanoparticles with the desired composition were obtained after the reduction of their salts with $NaBH_4$ and afterwards heat treated in a TGA in a $N_2$ atmosphere at various temperatures. The $Cr_xNi_{1-x}$ materials were also prepared by mechanical milling. Utilizing a ball-to-powder mass ratio of 20 : 1 and selecting the proper alloy compositions we were able to obtain nanocrystalline $Cr_xNi_{1-x}$ particles. Thermal demagnetization in the vicinity of the Curie temperature of the nanoparticles was studied using a modified TGA-SDTA method. The alloyʼs phase composition, size and morphology were determined with XRD measurements and TEManalyses.
Keywords: mechanical alloying, magnetic nanoparticles, magnetic hyperthermia, Curie point
Published: 21.12.2015; Views: 771; Downloads: 45
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