24 results on '"in situ sinteza"'
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2. In situ sinteza nanodelcev ZnO s pomočjo fitokemikalij in plinske plazme za doseganje večfunkcionalnih lastnosti tekstilij
- Author
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Verbič, Anja and Gorjanc, Marija
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in situ synthesis ,cinkov oksid ,večfunkcionalnost ,green synthesis ,plazma ,zinc oxide ,bombaž ,cotton ,in situ sinteza ,zelena sinteza ,ZnO ,poliester ,polyester ,multifunctional ,plasma - Abstract
V doktorski disertaciji je predstavljena raziskava razvoja novega okolju prijaznega postopka in situ sinteze delcev cinkovega oksida (ZnO) na bombažu (CO) in poliestru (PET), kjer so bili namesto kemičnih reducentov uporabljeni vodni ekstrakti odpadnega rastlinskega materiala (invazivne tujerodne rastline in živilski odpadki) in namesto kemične alkalije uporabljen vodni ekstrakt lesnega pepela. Receptura in situ sinteze ZnO je bila optimizirana s proučevanjem različnih metod sinteze in vplivov parametrov sinteze (vrsta in koncentracija prekurzorja in »zelenih« reducentov, vrsta reducenta, vrstni red reagentov pri sintezi, čas in temperatura sinteze). Zaradi različne vsebnosti fenolnih skupin (TPC) »zelenih« reducentov, ki vplivajo na stopnjo antioksidativnosti in redukcijske sposobnosti reducenta, se je kot ključni parameter za uspešno oblikovanje ZnO direktno na CO in enakomerno porazdelitev po vlaknih ter odlično sposobnost tkanine blokiranja ultravijoličnega (UV) sevanja (50+), izkazal vrstni red reagentov (Alkalija–Zn-prekurzor–Reducent). Cinkov acetat je bolj primeren prekurzor za sintezo na CO kot cinkov nitrat, saj se s slednjim mehanske lastnosti tkanine močno poslabšajo. Ugotovljeno je bilo, da se lahko glede na uporabljen »zeleni« reducent prilagodi tudi omočljivost CO, in sicer reducenti z višjo vsebnostjo TPC omogočajo hidrofilne lastnosti, tisti z nižjo vsebnostjo TPC pa hidrofobne. Pri sinteznem postopku na PET je bila vpeljana plazma kisika za povečanje reaktivnost tkanine do reakcijskih raztopin in kasneje kot zamenjava alkalije. S plazmo se je povečala hidrofilnost PET in enakomerna adsorpcija reagentov, kar je omogočilo homogenost in situ sintetiziranih ZnO po celotni tkanini oz. vlaknih. Pri tem se je s številom plazemskih obdelav višala tudi UV zaščita tkanine, kot posledica zvišanja vsebnosti ZnO. Tako alkalija kot plazma kisika vplivata na povečanje aktivnih mest na PET, ki predstavljajo nukleacijska mesta prekurzorja za oblikovanje ZnO s pomočjo »zelenega« reducenta. S stališča čim bolj okolju prijazne in situ sinteze ZnO, zmanjšanja porabe vode, časa priprave reagentov in homogenosti in situ sintetiziranih ZnO na tkanini, se namesto alkalije lahko uporabi plazma kisika. This doctoral dissertation presents the development of a novel, environmentally friendly process for in situ synthesis of zinc oxide (ZnO) on cotton (CO) and polyester (PET) using aqueous extracts of invasive alien plants and food waste instead of classical chemical reducing agents, and aqueous extract of wood ash instead of chemical alkali. The ZnO synthesis procedure was optimised by studying different synthesis methods and parameters (type and concentration of precursor and »green« reducing agent, the order of synthesis solutions, synthesis time and temperature). Due to the different amounts of phenolic compounds (TPC) present in the »green« reducing agents, the order of the synthesis solutions (Alkali䀒Precursor-Reducing agent) proved to be a key parameter influencing the successful in situ synthesis and the uniform distribution of ZnO particles on fibres and consequently achieving the excellent ultraviolet (UV) protective properties (50+) of the CO fabric. Zinc acetate is a more suitable precursor for the in situ synthesis of ZnO than zinc nitrate, since with the latter, mechanical properties of the fabric are greatly impaired. Depending on the »green« reducing agent used, the wettability of the CO fabric can be adjusted. The reducing agents with higher TPC values enable hydrophilic properties, while the ones with lower TPC values enable hydrophobic properties of the CO. Oxygen plasma treatment was incorporated into the synthesis process on PET, first to increase the reactivity of PET to the synthesis solutions, and finally as a substitute for alkali. Plasma increased the hydrophilicity of PET and enabled an even adsorption of the reagents, resulting in uniform distribution of the in situ synthesised ZnO on the fabric. As the number of plasma treatments increased, the UV protection of fabrics also increased, due to higher ZnO content. Both alkali and oxygen plasma increase the amount of active binding sites on PET, which represent precursor nucleation sites for the formation of ZnO using »green« reducing agent. From the point of view of the most environmentally friendly in situ synthesis of ZnO, reduction of water consumption, preparation time for reagents and homogeneity of in situ synthesized ZnO on the fabric, oxygen plasma can be used instead of alkali.
- Published
- 2023
3. In situ sinteza i karakterizacija tankih biokompatibilnih kompozitnih prevlaka hidroksiapatit/pasivni oksid za potencijalnu upotrebu u medicini
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Pantović Pavlović, Marijana, Ignjatović, Nenad, Eraković Pantović, Sanja, Panić, Vladimir V., Pantić, Igor, and Bugarski, Branko
- Abstract
Definisanje nove metode anodizacije/anaforetske depozicije za nanošenje kalcijum fosfatnih i hibridnih prevlaka na bazi kalcijum fosfatnih keramika na titanijumske spustrate sa unapredjenim svojstvima je bio predmet doktorske disertacije koja je pred Vama. Ova doktorska disertacija daje doprinos rešavanju problema višestepenog pred-tretmana i post-tretmana površine radi dobijanja prevlake na supstratu, adhezije prevlake, antimikrobnih i citotoksičnih svojstava koja se javlјaju kod biomaterijala. Primarno se bavi kreiranjem i optimizacijom novog in situ procesa anodizacije/anaforetske depozicije za dobijanje multifunkcionalnih kompozitnih biomaterijala. In situ metoda rezultira u poboljšanoj adheziji bioaktivne prevlake, povećanoj bioaktivnosti i biokompatibilnosti sa povećanim antimikrobnim svojstvima i odsustvom citotoksičnosti. Izučavani biomaterijali ostvaruju pobolјšana svojstva kao što su: otpornost na koroziju, odsustvo toksičnosti za lјudsko telo i odgovarajuća čvrstoća što omogućava njihovo potencijalno korišćenje u medicini i stomatologiji. Cilј ove doktorske disertacije je bio kreiranje novog in situ procesa anodizacije/anaforetske depozicije i adekvatna modifikacija parametara procesa za nanošenje kompozitnih kalcijum fosfatnih prevlaka na titan i njegove legure, pri čemu se inovativnost ogleda u objedinjavanju procesa sinteze kalcijum fosfatne prevlake i modifikacije površine supstrata delimičnom inkorporacijom keramičke prevlake u kristalnu strukturu supstrata. Karakterizacija ovako dobijenih prevlaka je obavljena različitim fizičko-hemijskim, biohemijskim i biološkim metodama. Ispitivanja su obuhvatila morfološku karakterizaciju i morfološke promene kalcijum fosfatnih prevlaka elektronskim mikroskopijama, pri čemu su korišćene sledeće tehnike karakterizacije: mikroskopija atomskih sila – AFM, skenirajuća elektronska mikroskopija – SEM i visoko-rezoluciona skenirajuća elektronska mikroskopija FE-SEM. Hrapavost podloge se određivala metodama AFM i ručnim meračem linearne hrapavosti (Handheld Roughness Tester). Metodom merenja difrakcije X-zraka (XRD) utvrđeni su kristalografski i fazni sastavi, kao i strukturne promene kompozita. Ova metoda je korišćena i pri dokazivanju bioaktivnosti prevlaka na bazi amorfnog kalcijum fosfata bez i sa hitozan oligosaharid laktatom (ChOL). Atenuiranom totalno refleksujućom infracrvenom spektroskopijom sa Furijeovom trasformacijom (ATR-FTIR) je dokazana uspešnost novog in situ procesa, prvenstveno kada je u pitanju dobijanje hibridnih multifunkcionalnih kompozitnih prevlaka sa ChOL... Completely new method of anodization/anaphoretic deposition for the deposition of calcium phosphate and hybrid coatings based on calcium phosphate ceramics on titanium supstrate with improved properties was the objective of the doctoral dissertation in front of you. The dissertation contributes to solving the problem of multistage pretreatment and posttreatment of the surface in order to obtain a coating on the substrate, adhesion of the coating, antimicrobial and cytotoxic properties that occur in biomaterials. It primarily deals with the application and optimization of the new in situ anodizing/anaphoretic deposition process for obtaining multifunctional composite biomaterials. The in situ method leads to improved bioactive coating adhesion, increased bioactivity and biocompatibility of biomaterials with increased antimicrobial properties and absence of cytotoxicity. Studied biomaterials have improved characteristics such as: corrosion resistance, absence of toxicity for the human body and adequate strength, which enables their possible use in biomedicine. The objective of this doctoral dissertation was to define a completely new in situ anodizing/anaphoretic deposition process and adequate modification of process parameters for the application of composite calcium phosphate coatings on titanium and its alloys, wherein innovation is reflected in combining calcium phosphate coating synthesis and surface modification by partially incorporating a ceramic coating into the crystalline structure of the substrate. The characterization of the coatings obtained in this manner was performed by various physico-chemical, biochemical and biological methods. The experiments of morphological characterization and morphological changes of calcium phosphate coatings included following electronic microscopy characterization techniques: atomic forces microscopy - AFM, scanning electron microscopy - SEM and field emission scanning electron microscopy FE-SEM. The substrate roughness was determined by AFM and Handheld Roughness Tester methods. The X-ray diffraction (XRD) method was used for determination of crystallographic and phase compositions as well as composites structural changes. This method was also used to demonstrate the bioactivity of amorphous calcium phosphate coatings with and without chitosan oligosaccharide lactate (ChOL). Attenuated totally reflective Fourier transform infrared spectroscopy with (ATR-FTIR) was used to prove the successfull execution of the new in situ process, primarily when it comes to obtaining hybrid multifunctional composite coatings with ChOL...
- Published
- 2022
4. Zelena in situ sinteza nanodelcev srebra na bombažni tkanini
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Čuk, Nina and Gorjanc, Marija
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in situ sinteza ,in situ synthesis ,silver nanoparticles ,invasive alien species ,invazivne tujerodne rastline ,srebrovi nanodelci ,rastlinske komponente živilskega odpadka ,food waste plant materials - Abstract
V diplomskem delu je bila proučena in situ sinteza nanodelcev srebra na surovi bombažni tkanini. Kot prekurzor je bil uporabljen srebrov nitrat, kot reducenti pa vodni ekstrakti rastlinskih komponent živilskega odpadka (listi zelenega čaja, koščice avokada in olupki granatnega jabolka) in invazivnih tujerodnih rastlinskih vrst (korenika japonskega dresnika, plodovi octovca in cvetovi zlate rozge). Za primerjavo je bila bombažna tkanina obdelana tudi samo v reducentih. Barvne vrednosti (vrednosti CIE L*a*b*) vzorcev in globina obarvanja (vrednosti K/S) so bile določene z refleksijskim spektrofotometrom. Zaščitne lastnosti obdelanih vzorcev proti ultravijoličnem sevanju (vrednosti UZF) so bile določene z uporabo UV-Vis spektrofotometra. Morfologija vlaken oziroma oblikovanih nanodelcev je bila opazovana z vrstično elektronsko mikroskopijo (SEM). Vsebnost srebra na vzorcih je bila določena z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS). Vzorcem, kjer je bila in situ sinteza izvedena, so bile proučene tudi njihove protimikrobne lastnosti. Vodni rastlinski ekstrakti so reducirali srebrov nitrat v krogelno oblikovane nanodelce z različno velikostjo in vsebnostjo glede na posamezen reducent. Le-to je vplivalo na uspešnost redukcije rasti bakterij Escherichia coli in Staphylococcus aureus, ki je bila pri vseh tako obdelanih vzorcih odlična. Odlična zaščita proti UV-sevanju je bila izmerjena tako za vzorce z vsebnostjo srebra kot tudi za večino tistih brez prisotnosti srebra. Po večkratnih pranjih vzorci s formiranimi srebrovimi nanodelci še vedno nudijo odlično zaščito proti UV-sevanju, ostali obdelani vzorci pa so uvrščeni v prav dobro ali dobro zaščitno kategorijo. Prisotnost srebrovih nanodelcev vpliva tudi na temnejše barve, ki se odražajo v bolj rdečkastih in rumenkastih barvnih odtenkih. Po pranju večina vzorcev postane svetlejših in modrikastih. In situ synthesis of silver nanoparticles on raw cotton fabric was studied for Diploma thesis. Synthesis occurred directly on cotton when it was immersed in precursor solution of silver nitrate and after in water-extracts of food waste plant materials (green tea leaves, avocado seed and pomegranate peel) and invasive alien species (Japanese knotweed rhizome, Staghorn sumac fruit and Goldenrod flowers). For comparison, the cotton fabrics were treated also only with water-extracts. Colour values (CIE L*a*b) and colour depth (K/S values) were determined using a reflectance spectrophotometer. Ultraviolet protective properties of the samples (UPF values) were analysed using UV/VIS spectrophotometer. The morphology of fibres and formed nanoparticles was analysed using scanning electron microscopy (SEM). Silver content was determined using inductively coupled plasma mass spectrometry (ICP-MS). Antibacterial properties of the samples, where in situ synthesis was performed, were also analysed. Different size and content of spherical shaped nanoparticles were formed on fibres using water-extracts as reducing agents. Size and shape of silver nanoparticles influence the reduction of Escherichia coli in Staphylococcus aureus bacteria. The antimicrobial properties were excellent for the samples with synthesized nanoparticles. Furthermore, excellent protection against ultraviolet radiation was determined for the samples without and with formed nanoparticles. After twelve times washing cycles, the samples with silver nanoparticles still show excellent protection against ultraviolet radiation, all other sample were classified with very good or good protection category. The presence of nanoparticles on cotton also influences its colour, which is darker, with reddish and yellowish hue. Most of the samples become lighter and bluish after repetitive washings.
- Published
- 2019
5. In situ synthesis of Cu/Cu2O nanoparticles on the TEMPO oxidized cotton fabric
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Marković, Darka, Korica, Matea, Kostić, Mirjana, Radovanović, Željko, Šaponjić, Zoran, Mitrić, Miodrag, Radetić, Maja, Marković, Darka, Korica, Matea, Kostić, Mirjana, Radovanović, Željko, Šaponjić, Zoran, Mitrić, Miodrag, and Radetić, Maja
- Abstract
Recent breakthrough in nanotechnologies had large impact on research in the field of medical textiles. So far many efforts have been made to fabricate antimicrobial textile materials with incorporated metal (Ag, Cu) and metal oxide (TiO2, ZnO, CuO, Cu2O) nanoparticles (NPs) and to learn more about the mechanism of their action1-3. The possible application of Cu, CuO and Cu2O NPs for antibacterial protection of cotton fabrics became the focus of many research groups since the copper in different forms (ionic, copper oxides, copper complexes) is very active against various bacterial strains and precursor salts of copper are much cheaper than those of silver. Unlike in the case of Ag NPs where the dip-coating from Ag NPs suspensions/colloids was mostly applied for nano-finishing of cotton fabrics, in situ synthesis of Cu, CuO and Cu2O NPs seems to be the method of choice in published studies until now4,5. Namely, the dominant approach relies on the introduction of carboxyl groups to cotton fibers by coating them with appropriate polymer or chemical modification of cellulose, adsorption of Cu2+-ions and their reduction. In our study we applied the TEMPO/NaClO/NaClO2 system under neutral conditions for selective oxidation of cellulose in order to enhance its ability to bind Cu2+-ions. We focused our study on much shorter oxidation times since the aim was to preserve the structure of cellulose fibers i.e. their mechanical strength. Therefore, the main goal of our study was to discuss the influence of the functional groups generated by TEMPO-mediated oxidation of cotton fabric at different reaction times on the amount, activity and stability of in situ synthetized Cu/Cu2O NPs using sodium borohydride as a reducing agent at room temperature., In situ sinteza nanočestica Cu/Cu2O na pamučnoj tkanini diskutovana u ovom radu bazirana je na adsorpciji Cu2+-jona na karboksilnim grupama formiranim TEMPO oksidacijom celuloze i njihovoj redukciji natrijum-borhidridom. Hemijske promene nastale TEMPO oksidacijom su praćene titrimetrijski određivanjem sadržaja karboksilnih grupa u pamuku. Prisustvo nanočestica Cu/Cu2O na pamučnoj tkanini potvrđeno je SEM i AAS analizama. Promene obojenja tkanina su određene refleksionom spektrofotometrijom. Antibakterijska aktivnost generisanih nanočestica Cu/Cu2O je testirana prema Gram-negativnoj bakteriji E. coli i Gram-pozitivnoj bakteriji S. aureus. Produžavanje vremena TEMPO oksidacije za rezultat je imalo povećanje sadržaja karboksilnih grupa na pamučnoj tkanini. Stoga su veće količine Cu2+-jona mogle da se adsorbuju na supstratu. Ovo je dalje za posledicu imalo stvaranje većih količina nanočestica Cu/Cu2O. Svi ispitivani tekstilni nankompoziti su obezbedili maksimum redukcije bakterija E. coli i S. aureus. Takođe je utvrđeno da pamučne tkanine sa inkorporiranim nanočesticama Cu/Cu2O pružaju kontrolisano otpuštanje Cu2+ -jona u fiziološkom rastvoru što je imperativ za prevenciju infekcija.
- Published
- 2017
6. In-situ sinteza nanodelcev ZnO na bombažni tkanini z reducentom ekstrahiranim iz avokadove koščice
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Marčič, Tina and Gorjanc, Marija
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cinkov oksid ,zelena sinteza ,green synthesis ,avokadova koščica ,avocado pit ,nanodelci [Ključne besede] ,zinc oxide ,extract ,nanoparticles [Keywords] ,ekstrakt - Abstract
Namen diplomskega dela je bil ugotoviti, ali se lahko ekstrakt avokadove koščice uporabi kot naravni reducent za in-situ sintezo nanodelcev cinkovega oksida (ZnO) na bombažni tkanini za dosego dobre zaščite pred ultravijoličnim (UV) sevanjem. Zato je bil preučevan vpliv koncentracije prekurzorja (cinkov klorid (ZnCl2)), vrstni red obdelave bombažne tkanine s prekurzorjem in reducentom ter temperature sinteze. Na UV/VIS spektrofotometru je bil vzorcem določen UV zaščitni faktor (UZF), na refleksijskem spektrofotometru pa barva vzorcev v barvnem prostoru CIELAB. Morfologija vlaken oziroma sintetiziranih nanodelcev na vlaknih je bila proučevana z vrstično elektronsko mikroskopijo (SEM). Vzorcem je bila izmerjena barva in določen UZF tudi po petkratnem gospodinjskem pranju. Rezultati raziskave so pokazali, da je temperatura in-situ sinteze pomembna, in sicer so imeli vzorci višje UZF vrednosti, če so bili obdelani pri sobni temperaturi kot pri 60 °C. Na oblikovanje nanodelcev in UZF vrednosti vplivata tudi vrstni red obdelave tkanine s prekurzorjem in reducentom ter molarna koncentracija prekurzorja. Višje vrednosti UZF so imeli vzorci, kjer je bila uporabljena 1 M raztopina ZnCl2, kot pa 0,5 M. V primeru, kjer je in-situ sinteza potekala tako, da je bil vzorec najprej obdelan v prekurzorju in nato v reducentu, je vzorec izkazal najvišjo zaščito pred UV sevanjem (dobra UV zaščita). Vzorec ni bil med najtemnejšimi, torej barva ni bila tista, ki je vplivala na UZF, ampak številni nanodelci Zn, ki so se oblikovali na površini bombažnih vlaken, kar je bilo razvidno tudi iz SEM analize. Vrstni red obdelave tkanine, kjer se je tkanino najprej obdelalo v reducentu in nato v prekurzorju, je dal najslabše rezultate UZF. Iz SEM analize je razvidno, da so se na vlaknih oblikovali nanodelci ZnO, vendar očitno ne v zadostni količini, da bi tako obdelana tkanina zagotovila zaščito pred UV sevanjem. Po pranju se nekaterim vzorcem zviša UZF, kar je presenetljivo. Predvideva se, da so nanodelci pri pranju migrirali iz notranjosti vlaken na njihovo površino in s tem zvišal UZF. The purpose of the bachelor’s thesis was to determine whether the avocado pit extract can be used as a natural reducing agent for in-situ synthesis of zinc oxide nanoparticles (ZnO) on cotton fabric and whether good protection against ultraviolet (UV) radium can be achieved. For this purpose, the molar concentration of the precursor (zinc chloride (ZnCl2)), the order of treatment of the cotton fabric with the precursor and reducing agent, and the temperature of the synthesis were studied. On the UV/VIS spectrophotometer, the sample was determined by the UV protection factor (UZF) and the color of the samples (CIELAB) on the reflection spectrophotometer. The morphology of fibers or synthesized nanoparticles on fibers was studied by linear electron microscopy (SEM). The samples were measured in color and were determined by UZF after a five-time household wash. The results of the study showed that the in-situ synthesis temperature was important and samples had higher (UZF) values if they were treated at the room temperature than at 60 °C. The order of processing of the fabric with the precursor and reducing agent and the molar concentration of the precursor were also influenced by the formation of nanoparticles and UZF values. Higher values of UZF had samples where 1 M ZnCl2 solution was used than 0.5 M. In the case where the in-situ synthesis was carried out in such a way that the sample was first treated in the precursor and then in the reducing agent, the sample showed the highest protection against UV radiation (good UV protection). The sample was not among the darkest, so the color was not the one that affected the UZF but the numerous nanoparticles of Zn formed on the surface of the cotton fibers, which was also evident from the SEM analysis. The order of processing of the fabric where the fabric was, first, treated in the reducing agent and then in the precursor gave the worst results of the UZF. From the SEM analysis, it can be seen that ZnO nanoparticles were formed on the fibers, but apparently not in sufficient quantity for the treated fabric to provide protection against UV radiation. After washing, some patterns increase UZF, which is surprising. It is anticipated that the nanoparticles migrated to the surface of the fibers by washing and, therefore, increased the UZF.
- Published
- 2019
7. In situ sinteza metalnim ionima dopiranog hidroksiapatita u polimernoj matrici kitozana
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Paun, Helena and Ivanković, Hrvoje
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kitozan ,zinc ,in situ ,hydroxyapatite ,TECHNICAL SCIENCES. Chemical Engineering. Chemical Engineering in Material Development ,hidroksiapatit, cink, kitozan, in situ ,chitosan ,TEHNIČKE ZNANOSTI. Kemijsko inženjerstvo. Kemijsko inženjerstvo u razvoju materijala ,hidroksiapatit ,cink - Abstract
Inženjerstvo koštanog tkiva je interdisciplinarno područje usmjereno na razvoj biomaterijala za izradu trodimenzijskih okosnica koje oponašaju prirodno koštano tkivo. Okosnica se ugradnjom na oštećeno područje kosti sjedinjuje s okolnim tkivom, potiče njegovu regeneraciju, te se istovremeno razgrađuje i osigurava mjesto za rast novog koštanog tkiva. Okosnice koje oponašaju prirodno koštano tkivo izrađene su iz organsko-anorganskih kompozitnih materijala po uzoru na prirodno koštano tkivo koje se sastoji od istih. Organsku fazu čini izvanstanična matrica većinski građena od kolagena, koju zbog strukturalne sličnosti najčešće oponašaju prirodni polimeri. Hidroksiapatit je glavna anorganska komponenta koštanog tkiva, zbog čega se koristi kao anorganska faza u izradi okosnica. Biološki hidroksiapatit u svojoj strukturi sadrži elemente u tragovima koji su neophodni za metabolizam kosti i organizam. Mnoga istraživanja usmjerena su na dopiranje hidroksiapatita cinkovim ionom koji ima antibakterijska svojstava te pozitivno utječe na aktivnost osteoblasta i regeneraciju tkiva. U ovom radu su pripremljeni uzorci cinkovim ionom dopiranog hidroksiapatita (0, 1, 5 i 10 mol% cinka) metodom precipitacije. Sinteza je provedena korištenjem prekursora kalcijevih iona iz biogenog i sintetskog izvora. Sastav uzoraka, prije i nakon toplinske obrade, utvrđen je rendgenskom difrakcijskom analizom i infracrvenom spektroskopijom s Fourierovim transformacijama. Sintezom iz biogenog izvora nastaje dvofazni sustav hidroksiapatita i oktakalcij fosfata, dok iz sintetskog izvora jednofazni sustav hidroksiapatita. Nakon toplinske obrade uzoraka nastaje dvofazni sustav α i ß-trikalcijev fosfata. Ugradnja cinkova iona u strukturu oktakalcij fosfata pentahidrata i ß-trikalcijev fosfata praćena je promjenama parametara elementarne rešetke. Zbog neznatnih promjena parametara elementarne rešetke hidroksiapatita, pretpostavlja se da je došlo do adsorpcije cinkova iona na površinu kristala. Dodatno, provedena je in situ sinteza cinkom dopiranog hidroksiapatita (sintetski prekursor kalcijevih iona) u polimernoj matrici kitozana. Karakterizacija dobivenih poroznih struktura provedena je infracrvenom spektroskopijom s Fourierovim transformacijama i pretražnim elektronskim mikroskopom. Bone tissue engineering is an interdisciplinary field focused on the development of biomaterials as three-dimensional scaffolds which mimic natural bone tissue. After implantation at injured site it integrates with the surrounding tissue, promotes bone regeneration, degrades and provides space for new bone tissue. The imitation of natural bone tissue is obtained by using biomaterials based on organic/inorganic materials. The organic phase is an extracellular matrix mostly composed of collagen. Due to its similarity to the extracellular matrix structure, the organic phase is often imitated by natural polymers. Hydroxyapatite is the major inorganic component of bone tissue and is often used in biomedical areas. Biological apatite contains trace elements in its structure which are essential for bone and body metabolism. Many studies have been focused on doping hydroxypatite structure with zinc ion, which is interesting because of antibacterial properties and positive effect on osteoblastic and tissue regeneration activity. In this study zinc doped hydroxyapatite (0, 1, 5 and 10 mol% zinc) was prepared by using precursors of calcium ions from biogenic and synthetic source. The composition of the samples was determined by X-ray diffraction analysis and infrared spectroscopy with Fourier transforms. From biogenic source was obtained two-phase system of hydroxyapatite and octacalcium phosphate pentahydrate, while from synthetic source one-phase system of hydrpxyapatite. After heat treatment it was obtained two-phase system of α and β-tricalcium phosphate. Decrease of cell parameters of octacalcium phosphate pentahydrate and β-tricalcium phosphate confirmed doped structures with zinc ions. However, it can be assumed that hydroxyapatite is not zinc doped and that zinc ions are adsorbed on crystal surface as cell parameter did not decrease. Additionally, in situ synthesis of zinc doped hydroxyapatite (from synthetic source) within chitosan matrix was obtained. Characterization of porous structures was determined by infrared spectroscopy with Fourier transforms and scanning electron microscopy.
- Published
- 2018
8. In-situ synthesis of titanium carbide particles in an iron matrix during diode-laser surface alloying of ductile cast iron: In situ sinteza delcev titanovega karbida v osnovi železa med površinskim legiranjem litega železa z diodnim laserjem
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Janicki, Damian
- Published
- 2017
9. In situ sinteza hidroksiapatita u matrici biorazgradivih polimera
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Rogina, Anamarija
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Kitozan ,Hidroksiapatit ,Visokoporozna struktura (nosač) ,Bubrenje ,MC3T3-E1 preosteoblasti ,diferencijacija - Abstract
Oštećenja koštanog tkiva i zatajenje organa uzrokovanih defektima, prijelomima i drugim ozljedama predstavljaju jedan od većih problema očuvanja ljudskog zdravlja. Manjak dostupnih donorskih organa te imunološko odbacivanje stranog tkiva otežavaju presađivanje. Različite kirurške metode primjenjuju umjetne materijale poput proteza, umjetnih srčanih zalistaka i drugih organa. Biološka inertnost postojećih komercijalnih usadaka onemogućuje prožimanje i srastanje okolnog tkiva s njima na mjestu ugradnje. Stoga je razvoj liječenja tkivnih oštećenja usmjeren prema regenerativnoj medicini. Regenerativne metode u liječenju koštanih defekata temelje se na primjeni matičnih stanica uzgojenih na biorazgradivom poroznom materijalu koji oponaša izvanstaničnu matricu prirodne kosti s obzirom na površinska, kemijska, biološka i mehanička svojstva. Za oponašanje prirodnog koštanog tkiva potreban je razvoj nanostrukturiranog kompozitnog materijala visoke poroznosti koji se, kroz određeno vrijeme u živom organizmu u potpunosti razgrađuje. Primjena biorazgradivih polimera i hidroksiapatitne keramike ima veliki potencijal u obnovi oštećenog tkiva. Sinergija svojstava polimerne faze (biorazgradivost, biokompatibilnost, mehanička izdržljivost) i hidroksiapatitne keramike (bioaktivnost, bioresorpcija) omogućuje stvaranje kompozitnih biomaterijala kao autogenih ili alogenih nadomjestaka. U ovom doktorskom radu pripravljeni su kompozitni materijali na temelju kitozana i in situ hidroksiapatita (HA) reakcijama kemijske koprecipitacije. Ovisnost sastava in situ stvorene anorganske faze o reakcijskim parametrima (temperatura, vrijeme sinteze, pH, dodatak aditiva) ispitana je rendgenskom difrakcijskom analizom i infracrvenom spektroskopijom s Fourierovim transformacijama. Morfologija i veličina kristala hidroksiapatitne faze istražena transmisijskim elektronskim mikroskopom ukazuju na stvaranje igličastih kristala nanometarskih veličina. Visokoporozne strukture (nosači) s različitim udjelom in situ HA pripravljene su metodom toplinski inducirane fazne separacije uz naknadno geliranje i ekstrakciju (engl. freeze-gelation/freeze-extraction). Pretražnom elektronskom mikroskopijom istražen je utjecaj količine HA na mikrostrukturu nosača. Mjerenja živinim porozimetrom potvrđuju visoku poroznost pripravljenih nosača s vrijednostima otvorene poroznosti iznad 84 %. Vrijednosti kapaciteta bubrenja i tlačne čvrstoće nosača izmjerenih u Dulbeccovom fosfatnom puferu smanjuju se s povećanjem udjela in situ HA. Analiza citotoksičnosti s L929 stanicama fibroblasta potvrđuje necitotoksičnost ispitanih kompozitnih nosača. In vitro nasađivanje MC3T3-E1 preosteoblasta ukazalo je na dobru životnu aktivnost stanica do 14 dana uzgajanja. Diferencijacija MC3T3-E1 preosteoblasta potvrđena imunološkim ispitivanjima osteoblastnih markera (osteopontina i vezujućeg sijaloproteina) ukazuje na osteogeni potencijal kompozitnih nosača.
- Published
- 2015
10. Designing UV-protective and hydrophilic or hydrophobic cotton fabrics through in-situ ZnO synthesis using biodegradable waste extracts
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Anja Verbič, Katja Brenčič, Matej Dolenec, Gregor Primc, Nina Recek, Martin Šala, and Marija Gorjanc
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multifunctional textile ,cinkov oksid ,večfunkcionalne tekstilije ,General Physics and Astronomy ,zinc oxide ,in-situ sinteza ,bombaž ,Surfaces and Interfaces ,General Chemistry ,in-situ synthesis ,Condensed Matter Physics ,cotton ,Surfaces, Coatings and Films ,tujerodne invazivne rastline ,udc:677 ,food waste ,živilski odpadki ,invasive alien plants - Abstract
An extensive study on using plant waste aqueous extracts as natural chemicals for in-situ synthesis of zinc oxide (ZnO) on cotton is presented. Reducing agents were prepared from green tea leaves (GT), pomegranate peels (PG), and staghorn sumac leaves (SsL) and drupes (SsD), and the alkaline medium from discarded wood ash. Zinc acetate was found to be more appropriate precursor than zinc nitrate. Formation of ZnO on cotton was confirmed by energy dispersive spectroscopy, X-ray photoelectron spectroscopy and X-ray diffraction analysis (XRD). The inductively coupled plasma mass spectrometry and X-ray fluorescence results showed the highest amount of ZnO on cotton was formed using PG and SsL extracts, which was also confirmed with scanning electron microscopy and UV/visible spectroscopy. The ZnO-functionalised samples exhibited excellent UV-blocking ability and different wetting properties (hydrophilic or hydrophobic) depending on the reducing agent used due to their different total phenolic content. This study shows that by choosing the plant waste source as a reducing agent for ZnO formation directly on cotton, the properties of cotton can be designed to be hydrophilic or hydrophobic with excellent UV-blocking properties. The XRD results of ex-situ synthesis prove that the short reaction time enables the formation of ZnO.
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- 2022
11. Multifunctional antibacterial and ultraviolet protective cotton cellulose developed by in situ biosynthesis of silver nanoparticles into a polysiloxane matrix mediated by sumac leaf extract
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Brigita Tomšič, Ada Ferri, Elisa Savio, Barbara Simončič, Matic Šobak, Ida Poljanšek, Ivan Jerman, and Danaja Štular
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General Physics and Astronomy ,bombaž ,02 engineering and technology ,zelena in situ sinteza ,engineering.material ,cotton cellulose ,010402 general chemistry ,medicine.disease_cause ,01 natural sciences ,Ag nanodelci ,Silver nanoparticle ,Matrix (chemical analysis) ,udc:677 ,octovec ,ekstrakt listov ,chemistry.chemical_compound ,Coating ,Biosynthesis ,medicine ,celuloza ,UV protection ,protimikrobna aktivnost ,Cellulose ,Ag NPs ,antimicrobial activity ,Chemistry ,technology, industry, and agriculture ,Surfaces and Interfaces ,General Chemistry ,021001 nanoscience & nanotechnology ,Condensed Matter Physics ,Antimicrobial ,0104 chemical sciences ,Surfaces, Coatings and Films ,engineering ,UV-zaščita ,green in situ synthesis ,0210 nano-technology ,Antibacterial activity ,sumac leaf extract ,Ultraviolet ,Nuclear chemistry - Abstract
A novel facile and eco-friendly procedure for fabrication of multifunctional antibacterial and ultraviolet (UV) protective cotton surface was presented, including premodification of cellulose fibres with a polysiloxane matrix, followed by green in situ biosynthesis of silver nanoparticles (Ag NPs) in the presence of sumac leaf extract as a reducing and stabilising agent. During the biosynthesis, face-centred cubic Ag NPs with an average size of 52–105 nm were generated on the cotton fibres. Increasing the concentration of the AgNO3 precursor resulted in increased concentration of Ag NPs of 50–11,000 mg/kg. The chemically modified cotton surface exhibited excellent antimicrobial and UV protection properties. The additive antibacterial activity of Ag NPs and sumac leaf extract showed biocidal activity against S. aureus even at the lowest Ag NP concentration of 50 mg/kg, and in the case of E. coli, biocidal activity was achieved at a concentration of 340 mg/kg. The presence of both Ag NPs and sumac leaf extract provided UV protection factor greater than 40, irrespective of Ag NP concentration. The increase in Ag NP concentration significantly improved the durability of the coating.
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- 2022
12. Novel Green In Situ Synthesis of ZnO Nanoparticles on Cotton Using Pomegranate Peel Extract
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Ivan Jerman, Anja Verbič, Martin Šala, and Marija Gorjanc
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Technology ,in situ synthesis ,cinkov oksid ,Materials science ,Scanning electron microscope ,Sonication ,zinc oxide nanoparticles ,Nanoparticle ,chemistry.chemical_element ,bombaž ,Zinc ,medicine.disease_cause ,cotton ,Article ,udc:677 ,in situ sinteza ,pomegranate ,granatno jabolko ,medicine ,General Materials Science ,phytosynthesis ,Fourier transform infrared spectroscopy ,Wurtzite crystal structure ,Microscopy ,QC120-168.85 ,nanodelci ,QH201-278.5 ,Engineering (General). Civil engineering (General) ,TK1-9971 ,Descriptive and experimental mechanics ,food waste ,chemistry ,Chemical engineering ,živilski odpadki ,Electrical engineering. Electronics. Nuclear engineering ,TA1-2040 ,Inductively coupled plasma ,Ultraviolet - Abstract
This work presents the novel and entirely green in situ synthesis of zinc oxide nanoparticles (ZnO-NP) on cotton fabric. Pomegranate peel extract was used as a reducing agent and wood ash extract was used as an alkali source for the formation of ZnO-NP from zinc acetate. Four different synthesis methods, which varied in drying between immersion of fabric in the active solutions for synthesis and the use of padding and ultrasonication, were investigated to evaluate the most suitable one to achieve excellent ultraviolet (UV) protective properties of the functionalized textile. For comparison, the cotton fabrics were also functionalized with each active solution separately or in a combination of two (i.e., Zn-acetate and plant extract). Scanning electron microscopy (SEM), inductively coupled plasma mass spectroscopy (ICP-MS), Fourier transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD) analysis, and atomic force microscopy (AFM) confirm the successful formation of ZnO-NP on cotton. Among the synthesis methods, the method that included continuous drying of the samples between immersion in the active solutions for synthesis (Method 4) was found to be the most suitable to deliver uniformly impregnated cotton fibers with numerous small ZnO wurtzite structured crystals and excellent UV protection, with a UV protection factor of 154.0. This research presents an example of a green circular economy where a bio-waste material can be used to produce ZnO-NP directly on cotton at low temperatures and short treatment times without the addition of chemicals and enables the production of cellulosic fabrics with excellent UV protection.
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- 2021
- Full Text
- View/download PDF
13. Vpliv parametrov in-situ sinteze ZnO na bombažu za doseganje UV zaščite
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Verbič, Anja and Gorjanc, Marija
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nanodelci ,cinkov oksid ,UV sevanje ,zinc oxide ,in-situ sinteza ,bombaž ,nanoparticles ,UV protection ,in-situ synthesis ,zaščita pred UV sevanjem ,cotton ,UV radiation - Abstract
Cinkov oksid (ZnO) je anorganska spojina, ki poleg fotokatalitičnosti, polprevodnosti in protimikrobnosti nudi odlično zaščito pred ultravijoličnim (UV) sevanjem. Tekstilije, ki nudijo UV zaščito imajo izreden pomen pri preprečevanju poškodb, ki nastanejo zaradi izpostavljenosti UV sevanju. Namen raziskave magistrskega dela je bil proučiti pogoje in-situ sinteze nanodelcev cinkovega oksida (ZnO-ND) na bombažni tkanini in doseči visok ultravijolični zaščitni faktor (UZF) funkcionalizirane tkanine. V prvem delu raziskave je bil proučevan vpliv vrste reducenta (Na2CO3, KOH, NaOH) in njegove molarne koncentracije (0,1M in 1M) na oblikovanje nanodelcev in vrednost UZF bombažne tkanine. V drugem delu raziskave so bili proučevani še drugi dejavniki, kot so čas obdelave tkanine v prekurzorju (ZnCl2), čas sinteze (čas obdelave po dodatku reducenta) in čas sušenja po in-situ sintezi. Visoke vrednosti UZF (50+), ki so bile določene na UV/Vis spektrofotometru, so bile dosežene pri in-situ sintezi ZnO-ND z uporabo NaOH in KOH v molarni koncentraciji 1M. Višje vrednosti UZF so bile dosežene z uporabo NaOH kot KOH. Z masno-spektrometrično analizo induktivno sklopljene plazme (ICP-MS) je bilo potrjeno, da je vsebnost cinka na tkanini, kjer je bil za in-situ sintezo uporabljen NaOH, višja kot pri uporabi KOH. Iz posnetkov vrstične elektronske mikroskopije (SEM) je bilo razvidno, da so bili pri in-situ sintezi oblikovani ZnO-ND okrogle oblike, ki so povsem oplaščili vlakna. Ugotovljeno je bilo, da ima na tvorbo ZnO-ND in visoke vrednosti UZF tkanine izreden vpliv daljši čas sinteze, ne pa tudi daljši čas obdelave tkanine v prekurzorju. Čas sušenja po in-situ sintezi ni bistveno vplival na vrednosti UZF tkanine, je pa vplival na obliko nanodelcev, ki so se oblikovali na površini bombažnih vlaken. Z daljšim časom sušenja so se oblikovali nanodelci bolj pravilnih okroglih oblik. Funkcionalizirane tkanine niso imele dobrih obstojnosti na pranje, saj se je že po prvem pranju večina nanodelcev odstranila. Zinc oxide (ZnO) is an inorganic compound, which in addition to photocatalytic, semi-conductive and antibacterial properties, provides excellent protection against ultraviolet (UV) radiation. Textiles that offer UV protection play an important role in prevention of skin damages caused by UV radiation. The aim of master's thesis research, was to investigate different parameters of in-situ synthesis of ZnO nanoparticles (ZnO-NP) on cotton in order to achieve high UV protecton factor (UPF). In the first part of the research the influence of different reducing agents (Na2CO3, KOH, NaOH) and it's molar concentration (0,1M and 1M) on formation of nanoparticles and UPF values of cotton fabric was studied. The second part of the research was focused on other parameters of in-situ synthesis, such as treatment time in ZnCl2 precursor, synthesis time (time of treatment after adding the reducing agent) and drying time after in-situ synthesis. Using UV/Vis spectroscopy high UPF values were determined on cotton fabric, where in-situ synthesis was performed using NaOH and KOH, both in 1M molar concentration. The use of NaOH resulted in higher UPF value of cotton fabric. The content of ZnO particles was examined with inductively coupled plasma mass spectrometry (ICP-MS). As expected, the results showed higher content of zinc on the fabric, where NaOH was used for in-situ synthesis. Scanning electron microscopy (SEM) showed that use of this reducing agent resulted in cotton fabric, completely covered with small, round shaped nanoparticles. From the second part of the research it was discovered that synthesis time has the biggest influence on UPF value of cotton fabric. Treatment time in precursor did not importantly affect the UV protection of the fabric. Besides that, longer drying time did not result in higher UPF value, although it had a big influence on morphology of the synthesized nanoparticles. With longer drying time the nanoparticles were more round shaped. The samples had poor wash fastness even after the first wash, which was observed by removal of the majority of ZnO nanoparticles.
- Published
- 2018
14. Radijaciono-hemijska sinteza termo-I pH-osetljivih antibakterijskih srebro/poli(N-izopropilakrilamid-ko- itakonska kiselina) nanokompozita
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Kalagasidis-Krušić, Melina, Radosavljević, Aleksandra, Nikolić, Marija, Kačarević-Popović, Zorica M., Milosavljević, Nedeljko, Spasojević, Jelena P., Kalagasidis-Krušić, Melina, Radosavljević, Aleksandra, Nikolić, Marija, Kačarević-Popović, Zorica M., Milosavljević, Nedeljko, and Spasojević, Jelena P.
- Abstract
U okviru ove doktorske disertacije izvedena je radijaciono-hemijska sinteza i karakterizacija novih nanokompozita na bazi umreţenih polimernih matrica N-izopropilakrilamida (NiPAAm) i itakonske kiseline (IK) i nanočestica srebra (Ag/P(NiPAAm/IK)). Za sintezu nanokompozita je korišćena radiolitička metoda koja omogućava umreţavanje i fino podešavanje svojstava nosača tj. polimerne matrice, ali i formiranje nanočestica srebra ţeljenih svojstava unutar polimerne matrice (in situ sinteza). Radiolitička metoda sinteze je izvedena pod dejstvom gama zračenja na kobaltnom (60Co) izvoru. Sintetisani uzorci su podvrgnuti detaljnoj fizičko-hemijskoj karakterizaciji u cilju dobijanja informacija o polimernim matricama kao nosačima i nanočesticama srebra kao nanopuniocima, ali i u cilju ispitivanja njihovog sinergističkog dejstva u nanokompozitnim sistemima.Morfologija umreţenih sistema je ispitana primenom skenirajuće elektronske mikroskopije (SEM) i mikro kompjuterizovane topografije (mikro-CT), a studija bubrenja praćenjem kinetike bubrenja u medijumima različitih pH-vrednosti i temperature, pri čemu su simulirani fiziološki uslovi. Utvrđeno je da prisustvo itakonske kiseline i inkorporacija nanočestica srebra utiču na morfologiju nanokompozita, parametre polimerne mreţe, kao i na kapacitet bubrenja.Optička svojstva nanokompozita su ispitana metodom spektroskopije u ultraljubičastoj i vidljivoj oblasti spektra (UV-Vis) i teorijskim modelovanjem primenom MiePlot 3.4 programskog paketa čiji je algoritam zasnovan na Mie-ovoj teoriji. U apsorpcionim spektrima je zapaţena karakteristična plazmonska apsorpcija sa maksimumom u opsegu od 390 nm do 412 nm, dok jemodelovanjem određeno da se vrednost prečnika nanočestica srebra kreće između 6,8 nm i 16,2 nm..., In this study, radiation-chemical synthesis and characterization of the novel nanocomposite systems based on silver nanoparticles (AgNPs) and crosslinked copolymer matrix of N-isopropylacrylamide (NiPAAm) and itaconic acid (IA) (Ag/P(NiPAAm/IA)) were performed. Radiolytic method, which is used for synthesis, enables fine tuning of properties of polymer matrix as a carrier, as well as formation of the silver nanoparticles with desired properties within polymer matrix (in situ synthesis). The radiolytic synthesis method is carried out by gamma irradiation at a cobalt (60Co) radiation facility. Synthesized samples were undergo to detailed physico-chemical characterization in order to obtain information about polymer matrix as a carrier and silver nanoparticles as a nanofillers, but also to examine their synergistic effects in the nanocomposite systems.Morphology of the crosslinked systems was performed by scanning electron microscopy (SEM) and micro computerized topography (micro-CT), while swelling study was performed by monitoring the swelling kinetics in the swelling media with different pH and temperature, i.e. in simulated physiological conditions. It has been shown that the addition of itaconic acid and incorporation of AgNPs have influences on the morphology, network parameters as well as on the swelling capacity.The optical properties of the nanocomposites were investigated by ultraviolet–visible spectroscopy (UV-Vis) and theoretical modeling using MiePlot 3.4 software package, with algorithm based on Mie's theory. Obtained absorption spectra exhibit the characteristic plasmon peak with maximabetween 390 nm and 412 nm, while the modeling has shown that the mean size of the silver nanoparticles was in the range between 6.8 nm and 16.2 nm...
- Published
- 2016
15. Preparation of ZnO/PANI nanocomposites and its application in photocatalytic decomposition of dyes
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Živković, Ivana and Hrnjak-Murgić, Zlata
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nanokompozit ,cinkov oksid ,PANI ,nanocomposite ,Acid blue 25 bojilo ,zinc oxide ,fotokataliza ,TECHNICAL SCIENCES. Chemical Engineering. Chemical Engineering in Material Development ,simulated solar radiation ,TEHNIČKE ZNANOSTI. Kemijsko inženjerstvo. Kemijsko inženjerstvo u razvoju materijala ,simulirano Sunčevo zračenje ,Acid blue 25 colorant ,photocatalysis - Abstract
U radu provedena je in-situ sinteza polianilina (PANI) u prisustvu ZnO katalizatora za pripravu ZnO/PANI nanokompozitnog fotokatalizatora za katalitičko pročišćavanje otpadnih voda. Sinteza PANI polimera provedena je na različitim uvjetima, tj. modificiran je postupak in-situ sinteze tako da je prvo kratko sintetiziran čisti PANI polimer, a kasnije je nastavljena in-situ sinteza u prisustvu ZnO nanočestica. Također, varirano je vrijeme polimerizacije; 90 min; 120 min i 180 min. Pripremljeni uzorci ZnO/PANI nanokompozitnih fotokatalizatora karakterizirani su visokorezolucijskom pretražnom elektronskom mikroskopijom (FE-SEM), FTIR spektroskopijskom analizom te im je određena elektrovodljivost čime je potvrđena uspješna in-situ sinteza nanokompozita ZnO/PANI. Provedena je ocjena fotokatalitičke aktivnosti sintetiziranih ZnO/PANI nanokompozitnih fotokatalizatora razgradnjom Acid Blue 25 (AB25) bojila kojim je bila onečišćena voda uz simulirano Sunčevo zračenje. UV/VIS spektrofotometrom praćeno je obezbojenje u vodi, određivanjem absorbancije na λmax=622 nm za AB25 bojilo. Stupanj mineralizacije prisutnog bojila u vodi određen je mjerenjem vrijednosti ukupnog organskog ugljika (TOC) koji ukazuje na stupanj razgradnje cijele molekule bojila, a ne samo kromoforne skupine. Rezultati fotokatalitičke aktivnosti ZnO/PANI uz simulirano Sunčevo zračenje pokazuju da su sintetizirani fotokatalizatori djelotvorni, ali nije uspostavljen sinergistički efekt djelovanja ZnO i PANI polimera koji bi omogućio veću efikasnost razgradnje AB25 bojila od čistog ZnO katalizatora. The development of innovative waste water treatment technology aslo implies the development of new polymer nanocomposites with expanded photocatalytic activity, shifted towards the visible UV / VIS spectrum of solar radiation. For this reason, the quasi in situ synthesis was used to prepare the ZnO / PANI nanocomposite, which was used in photocatalysis with simulated solar radiation. High-resolution scanning electron microscopy (FE-SEM) confirmed the successful synthesis of the ZnO / PANI nanocomposite. FTIR analysis also showed the presence of the nanocomposite due to presence of characteristic vibrational tapes for PANI and ZnO. Evaluation of photocatalytic activity for prepared ZnO / PANI nanocomposite samples was carried out and purification of wastewater with Acid Blue 25 (AB25) dye was carried out. Discoloration of the wastewater was monitored by the UV / VIS spectrophotometer by determining absorbance (λ = 622 nm for AB25). The degree of mineralization of the dye in wastewater was determined by measuring the value of total organic carbon (TOC). The results of photocatalytic activity with simulated solar radiation show that photocatalyst is effective at low concentrations of contamination as confirmed by achieving a high percentage of cloudiness and relatively low (satisfactory) TOC values.
- Published
- 2017
16. Priprema ZnO/PANI nanokompozita i njegova primjena u fotokatalitičnoj razgradnji bojila
- Author
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Živković, Ivana
- Subjects
nanokompozit, cinkov oksid, PANI, fotokataliza, simulirano Sunčevo zračenje, Acid blue 25 bojilo - Abstract
U radu provedena je in-situ sinteza polianilina (PANI) u prisustvu ZnO katalizatora za pripravu ZnO/PANI nanokompozitnog fotokatalizatora za katalitičko pročišćavanje otpadnih voda. Sinteza PANI polimera provedena je na različitim uvjetima, tj. modificiran je postupak in-situ sinteze tako da je prvo kratko sintetiziran čisti PANI polimer, a kasnije je nastavljena in-situ sinteza u prisustvu ZnO nanočestica. Također, varirano je vrijeme polimerizacije ; 90 min ; 120 min i 180 min. Pripremljeni uzorci ZnO/PANI nanokompozitnih fotokatalizatora karakterizirani su visokorezolucijskom pretražnom elektronskom mikroskopijom (FE-SEM), FTIR spektroskopijskom analizom te im je određena elektrovodljivost čime je potvrđena uspješna in-situ sinteza nanokompozita ZnO/PANI. Provedena je ocjena fotokatalitičke aktivnosti sintetiziranih ZnO/PANI nanokompozitnih fotokatalizatora razgradnjom Acid Blue 25 (AB25) bojila kojim je bila onečišćena voda uz simulirano Sunčevo zračenje. UV/VIS spektrofotometrom praćeno je obezbojenje u vodi, određivanjem absorbancije na λmax=622 nm za AB25 bojilo. Stupanj mineralizacije prisutnog bojila u vodi određen je mjerenjem vrijednosti ukupnog organskog ugljika (TOC) koji ukazuje na stupanj razgradnje cijele molekule bojila, a ne samo kromoforne skupine. Rezultati fotokatalitičke aktivnosti ZnO/PANI uz simulirano Sunčevo zračenje pokazuju da su sintetizirani fotokatalizatori djelotvorni, ali nije uspostavljen sinergistički efekt djelovanja ZnO i PANI polimera koji bi omogućio veću efikasnost razgradnje AB25 bojila od čistog ZnO katalizatora.
- Published
- 2017
17. PRIPRAVA I KARAKTERIZACIJA KOMPOZITNOG MATERIJALA NA TEMELJU HIDROKSIAPATITA I BIORAZGRADIVOG POLIMERA
- Author
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Ferk, Elvira
- Subjects
hidroksiapatit (HA) ,biorazgradivi polimer ,kompozitni biomaterijal ,precipitacija iz polimerne otopine ,kompozitni film - Abstract
Cilj rada je priprava bioaktivnog i biorazgradivog kompozitnog materijala na temelju hidroksiapatita i biorazgradivog polimera koji svoju primjenu nalazi u inženjerstvu tkiva kao zamjenski materijal tvrdog koštanog tkiva (kosti i zubi). Glavni zadatak je in situ sinteza hidroksiapatita nanometarskih dimenzija u matrici biorazgradivog polimera upotrebom jeftinih i lako pristupačnih polaznih komponenti pri nižim temperaturama (bez termičke obrade). Budući da su načini regeneracije kosti upotrebom koštanih presadaka od pacijenta, donora ili životinje etički upitni i mogu uzrokovati brojne nepovoljne posljedice i komplikacije, od velike je važnosti pronaći novi materijal koji bi mogao zamijeniti svojstva i funkciju kosti za presađivanje. Dosadašnji rezultati istraživanja upućuju na to da nanostrukturirani kompozitni materijali u obliku 2D filmova ili 3D okosnica (skeleta), na temelju biorazgradivih polimera i bioaktivne keramike kao što je hidroksiapatit (HA), posjeduju sposobnost simuliranja površinskih i/ili kemijskih svojstava kosti i kao takvi predstavljaju alternativu za proteze i okosnica. Provedena su preliminarna istraživanja sinteze nanometarskog hidroksiapatita (nano-HA) precipitacijom iz vodene otopine polaznih komponenti (kalcij karbonata i uree fosfata) pri sobnoj temperaturi, 37 i 50 °C uz regulaciju pH otopine. Nakon potvrde nastanka hidroksiapatita pri svim navedenim uvjetima sinteza (FTIR spektroskopijom i rendgenskom difrakcijskom analizom) provedena je in situ sinteza nano-HA u matrici biorazgradivog polimera (kitozan) simultanom precipitacijom HA i polimera iz polimerne otopine pri prethodno navedenim uvjetima (sobna temperatura, 37 i 50 °C). Bolja topljivost kitozana kao i homogenost dobivenog kompozitnog biomaterijala postignuta je dodatkom određenog monosaharida (glukoza, fruktoza) polimernoj otopini. Sastav i struktura dobivenih kompozitnih biomaterijala utvrđeni su instrumentalnim metodama: FTIR spektroskopijom, rendgenskom difrakcijskom analizom (XRD) i simultanom termogravimetrijskom i diferencijalno toplinskom analizom (TG/DTA).
- Published
- 2012
18. Derivati izoindolina, sinteza i biološka aktivnost. I. Prirodni i sintetski derivati izoindolina.
- Author
-
Sović, I. and Karminski-Zamola, G.
- Subjects
HETEROCYCLIC compounds ,ORGANIC compounds research ,PROTEIN kinase inhibitors ,ORGANIC synthesis research ,BENZENEDICARBONITRILE - Abstract
Copyright of Kemija u Industriji is the property of Croatian Society of Chemical Engineers and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
- Published
- 2014
- Full Text
- View/download PDF
19. Visoko tehnološko razvito poliamidno pletivo s superhidrofobnimi, oleofobnimi in samočistilnimi lastnostmi
- Author
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Vidas, Andreja and Simončič, Barbara
- Subjects
oleofobnost ,SiO2 particles ,Polyamide ,sol-gel ,delci SiO2 ,zaščitne lastnosti ,oleophobicity ,protective properties ,superhidrofobnost ,Poliamid ,superhydrophobicity - Abstract
V tem diplomskem delu je bil preučevan učinek obdelave poliamidnega (PA) pletiva s postopkom sol-gel, na razvoj visokotehnolopke tekstilije z zaščitnimi lastnostmi. V izdelavo visoko tehnološkega poliamidnega pletiva so bili vključeni trije glavni postopki, ki so si sledili v naslednjem vrstnem redu: postopek apretiranja sol-gel z uporabo v naprej pripravljenih delcev SiO2, in situ sinteza delcev SiO2 v prisotnosti pletiva ter apretiranje s komercialnim perfluoriranim oligosiloksanskim sredstvom (FAS) po impregnirnem postopku. Vzorci so bili za določanje pralne obstojnosti tovrstne apreture oprani z enim (1PC) in štirimi pralnimi cikli (4PC). Obdelanim in neobdelanim vzorcem so bile določene morfološke, kemijske in mehansko-fizikalne lastnosti, ki so bile izmerjene z vrstično elektronsko mikroskopijo (SEM), infrardečo spektroskopijo s Fourerjevo transformacijo (FT-IR), merjenjem zračne prepustnosti ter pretržne trdnosti. Učinek apreture na vodo- in oljeodbojne lastnosti je bil ovrednoten na podlagi meritev statičnih stičnih kotov vode in n-heksadeksana ter kotov zdrsa kapljic vode s površine vzorcev. Rezultati so pokazali, da sta se pretržna trdnost in zračna prepustnost končnega obdelanega pletiva (vzorec PA+SP+IS+FAS) nekoliko zmanjšali v primerjavi z neapretiranim vzorcem. Tristopenjski postopek obdelave pletiva PA je omogočil doseganje statičnih stičnih kotov kapljice vode nad 140° in n-heksadeksana nad 130°. Tovrstna visokotehnološka obdelava poliamidnega (PA) pletiva se izkaže kot učinkovita pri podeljevanju zaščitnih vodoodbojnih ter še posebno oleofobnih lastnostih ter je kot rezultat podelila pletivo z zelo dobrim približkom »Lotusovega učinka«. Barvna razlika med apretiranimi in neapretiranimi vzorci ostaja praktično minimalna, pride namreč do zanemarljive potemnitve pri apretiranih vzorcih. This diploma thesis aimed to study the effect of the sol-gel treatment of polyamide (PA) knit fabric on the developement of the high-tech textile with the protective properties. Fabrication of the high-tech polyamide knit fabric included three following procedures: sol-gel treatment with the pre-prepared SiO2 particles, in situ synthesis of SiO2 particles in the presence of the knit fabric, and coating with commercial perfluorinated siloxane agent (FAS) by a pad-dry-cure process. In order to investigate the washing fastness, samples were subjected to one (1PC) and four washing cycles (4PC). The morphological, chemical and mechanical-physical properties of untreated and treated samples were evaluated by scanning electron microscopy (SEM), infrared spectroscopy by Fourier transform (FT-IR), and measurements of air permeability and tensile strenght. The effect of apreture on the water and oil repellency was evaluated by measurements of static contact angles of water and n-hexadecane droplets, and water sliding (roll-off) angles. The results showed that air permeability and tensile strenght of the final treated knit fabric slightly decreased, compared to the untreated sample. The three-step modification process enabled the achievement of the static contact angle of water and n-hexadecane higher than 140° and 130°, respectively. This high-tech modification process of the PA knit fabric enables effective fabrication of the protective highly hydrophobic and highly oleophobic properties with good washing fastness and with performance close to the »Lotus effect«. The color difference between the treated and non-treated samples remains practically minimal, with neglible darkening in the treated samples.
- Published
- 2019
20. Modifikacija i karakterizacija Ppy/TiO2 nanokompozitnog fotokatalizatora
- Author
-
Šijaković, Anamarija and Hrnjak-Murgić, Zlata
- Subjects
nanocomposite photocatalysts ,azo dyes ,modification of polypyrole ,fotokataliza ,TECHNICAL SCIENCES. Chemical Engineering. Chemical Engineering in Material Development ,vodljivi polimeri ,azo bojila ,TEHNIČKE ZNANOSTI. Kemijsko inženjerstvo. Kemijsko inženjerstvo u razvoju materijala ,modifikacija polipirola ,nanokompozitni fotokatalizatori ,conductive polymers ,photocatalysis ,modifikacija polipirola, vodljivi polimeri, nanokompozitni fotokatalizatori, azo bojila, fotokataliza - Abstract
U ovom radu provedena je in situ sinteza vodljivog polimera polipirola (PPy) uz prisustvo nanočestica titanijeva dioksida (TiO2) za pripremu nanokompozitnog fotokatalizatora (PPy/TiO2). Modificiranje PPy/TiO2 fotokatalizatora provedeno je deprotoniranjem s amonijevim hidroksidom (NH4OH) dok je proces reprotoniranja proveden s klorovodičnom kiselinom (HCl) s ciljem da se istraži utjecaj promijene vodljivosti PPy na katalitičku efikasnost tijekom procesa fotokatalize. Postupci reprotoniranja i deprotoniranja provedni su u različitim vremenskim periodima. Uzorci su okarakterizirani infracrvenom spektroskopijom s Fourierovom transformacijom (FTIR) i mjerenjem elektrovodljivosti nultog i modificiranih PPy/TiO2 fotokatalizatora. Efikasnost fotokatalitičke razgradnje organskog azo bojila Reactive Red 45 (RR45), koje je korišteno kao onečišćenje u vodi, odnosno stupanj njegovog uklanjanja praćen je mjerenjem apsorbancije UV/VIS spektroskopijom. Također, određena je i mineralizacija RR45 bojila, odnosno određena je koncentracija ukupnog organskog ugljika (TOC) koji je prisutan u otpadnoj vodi nakon fotokalize. Iz rezultata fotokatalitičke aktivnosti PPy/TiO2 katalizatora vidljivo je da se ona mijenja s modifikacijom, tj. s promjenom vodljivosti PPy odnosu na čisti sintetizirani fotokatalizator. In this paper, in situ synthesis of conductive polymer polypyrole (PPy) in the presence of nanoparticles titanium dioxide (TiO2) for the preparation of nanocomposite photocatalyst (PPy/TiO2) was performed. Modification of PPy/TiO2 photocatalyst was carried out by deprotonation with the ammonium hydroxide (NH4OH) while the reprotonation process was carried out with hydrochloric acid (HCl) to explore the influence of PPy conductivity variation on catalytic efficiency during photocatalysis. Reprotonation and deprotonation procedures are performed for different period of time. Samples are characterized by Infrared Fourier Transform Transformation (FTIR) spectroscopy and by measurement conductivity of pure and modified PPy/TiO2 photocatalysts. Efficacy of photocatalytic degradation of organic azo dye Reactive Red 45 (RR45) was followed, which was used as a water contaminant. The degree of RR45 removal was monitored by measuring the absorbance by UV/VIS spectroscopy. Also, the mineralization of RR45 was determined as it represents the concentration of total organic carbon (TOC) present in the wastewater after photocatalysis. From the photocatalytic activity of the PPy/TiO2 catalyst, it is apparent that it changes with modification, i.e. with the change of conductivity of PPy compared to the synthesized photocatalyst.
- Published
- 2018
21. Uuspoedba svojstava PANI/ZnO kompozitnog fotokatalizatora : sinteza neutralni vs. kiseli medin
- Author
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Vrban, Ivan, Živković, Ivana, Gilja, Vanja, Žic, Mark, Hrnjak-Murgić, Zlata, Vrsaljko, Domagoj, Dejanović, Igor, and Žižek, Krunoslav
- Subjects
PANI/ZnO kompozi ,fotokatalizator ,sinteza ,medij sinteze - Abstract
Polianilin/cinkov oksid (PANI/ZnO) nanokompoziti sintetizirani su in-situ, kemijskom oksidativnom polimerizacijom monomera anilina, za katalitičko pročišćavanje otpadnih voda. Sinteza PANI/ZnO nanokompozita (katalizator-N) u neutralnom provedena je u vodenom mediju s određenim udjelom organskog otapala (dietilen glikol, DEG), koncentracija dietilen glikola bila je 0, 024 mol/dm3. Postupak sinteze PANI/ZnO nanokompozita (katalizator-K) u kiselom mediju modificiran je tako da je prvo kratko sintetiziran čisti PANI polimer, a potom je nastavljena in-situ sinteza uz prisustvo ZnO nanočestica. Čisti ZnO i sintetizirani PANI/ZnO nanokompozitni fotokatalizatori karakterizirani su FTIR spektroskopski te im je određena elektrovodljivost. Fotokatalitička učinkovitost PANI/ZnO nanokompozitnih fotokatalizatora ocijenjena je analizom efikasnosti razgradnje Acid Blue 25 (AB25) bojila u vodi pod djelovanjem simuliranog Sunčevog zračenja. UV/VIS spektrofotometrijski praćeno je obezbojenje u vodi, određivanjem absorbancije na λmax = 622 nm za AB25 bojilo. Rezultati istraživanja pokazuju da PANI/ZnO nanokompozitni fotokatalizatori sintetizirani u neutralnom mediju s DEG otapalom imaju relativno dobru efikasnost fotokatalitičke razgradnje AB25 bojila dok fotokatalizatori sintetizirani u kiselom mediju imaju nižu efikasnost razgradnje uz simulirano Sunčevo zračenje.
- Published
- 2018
22. Radiation-chemical synthesis of thermo- and pH-sensitive antibacterial silver/poly(N-isopropilacrylamide-co-itaconic acid) nanocomposites
- Author
-
Spasojević, Jelena P., Kalagasidis-Krušić, Melina, Radosavljević, Aleksandra, Nikolić, Marija, Kačarević-Popović, Zorica M., Milosavljević, Nedeljko, and Kačarević-Popović, Zorica
- Subjects
nanokompoziti ,silver nanoparticles ,antimicrobial activity ,antimikrobna aktivnost ,itaconic acid ,inteligentni hidrogelovi ,gamma irradiation ,N-izopropilakrilamid ,gama zračenje ,intelligent hydrogels ,otpuštanje jona srebra ,nanocomposites ,silver ion release ,cytotoxicity ,citotoksičnost ,nanočestice srebra ,N-isopropylacrylamide ,itakonska kiselina - Abstract
U okviru ove doktorske disertacije izvedena je radijaciono-hemijska sinteza i karakterizacija novih nanokompozita na bazi umreţenih polimernih matrica N-izopropilakrilamida (NiPAAm) i itakonske kiseline (IK) i nanočestica srebra (Ag/P(NiPAAm/IK)). Za sintezu nanokompozita je korišćena radiolitička metoda koja omogućava umreţavanje i fino podešavanje svojstava nosača tj. polimerne matrice, ali i formiranje nanočestica srebra ţeljenih svojstava unutar polimerne matrice (in situ sinteza). Radiolitička metoda sinteze je izvedena pod dejstvom gama zračenja na kobaltnom (60Co) izvoru. Sintetisani uzorci su podvrgnuti detaljnoj fizičko-hemijskoj karakterizaciji u cilju dobijanja informacija o polimernim matricama kao nosačima i nanočesticama srebra kao nanopuniocima, ali i u cilju ispitivanja njihovog sinergističkog dejstva u nanokompozitnim sistemima. Morfologija umreţenih sistema je ispitana primenom skenirajuće elektronske mikroskopije (SEM) i mikro kompjuterizovane topografije (mikro-CT), a studija bubrenja praćenjem kinetike bubrenja u medijumima različitih pH-vrednosti i temperature, pri čemu su simulirani fiziološki uslovi. Utvrđeno je da prisustvo itakonske kiseline i inkorporacija nanočestica srebra utiču na morfologiju nanokompozita, parametre polimerne mreţe, kao i na kapacitet bubrenja. Optička svojstva nanokompozita su ispitana metodom spektroskopije u ultraljubičastoj i vidljivoj oblasti spektra (UV-Vis) i teorijskim modelovanjem primenom MiePlot 3.4 programskog paketa čiji je algoritam zasnovan na Mie-ovoj teoriji. U apsorpcionim spektrima je zapaţena karakteristična plazmonska apsorpcija sa maksimumom u opsegu od 390 nm do 412 nm, dok je modelovanjem određeno da se vrednost prečnika nanočestica srebra kreće između 6,8 nm i 16,2 nm... In this study, radiation-chemical synthesis and characterization of the novel nanocomposite systems based on silver nanoparticles (AgNPs) and crosslinked copolymer matrix of N-isopropylacrylamide (NiPAAm) and itaconic acid (IA) (Ag/P(NiPAAm/IA)) were performed. Radiolytic method, which is used for synthesis, enables fine tuning of properties of polymer matrix as a carrier, as well as formation of the silver nanoparticles with desired properties within polymer matrix (in situ synthesis). The radiolytic synthesis method is carried out by gamma irradiation at a cobalt (60Co) radiation facility. Synthesized samples were undergo to detailed physico-chemical characterization in order to obtain information about polymer matrix as a carrier and silver nanoparticles as a nanofillers, but also to examine their synergistic effects in the nanocomposite systems. Morphology of the crosslinked systems was performed by scanning electron microscopy (SEM) and micro computerized topography (micro-CT), while swelling study was performed by monitoring the swelling kinetics in the swelling media with different pH and temperature, i.e. in simulated physiological conditions. It has been shown that the addition of itaconic acid and incorporation of AgNPs have influences on the morphology, network parameters as well as on the swelling capacity. The optical properties of the nanocomposites were investigated by ultraviolet–visible spectroscopy (UV-Vis) and theoretical modeling using MiePlot 3.4 software package, with algorithm based on Mie's theory. Obtained absorption spectra exhibit the characteristic plasmon peak with maxima between 390 nm and 412 nm, while the modeling has shown that the mean size of the silver nanoparticles was in the range between 6.8 nm and 16.2 nm...
- Published
- 2016
23. Green Chemistry for Environmental Sustainability - Prevention-Assurance-Sustainability (P-A-S) Approach
- Author
-
Kinjal J. Shah and Kinjal J. Shah
- Subjects
- Sustainability, Green chemistry
- Abstract
Green chemistry for environmental sustainability is an interdisciplinary science that seeks to reduce environmental problems and establish global sustainability. Given the recent development of energy-efficient technologies and the synthesis of green materials, research shows that green chemistry can be a powerful candidate for future technologies. This book discusses synthesis, catalysis, nanosynthesis, green processes, energy-efficient materials, biodegradable raw materials, and comprehensive environmental remediation, making it an excellent resource for aspiring researchers. This book explains what developments are taking place in green chemistry, why it is needed, what new methods can be used to break down traditional barriers, and how researchers can integrate them into their traditional research. To overcome barriers and achieve global environmental sustainability, this book focuses on a three-tiered strategy, namely, pollution and accident Prevention, safety and security Assurance, and energy and resource Sustainability (P-A-S). This book is also an excellent resource for environmental and sustainability managers to integrate new synthetic materials or technologies based on the principle of green chemistry into their traditional work. Ultimately, this book is aimed not only at academics or scientists but also at professionals without geopolitical boundaries.
- Published
- 2024
24. Advances in Materials Science Research. Volume 54
- Author
-
Maryann C. Wythers and Maryann C. Wythers
- Abstract
This volume includes seven chapters that present recent advances in materials science research. Chapter One explores metal-based antioxidant nanomaterials and their potential role in regulating the oxidative stress response of spondyloarthritis. Chapter Two deals with the in situ synthesis and characterization of anaphoretic multifunctional coatings on titanium with advanced properties. Chapter Three presents the basics of the development of sensors with zeolites and their applications. Chapter Four reviews the methods of synthesis and electrochemical applications of graphite and its analogues. Chapter Five includes a brief overview of the obtaining of pyrite, its applications, efficiency and the mechanisms of its actions in different processes and devices. Chapter Six reviews coprecipitation, which is one of the principal synthetic methodologies used to prepare magnetic nanoparticles, followed by coating them with silica and their applications in catalytic reactions. Lastly, Chapter Seven uses a full factorial design to identify the factors in thermomechanical processes that affect the mechanical properties of low carbon steel rebars.
- Published
- 2022
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