Influence of Prolonged Sintering Time on Density and Electrical Properties of Isothermally Sintered Cordierite-based Ceramics

Mechanical activation is a commonly used and relatively fast and inexpensive procedure for sample preparation before the sintering process. Cordierite, a stoichiometric mixture of three different oxides (2MgO center dot 2Al(2)O(3)center dot 5SiO(2)) is a very attractive, widely used high-temperature ceramic material. The mechanical activation of the starting mixtures with 5.00 mass% TiO2 was performed in a high energy ball mill during 10-80 min. The applied compaction pressure before the sintering process was 2t/cm(2), based on our recent investigation. The sintering process was performed at 1350 degrees C for 2h and 4h in air atmosphere. X-ray diffraction was used to analyze the phase composition of non-activated and 80 min activated samples, sintered for 2 and 4h, respectively. Scanning electron microscopy was performed to analyze the microstructure of both compacted and sintered samples. Atomic force microscope was used to investigate the surface of the sintered samples. This paper investigates the influence of prolonged sintering time on the densities of the sintered samples, along with electrical properties

The additive influence on sintering of zno-tio2 system according to triad “synthesis-structure-properties”

U okviru ove doktorske disertacije detaljno i sistematski je proučen uticaj aditiva magnezijum oksida na sintezu i sinterovanje sistema ZnO-TiO2. Smeša prahova ZnO, TiO2, MgO (0, 1,25 i 2,50 masenih % MgO), mehanički je aktivirana mlevenjem u visokoenergetskom planetarnom mlinu u toku 15 minuta. Metodama skenirajuće elektronske mikroskopije i rendgenske difrakcije analizirane su strukturne promene u materijalu koje se dešavaju tokom mehaničkog tretmana. Diferencijalnom termijskom analizom određene su karakteristične temperature u intervalu 20-1100°C. Takođe je detaljno ispitan uticaj mehaničke aktivacije na presovanje prahova. Proučavano je sinterovanje u izotermskim uslovima na temperaturama 800, 900, 1000 i 1100°C, kao i reakciono sinterovanje u neizotermskim uslovima u temperaturnim intervalima od sobne do 800, 900, 1000 i 1100°C pomoću dilatometrijske analize. Rendgenostrukturnim proučavanjem uzoraka sinterovanih izotermski utvrđen je fazni sastav dobijenog materijala, a mikrostrukturne karakteristike skenirajućom elektronskom mikroskopijom. Analizom mikrostrukturnih parametara aktiviranih smeša utvrđeno je da se suštinske mikrostrukturne promene odigravaju uglavnom u kristalnoj strukturi ZnO. U toku mehaničkog dejstva dolazi do značajnog smanjenja veličine kristalita cink-oksida, povećanja gustine dislokacija i mikronaprezanja u njegovoj kristalnoj strukturi, dok kod titan-dioksida nije primećena takva pojava. Uticaj aditiva na reakciju u čvrstoj fazi između ZnO i TiO2 praćen je u izotermskim i neizotermskim uslovima. Predložen je mehanizam sinterovanja, utvrđeno je da se sa dodatkom aditiva temperatura početka reakcionog sinterovanja neznatno menja, reakcija formiranja spinela (cink-ortotitanata) se pomera ka višim temperaturama, ali se najveće zgušnjavanje nakon procesa sinterovanja, kako izotermskog tako i neizotermskog, dešava upravo kod smeše sa najvećom koncentracijom dodatog aditiva. Ispitivanjem električnih svojstava utvrđeno je da električna otpornost opada sa frekvencom i temperaturom sinterovanja ali i da raste sa dodatkom aditiva. Na samom kraju, zaključujemo da smo našim istraživanjima predstavljenim u ovoj doktorskoj disertaciji, definisali zavisnosti između sinteze i svojstava, koja direktno vezuje sintezu i strukturu odn. strukturu i svojstva, čime je dat i doprinos prognozi svojstava materijala.In this doctoral dissertation the influence of additive addition on the synthesis and sintering of zinc titanate, Zn2TiO4, was studied. The powder mixtures of ZnO, TiO2 and MgO (0, 1.25 and 2.50 weight % MgO) were mechanically activated by milling using a high-energy ball mill for 15 minutes. Structural changes of the material that occur during mechanical treatment were analyzed using the scanning electron microscopy and X-ray powder diffraction. The characteristics maximums in the temperature range 20-1100°C were determined using differential thermal analysis. Isothermal sintering on temperatures 800, 900, 1000 and 1100°C as well as non-isothermal reaction sintering at the same temperatures were studied. X-ray diffraction was employed to determine a phase composition of sintered samples. Scanning electron microscopy was used in order to determine the phase microstructure evolution. Analysis of microstructural parameters revealed that essential microstructural changes occur mainly in the crystal structure of ZnO. Mechanical activation caused significant reduction of zinc oxide crystallite size, and increase of dislocation density and microstrains in the crystal structure. These phenomena were not observed for titan dioxide. The influence of additive addition on solid state reaction between ZnO and TiO2 was studied in isothermal and non-isothermal conditions. It was established that MgO addition has no influence on sintering temperatures, that moves the temperature of the beginning of reaction to higher temperatures and lags the formation of spinel (zinc-titanate), but the highest densification, after isothermal as well as non-isothermal sintering, is observed within mixture with highest content of mentioned additive. The electrical resistivity data revealed a clear decrease with increasing sintering temperatures as well as slight increase with MgO addition. And finally, we can conclude that observed results presented within this doctoral dissertation gave dependences between synthesis and properties, which directly combine synthesis and structure as well as structure and properties

The Influence of Compaction Pressure on the Density and Electrical Properties of Cordierite-based Ceramics

Due to its characteristics, cordierite, 2MgO center dot 2Al(2)O(3)center dot 5SiO(2), is a high-temperature ceramic material of a great scientific interest. Mechanical activation of the starting mixtures containing 5.00 mass% TiO2 was performed in a high-energy ball mill for 10 minutes. The compaction pressure varied from 0.5 to 6tcm(-2) (49-588 MPa). The sintering process was performed at 1350 degrees C for four hours in the air atmosphere. The phase composition of the activated and sintered samples was analyzed using X-ray diffraction. Scanning electron microscopy was used to analyze the microstructure of both compacted and sintered samples. The authors have investigated the influence of compaction pressure on the sintered samples and their electrical properties

Analysis of isothermal sintering of zinc-titanate doped with MgO

The aim of this work was analysis of isothermal sintering of zinc titanate ceramics doped with MgO obtained by mechanical activation. Mixtures of ZnO, TiO2 and MgO (0, 1.25 and 2.5%) were mechanically activated 15 minutes in a planetary ball mill. The powders obtained were pressed under different pressures and the results were fitted with a phenomenological compacting equation. Isothermal sintering was performed in air for 120 minutes at four different temperatures. Structural characterization of ZnO-TiO2-MgO system after milling was performed at room temperature using XRPD measurements. DTA measurements showed different activation energies for pure and doped ZnO-TiO2 systems. Thus addition of MgO stabilizes the crystal structure of zinc titanate

Identification of Agrobacterium vitis as a causal agent of grapevine crown gall in Serbia

In 2010, a serious outbreak of crown gall disease was observed on grapevines (Vitis vinifera L. cv. Cabernet Sauvignon) in several commercial vineyards located in the Vojvodina province, Serbia. Bacteria were isolated from the young tumor tissue on nonselective YMA medium and five representative strains were selected for further identification. Tumorigenic (Ti) plasmid was detected in all strains by PCR using primers designed to amplify the virC pathogenicity gene, producing a 414-bp PCR product. The strains were identified as Agrobacterium vitis using differential physiological and biochemical tests, and a multiplex PCR assay targeting 23S rRNA gene sequences. In the pathogenicity assay, all strains induced characteristic symptoms on inoculated tomato and grapevine plants. They were less virulent on tomato plants in comparison to the reference strains of A. tumefaciens and A. vitis. [Ministarstva nauke Republike Srbije, br. III46008: Development of integrated management of harmful organisms in plant production in order to overcome resistance and to improve food quality and safety

Sintering of mechanically activated magnesium-titanate and barium-zinc-titanate ceramics

In this article the influence of mechanical activation on sintering process of magnesium-titanate and barium-zinc-titanate ceramics has been investigated. Both nonactivated and mixtures treated in planetary ball mill for 80 minutes were sintered at 1100ºC and 1300ºC. The influence of mechanical activation on phase composition and crystal structure has been analyzed by XRD, while the effect of activation and sintering process on microstructure was investigated by scanning electron microscopy. It has been established that temperature of 1100ºC was to low to induce final sintering stage for both systems. Moreover, we concluded that barium-zinc-titanate ceramics exhibited better sinterability than magnesium-titanate ceramics

Influence of mechanical activation on microstructure and crystal structure of sintered MgO-TiO2 system

Mixtures of MgO-TiO2 were mechanically activated using high-energy planetary ball mill during 5, 10, 20, 40, 80 and 120 minutes. Sintering process was preformed in air at 1100°-1400°C for 2h. The decrease in powder's particle size was noticed as the time of mechanical activation increased and confirmed by particle size analyzer. XRD analyses were performed in order to acquire the information about phase composition. Different ratio mixtures of MgTiO3 and Mg2TiO4 are present within all sintered samples. The effect of tribophysical activation on microstructure was investigated by scanning electron microscopy. The differential thermal gravimetric analysis has been performed in order to investigate thermal behaviour of the mixtures.Smeše MgO-TiO2 su mehanički aktivirane u visoko-energetskom planetarnom mlinu tokom 5, 10, 20, 40, 80 i 120 minuta. Fazni sastav je određen rendgenskom difrakcijom. Sa porastom vremena mlevenja, primećeno je smanjenje veličine čestica praha. Takođe, ispitan je i efekat tribofizičke aktivacije na mikrostrukturu praha metodom skenirajuće elektronske mikroskopije. Radi ispitivanja termičkih svojstava praha, urađena je diferencijalna termijska analiza. Proces sinterovanja izveden je u vazduhu u temperaturnom opsegu od 1100°-1400°C tokom 2 sata. U svim sinterovanim uzorcima uočeno je prisustvo dve faze MgTiO3 i Mg2TiO4 ali njihov međusobni odnos koncentracija varira u odnosu na temperaturu sinterovanja

Phenolics content and antioxidant capacity of commercial red fruit juices

The content of phenolics: total phenols (TP), flavonoids (TF), anthocyanins (TA) and hydroxicinnamic acid as well as the total antioxidant capacity (TAC) in nine commercial red fruit juices (sour cherry, black currant, red grape) produced in Serbia were evaluated. The total compounds content was measured by spectrophotometric methods, TAC was determined using DPPH assays, and individual anthocyanins and hydroxycinnamic acids was determined using HPLC-DAD methods. Among the examined fruit juices, the black currant juices contained the highest amounts of all groups of the phenolics and exhibited strong antioxidant capacity. The amount of anthocyanins determined by HPLC method ranged from 92.36 to 512.73 mg/L in red grape and black currant juices, respectively. The anthocyanins present in the investigated red fruit juices were derivatives of cyanidin, delphinidin, petunidin, peonidin and malvidin. The predominant phenolic acid was neoclorogenic acid in sour cherry, caffeic acid in black currant, and p-coumaric acid in black grape juices. Generally, the red fruit juices produced in the Serbia are a rich source of the phenolic, which show evident antioxidant capacity

Polyphenol content and antioxidant activity of sour cherries from Serbia

The aim of this study is to evaluate the content of phenolics: the total phenols (TP), flavonoids (TF), anthocyanins (TA), as well as the total antioxidant capacity (TAC) in three sour cherry cultivars (Prunus cerasus L.) introduced to the southeast Serbia climate conditions. Among the researched sour cherries, ‘Oblacinska’ cultivar contained the highest amounts of all groups of phenolics, followed by ‘Cigancica’ > ‘Marela’. A significant difference were observed in the phenolic content among different cultivars and growing seasons (p<0.05), and the phenolic compounds were significantly higher in the growing season 2009. The examined cultivars possess a high antioxidant capacity, and all phenolics of highy correlation with TAC. The following compounds were identified and quantified using HPLC-DAD: 4 anthocyanins, the most abundant of which was cyaniding-3-glucoside in ‘Marela’ and ‘Oblacinska’, and cyanidin-3-glucosylrutinoside in ‘Cigancica’, and 4 hydroxycinnamic acids, the most abundant of which was neochlorogenic acid in all sour cherry cultivars. The growing and ripening process on the tree of sour cherry cv. Oblacinska was evaluated, also. The results showed significant increases in total phenols during the ripening, the total anthocyanins and total antioxidant capacity and 4 quantified anthocyanins, however the neochlorogenic acid decreased during the ripening. The study indicated that the growing and climate conditions in southeast Serbia are convenient for introducing sour cherry cultivars