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EN
The paper presents the influence of ZrO2 coating on Ti6Al7Nb titanium alloy depending on the method of deposition. The coatings were made by sol-gel method and atomic layer deposition (ALD). Wettability tests, pitting corrosion assessment and electrochemical impedance spectroscopy (EIS) were carried out in the paper. Complementary macro- and microscopic observations, roughness analysis by profilometric method and atomic force microscopy (AFM) were made. Based on the results obtained, it can be concluded that the type of method of depositing the layer on the surface of the material has a significant influence on its properties and that it should be taken into account during the process of the material improvement. Drawing on the findings presented, it can be inferred that roughness has a significant impact upon the surface wetttability of the tested surfaces and their related corrosion resistance. The obtainment of hydrophobic surfaces is for smaller rougidity values.
EN
The paper discusses preparation and characteristics of silica hydrophobic layers deposited on the plasma-modified glass supports. The surfaces were investigated using wettability measurements, profilometry, photoacoustic and infrared spectroscopy, X-ray photoelectron spectroscopy as well as scanning electron microscopy. The wettability measurements showed that the obtained surfaces are hydrophobic – the water contact angle was in the range of 140-150 degrees. The photoacoustic and infrared spectroscopy as well as X-ray photoelectron spectroscopy disclosed the surface compositions, particularly that of the hydrophobic alkyl groups deposited on them. They were methyl groups introduced during hydrophobization by hexamethyldisilazane. In addition, it was found that the number of groups on the surface depends on the kind of plasma by which the supports were activated. The optical profilometer showed differences in the surface roughness which affects their hydrophobicity. Moreover, the surface free energies were determined using the contact angle hysteresis method. They disclosed differences in each surface, depending on the way of supports activation. The largest hydrophobicity was obtained on the layer deposited on the support activated by the argon plasma. However, support activation by the air plasma resulted in a decrease of hydrophobicity compared to that of the non-activated surface.
EN
In this work, the fabrication of glass-ceramic materials containing MF3:Eu3++ (M = La, Gd) nanocrystals dispersed in silica sol-gel hosts has been presented. The transformation from liquid sols towards bulk samples was also examined based on IR measurements. The crystallization temperatures and formation of MF3 phases were verified based on TG/DSC analysis and XRD measurements. The optical properties of prepared Eu3+5D05D0 → 7FJ (J = 1–4) emission bands, which were recorded within the reddish-orange spectral area under near-UV illumination (λexc = 393 nm). Recorded luminescence spectra and double-exponential character of decay curves for prepared glass-ceramic samples indicated the successful migration of Eu3+ dopant ions from amorphous silica framework to low-phonon energy MF3 nanocrystal phases.
EN
Binary and ternary nanocomposites based on TiO2, SiO2 and ZnO were synthesized by PVA-based template-free gel combustion method. The morphology and the particles sizes of the synthesized samples depended on some parameters including the initial concentrations of metal salts and PVA amount in the sol, solvent composition and solution pH. Effects of these parameters were investigated and optimized by using the Taguchi method. In the experimental design, the Taguchi L25 array was used to investigate six factors at five levels. The samples were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) specific surface areas, scanning electron microscopy (SEM). The obtained results showed that the present method can be used to synthesize TiO2/SiO2/ZnO ternary nanocomposite with an effective surface area of 0.3 m2 · g−1 and ZnO/TiO2, TiO2/SiO2, ZnO/SiO2 binary nanocomposites with an effective surface area of 234 m2 · g-1, 6 m2 · g-1 and 0.5 m2 · g-1, respectively. The ZnO/TiO2 nanocomposite which was synthesized under the following experimental conditions: 2.5 wt.% Zn salt, 2.5 wt.% Ti salt, 2.0 wt.% PVA, pH = 1 and ethanol:water ratio 30:70 was selected by the Taguchi method as an optimum sample with the smallest particles (average diameter = 50 nm).
EN
Nanocomposite silica thin films made using the sol-gel method were studied. The nano-silica films were prepared using a mixture of tetraethyl orthosilicate (TEOS), deionized water, ethanol, and ammonia solution. To control the growth of the particles inside the film, the nanocomposite silica film was prepared using a mixture of the nano-silica sol and the silica sol. The change in the particle size with the heat treatment temperature ranging from 450 °C to 1100 °C was investigated. X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), NKD (refractive index-N, extinction coefficient-K, and thickness-D) and ultraviolet-visible (UV-Vis) spectrophotometry were used for characterization purposes. The XRD studies showed that the nano-silica thin films were amorphous at all annealing temperatures except for 1100 °C. The α-cristobalite crystal structure formed at the annealing temperature of 1100 °C. Optical parameters, such as refractive indices and extinction coefficients, were obtained using the NKD analyzer with respect to the annealing temperature of the films. The activation energy and enthalpy of the nanocomposite silica film were evaluated as 22.3 kJ/mol and 14.7 kJ/mol, respectively. The cut-off wavelength values were calculated by means of extrapolation of the absorbance spectra estimated using the UV-Vis spectroscopy measurements. A red shift in the absorption threshold of the nanocomposite silica films indicated that the size of the silica nanoparticles increased with an increase of the annealing temperatures from 450 °C to 900 °C, and this confirms the quantum confinement effect in the nanoparticles.
EN
Hydroxyapatite (HAp) ceramic materials are consi-dered as one of the most promising implant materials in bone surgery and in dentistry. They exhibit unique biocompatibility, bioactivity, and osteoconductivity, which are the most desirable biomaterial features. However, HAp itself is brittle, has low strength, high degree of crystallinity and low solubility at physiological pH. Doping synthetic HAp with metal ions plays an important role in improving its structural and physico--chemical properties. HAp doped with niobium ions has not been widely investigated so far. However, the results of studies available in the literature show that the synthesized CaO-P2O5-Nb2O5 compounds still show good biocompatibility, very low cytotoxicity and, additionally, they stimulate osteoblast proliferation. Therefore, this study is dedicated to the niobium--doped HAp ceramics obtained by two methods: mechano-chemical synthesis and sol-gel method. Bioceramics chemical composition, morphology, and structure were characterized by means of scanning electron microscopy imaging, BET method, X-ray diffraction, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The results indicate that nanoceramics of non-stoichiometric HAp with a clear Ca deficiency on the nanograin surface were obtained. Moreover, it has been observed that the presence of Nb dopants and the synthesis method directly affect unit cell parameters, crystallinity degree, crystallites size, porosity and distribution of niobium in the grain structure. Mechano-chemical synthesis has allowed effective niobium incorporation into the HAp structure, leading to the quite homogeneous Nb distribution in the grain volume. Whereas, Nb-doping by sol-gel method has led to dopants location mainly on the grain surface.
7
Content available remote Synthesis and characterization of TiO2 thin film on fly ash cenospheres
EN
Titanium dioxide (TiO2) thin films obtained on quartz glass and fly ash cenospheres were studied. Titanium(IV) butoxide (Ti(OBu)4), diethanoloamine (DEA), ethanol and deionized water were used as the starting materials. A layer of TiO2 nanoparticles was coated on the surface of the substrates using the sol-gel method. The thickness of the TiO2 coatings and the influence of the annealing temperature on the formation of TiO2 crystallites were studied. The dried gels were treated for 90 min in the temperature range of 400÷640°C to obtain crystallized anatase and rutile. Additional nanopowder TiO2 samples were prepared and their crystallinity was determined using X-ray diffraction (XRD). It was successfully shown that the anatase crystalline phase is formed when the TiO2 gel is heated to 480°C, while the rutile phase is obtained at 640°C. Changes in film thickness were studied using an atomic force microscope (AFM). The profound effect of gel viscosity on the thickness of the film was noticed. UV-Vis absorption spectroscopy, performed on the sample treated at 480°C (containing anatase phase only), showed strong ultraviolet light absorption below 400 nm. The estimated band-gap value was 3.2 eV. Transmission scanning microscopy (TEM) examination of the powders revealed agglomerated nanoparticles. A uniform, continuous layer on the surface of the treated microspheres was observed under a scanning electron microscope (SEM). The study shows that the annealing temperature has a profound effect on the phase composition and crystallite size of the sol-gel synthesized TiO2 nanopowders.
PL
Badaniom poddano warstwy z dwutlenku tytanu (TiO2), które zostały osadzone na powierzchni szkła kwarcowego i mikrosfer z popiołów lotnych. Wyjściowymi substratami były butanolan tytanu(IV) (Ti(OBu)4), dietanoloamina (DEA), etanol i woda dejonizowana. Warstwy z nanocząstkami TiO2 przygotowano, wykorzystując metodę zol-żel. Zbadano grubość otrzymanych warstw oraz wpływ temperatury wypalania na powstawanie krystalitów TiO2 syntetyzowanych w zol-żelu. Wysuszone żele poddano obróbce termicznej w zakresie temperatur 400÷640°C przez 90 minut w celu uzyskania krystalicznych form anatazu i rutylu. Za pomocą dyfrakcji rentgenowskiej (XRD) określono skład fazowy nanoproszków TiO2. Udało się wykazać, że krystaliczny anataz otrzymywany jest podczas ogrzewania żelu w temperaturze 480°C, natomiast krystaliczna faza rutylowa w 640°C. Zmianę grubości warstwy obserwowano z wykorzystaniem mikroskopu sił atomowych (AFM). Zaobserwowano duży wpływ lepkości zolu na grubość otrzymywanych powłok. Przeprowadzona przy użyciu spektroskopii absorpcyjnej UV-Vis analiza próbki poddanej obróbce termicznej w 480°C (w której jedyną występującą fazą był anataz) wykazała silną absorpcję promieniowania ultrafioletowego o długości fali poniżej 400 nm. Szacowana wartość energii pasma wzbronionego wynosiła 3,2 eV. Obrazy z transmisyjnego mikroskopu skaningowego (TEM) ukazały zaglomerowane nanocząstki, a obrazy ze skaningowego mikroskopu elektronowego (SEM) pokazały jednorodną warstwę na mikrosferach. Wykonane badania pokazują, że temperatura wypalania ma ogromny wpływ na skład fazowy i rozmiar krystalitów nanoproszków TiO2 syntetyzowanych metodą zol-żel.
EN
Purpose: The main purpose of this publication is to bring closer method of synthesis and examining basic properties of TiO2, ZnO and NiO nanoparticles (NPs), and investigate their possible biomedical application. Design/methodology/approach: Nanopowders were made with sol-gel method. Surface morphology studies of the obtained materials were made using Zeiss's Supra 35 scanning electron microscope and the structure using S/TEM TITAN 80-300 transmission electron microscope. In order to confirm the chemical composition of observed nanopowders, qualitative tests were performed by means of spectroscopy of scattered X-ray energy using the Energy Dispersive Spectrometer (EDS). The DLS (Dynamic Light Scattering) method was used to analyse the particle size distribution using the AntonPaar Litesizer 500 nanoparticle size analyser. Changes in particle size distribution at elevated temperatures were also observed. The TiO2, ZnO and NiO NPs with spherical shape were successfully produced by sol-gel method. Findings: The diameter of the as prepared nanoparticles does not exceed 25 nm which is confirmed by the TEM analysis. The highest proportion among the agglomerates of the nanoparticles has been shown to show those with a diameter of 80 to 125 nm. The qualitative analysis of EDS confirmed the chemical composition of the material. Practical implications: Nanoparticles (NPs) has been receiving an incrementally increasing interest within biomedical fields researchers. Nanoparticles properties (physical, chemical, mechanical, optical, electrical, magnetic, etc.) are different from the properties of their counterparts with a larger particle size. Originality/value: The nanoparticles were prepared using sol-gel method which allows the particle size to be controlled in a simple way.
EN
Mg substituted cobalt ferrite spinel powder samples with the general formula MgxCo1 – xFe2O4 (x = 0 to 0.25) were synthesized chemically through sol-gel method and annealed at 1100 °C for 2 h. They were initially screened for the structural and morphological properties by X-ray diffraction and field emission scanning electron microscopy, respectively. Vibrational properties of the samples were studied by Raman and infrared spectroscopies. X-ray diffraction confirmed the formation of single pure or near-pure phase with cubic spinel structure for all the samples with expected occupancy values. The field emission scanning electron microscopy revealed a decrease in the particle size with an increase in Mg concentration. Both structural and magnetic properties of the samples were characterized using Mössbauer spectroscopy while the magnetic properties were studied using vibrating sample magnetometry. The changes in magnetic moment of ions, their coupling with neighboring ions and cation exchange interactions were confirmed from the Mössbauer spectroscopy analysis. Saturation magnetization and coercivity values can be explained based on the Slater-Pauling curve. The magnetometry results showed a decrease in saturation magnetization of the samples with increase in Mg concentration.
EN
U-type ferrite typified by Ba4Co2Fe36O60 is used as a RAM (Radar Absorbing Materials) in the X-band (8-12 GHz). Ba4Co2Fe36O60 is known to have a complex crystal structure, which makes it difficult to obtain single phase and have low reproducibility. Previously known U-type ferrites have been fabricated based on a ceramic process that mixing (by a ball mill), calcining, grinding, binder mixing, drying, sieving, pressing and sintering. In contrast, the process of preparing the powder by the sol-gel method and its heat-treating is advantageous in that it can reduce the process steps and the required time. In addition, the precise stoichiometric control by the sol-gel method can effectively evaluate the effect of added or substituted elements. In this study investigates the crystal structure of Ba4Co2Fe36O60 synthesized by the sol-gel method and the morphology of U-type ferrite nano-powders according to various heat treatment conditions. Analysis of the crystal structure is used for XRD. Morphology and size are observed by SEM. In addition, VSM is performed to confirm the change of magnetic properties according to various heat treatment conditions.
EN
The goal of this article was to review the literature which discusses the problem of oily wastewater purification by membrane filtration. The authors focused on membranes containing zirconium compounds, mainly ZrO2, used in pressure driven membrane processes. The efficiency of the oil removal processes for various membranes (ceramic and composite), usually above 95% for the oil contaminated sewage, was compared. The influence of zirconium compounds on the properties of ceramic membranes was also discussed. The methods of producing ceramic membranes have been briefly characterized as well. Ceramic membranes are usually obtained by sol-gel technique but also by isostatic compression, reverse phase technique, or hydrothermal crystallization. Ceramic membranes are formed with zirconia, which cause an increase in filtration efficiency by improvement of hydrophilic properties of the membrane. Moreover, the addition of ZrO2 results in increased chemical and hydrothermal membrane stability. The efficiency of the filtration processes using the presented membranes was high, suggesting that membrane filtration processes are highly effective purification methods.
PL
Artykuł stanowi przegląd literatury, w którym omówiono problem oczyszczania ścieków olejowych w oparciu o filtrację membranową. Skupiono się na membranach ciśnieniowych zawierających związki cyrkonu, głównie ZrO2. Porównano skuteczność procesów oczyszczania dla różnych membran (ceramicznych i kompozytowych). Omówiono wpływ związków cyrkonu na właściwości użytkowe membran ciśnieniowych. Membrany ceramiczne są zwykle uzyskiwane za pomocą techniki zol-żel, ale również przez prasowanie izostatyczne, technikę odwróconej fazy lub krystalizację hydrotermiczną. Membrany ceramiczne są formowane z tlenkiem cyrkonu, co skutkuje wzrostem skuteczności filtracji.
PL
Metodą zol-żel nanoszono powłoki SiO₂ na podłoże ze stali nierdzewnej 316L w celu poprawy bioaktywności oraz odporności korozyjnej materiału. Powłoki otrzymywano z zolu zawierającego tetraetoksysilan (jako prekursor) oraz alkohol izopropylowy lub alkohol butylowy jako rozpuszczalnik. Próbki eksponowano w roztworze sztucznej krwi (SBF) przez 142 doby. Badania SEM i EDS wykazały, że wielowarstwowe powłoki SiO₂ uzyskane z zolu zawierającego izopropanol sprzyjają tworzeniu ceramiki apatytowej, co może świadczyć o ich bioaktywności. Zgodnie z wynikami badań potencjodynamicznych i ICP odporność korozyjna stali w roztworze SBF wzrasta po osadzeniu powłok SiO₂ metodą zol-żel.
EN
Single and multilayer SiO₂ coatings were deposited on 316L steel from (EtO) ₄Si-contg. iso-PrOH or BuOH solutions and immersed in artificial blood soln. for 142 days. The sample surfaces were studied by energy-dispersive spectroscopy. Iso-PrOH was a more efficient solvent than BuOH in generating the layer bioactivity. The corrosion resistance of the coating increased with increasing no. of layers.
PL
Metodą zol-żel nanoszono powłoki ZrO2 na podłoże ze stali nierdzewnej 316L. Powłoki otrzymywano z zolu zawierającego jako prekursor tetraetoksycyrkonian i butanol jako rozpuszczalnik. Otrzymane próbki eksponowano w roztworze sztucznej krwi (SBF) przez 120 doby. Badania potencjodynamiczne wykazały, że osadzenie pięciowarstwowych powłok ZrO2 powoduje dwukrotny wzrost odporności korozyjnej stali w czasie długoterminowej ekspozycji w roztworze SBF. Zgodnie z wynikami badań SEM i EDS wykazano, że na powierzchni cienkich warstw ZrO2 przyrasta ceramika apatytowa.
EN
ZrO2 coatings were sol-gel deposited on a base made of stainless steel 316L. The sol used for this purpose contained zirconium(IV) ethoxide (ZrEt) as the precursor and butanol as the solvent. The obtained samples were exposed to simulated body fluid (SBF) for 120 days. Potentiodynamic tests showed that the deposition of five-layer ZrO2 coatings results in a twofold increase in the corrosion resistance of the steel during long-term exposure to SBF. The results of SEM and EDS analyses demonstrated that apatite ceramic accretes on the surface of the thin ZrO2 layers.
PL
Celem pracy było otrzymanie wieloskładnikowej ceramiki typu PZT domieszkowanej chromem, tantalem i manganem, wykorzystując mokrą metodę chemiczną zol-żelową. Proces technologiczny otrzymywania ceramiki składał się z kilku etapów. W pierwszym etapie ceramiczny proszek o składzie Pb(Zr0,75Ti0,25)O3 otrzymano w wyniku syntezy zol–żelowej, a następnie w drugim etapie do bazowego składu wprowadzono domieszki w postaci tlenków chromu (w ilości 0,15% wag.), tantalu (w ilości 0,03% wag.) oraz manganu (w ilościach 0,5% wag. lub 1,0% wag.). Syntezowanie poszczególnych składników przeprowadzono metodą reakcji w fazie stałej, natomiast spiekanie zsyntezowanego materiału przeprowadzono dwiema metodami zagęszczania: spiekaniem swobodnym (FS) i metodą jednoosiowego prasowania na gorąco (HUP). Przeprowadzono badania mikrostrukturalne, rentgenowskie, homogeniczności składu (EDS) oraz podstawowych właściwości ferroelektrycznych i dielektrycznych. Badania wykazały, że wielopierwiastkowe modyfikowanie podstawowego składu Pb(Zr0,75Ti0,25)O3 domieszkami tlenków chromu, tantalu i manganu poprawia parametry użytkowe otrzymanych materiałów. Natomiast zastosowanie w procesie technologicznym metody jednoosiowego prasowania na gorąco (HUP) pozwala uzyskać próbki o jednorodnej drobnoziarnistej mikrostrukturze z większymi wartościami maksymalnej przenikalności elektrycznej. Wieloskładnikowe materiały typu PZT o tego typu właściwościach mogą znaleźć zastosowania w mikroelektronice i mikromechatronice do budowy wysokoczęstotliwościowych przetworników piezoelektrycznych.
EN
The aim of this work was to obtain multicomponent PZT-type ceramics doped with chromium, tantalum and manganese oxides. A technological process of obtaining the ceramics consisted of several stages. In the first step, the Pb(Zr0.75Ti0.25)O3 ceramic powder was synthesized by a sol-gel method, and in the second one, an admixture of chromium (0.15 wt.%), tantalum (0.03 wt.%) and manganese (0.5 wt.% or 1.0 wt.%) oxides was introduced to the base composition. The synthesis of individual components was performed by a solid phase reaction, and the sintering process was carried out by two methods: free sintering (FS) and hot uniaxial pressing (HUP). Microstructural studies, X-ray diffraction phase analysis, studies of the material homogeneity (EDS), and the basic ferroelectric and dielectric properties were carried out. The studies have shown that the multi-elemental modification of the basic composition of Pb(Zr0.75Ti0.25)O3 by the admixtures of chromium, tantalum and manganese oxides improve the performance of the obtained ceramics. The application of the hot uniaxial pressing method (HUP) in the technological process allows obtaining a sample with the homogeneous fine-grained microstructure and higher values of the maximum dielectric permittivity. The multicomponent PZT-based materials with that type of properties can be used in microelectronics and micromechatronics to build high-frequency piezoelectric transducers.
EN
In the present research technology of compositionally graded barium strontium titanate Ba1-xSrxTiO3 thin films deposited on stainless steel substrates by sol-gel spin coating followed with thermal annealing at T = 650°C is reported. Results of thermal behavior of the sol-gel derived powders with compositions used for fabrication of graded structure (i.e. with Sr mole fraction x =0.5, 0.4 and 0.3) are described. X-ray diffraction studies of the phase composition and crystal structure of such complex thin film configuration are given. It was found that gel powders exhibited a large total weight loss of about Δm ≈ 44-47%. Three stages of weight loss took place at temperature ranges: below T ≈ 300°C, at ΔT ≈ 300-500°C and between T = 600°C and T = 800°C. Phase analysis has shown that the dominating phase is Ba0.67Sr0.33TiO3 compound while the second phase is Ba0.7Sr0.3TiO3 or Ba0.5Sr0.5TiO3 for “up-graded” and “down-graded” structure, respectively.
EN
ZnO-SnO2 nanocomposite was prepared by the sol-gel method. The as-prepared nanocomposite was characterized by X-ray diffraction (XRD), scanning electron micrograph (SEM-EDX), FTIR and UV-Visible spectrometer analysis techniques. The average particle size of nanocomposite was calculated from the XRD study. The average particle size of the prepared nanocomposite was 22 nm. According to the UV-Visible spectrum, the band gap value of 5.06 eV was obtained for the ZnO-SnO2nanocomposite. From the analysis techniques it was found that the metal oxides of ZnO-SnO2 mainly consist of ZnO and SnO2 metal oxides. The antibacterial and antifungal activities of the ZnO-SnO2nanocomposite were studied against Staphylococcus aureus (ATCC25923), Listeria monocytogenes (ATCC 11994)(Gram-positive), Salmonella typhi (ATCC14028), Escherichia coli (ATCC 25922)Gram-negative), Candida albicans (ATCC10231), and Aspergillus niger (ATCC 16404) (fungi)by two methods through the turbidity method or reading optical density and inhibition zone, which were carried out in the absence of irradiation. We observed an effective antibacterial and antifungal activity of the ZnO-SnO2 nanocomposite against bacteria and fungi.
PL
Metodą zol-żel otrzymano na stali 316L trójwarstwowe powłoki ceramiczne SiO2 z zolu zawierającego tetraetoksysilan oraz jako rozpuszczalniki alkohol izopropylowy i alkohol butylowy. Ekspozycja próbek w roztworze sztucznej krwi przez 142 doby wykazała korzystne właściwości korozyjne próbek z powłoką SiO2 w porównaniu do niepokrytej stali. Przy stosowaniu alkoholu izopropylowego jako składnika zolu odporność korozyjna próbek wzrosła 4 razy. Powłoki ceramiczne SiO2 tworzą warstwę barierową oraz, co wykazano w badaniach EDS, sprzyjają tworzeniu warstwy hydroksyapatytu. Zmierzony stosunek wielkości pików Ca i P w warstwie wierzchniej próbek z powłoką odpowiada stosunkowi tych pierwiastków jaki występuje w syntetycznych hydroksyapatytach.
EN
Three-layer ceramic SiO2 coatings were deposited on steel 316L, from a sol containing tetraethoxysilane as well as isopropyl alcohol and butyl alcohol as the solvents. The exposure of the samples to a Simulated Body Fluid (SBF) for 142 days showed that the samples with the SiO2 coating were more corrosion resistant than the uncoated steel. When isopropyl alcohol was used as a component of the sol the corrosion resistance of the samples increased fourfold. Ceramic SiO2 coatings form a barrier layer and, as shown by EDS analyses, favour the formation of a hydroxyapatite layer. The ratio of Ca and P peak sizes measured in the surface layer of the coated samples corresponds to the ratio of these elements which occurs in synthetic hydroxyapatites.
18
EN
The paper presents production of TiO2-SnO2 nanocom-posites with the use of sol-gel method combined with hydrothermal processing of the formed hydroxide gel. As proven by XRD analysis, both oxides crystallise in tetragonal systems: TiO2–anatase, SnO2–cassiterite. Mean sizes of the crystallites are TiO2 ~30÷40 nm and SnO2 ~3÷4 nm, respectively. Moreover, the produced TiO2-SnO2 nanocomposites are characterised by a high specific surface area (~100 m2/g).
PL
W pracy opisano otrzymywanie nanokompozytów TiO2-SnO2 metodą zol-żel połączoną z obróbką hydrotermalną otrzymanego żelu wodorotlenkowego. Analiza XRD wykazała, że obydwa tlenki krystalizują w strukturach tetragonalnych: TiO2–anataz, SnO2–kasyteryt. Średnie wielkości krystalitów wynoszą odpowiednio TiO2 ~30÷40 nm, SnO2 ~3÷4 nm. Ponadto, otrzymane nanokompozyty TiO2-SnO2 charakteryzują się dużym rozwinięciem powierzchni właściwej (~100 m2/g).
19
Content available remote Otrzymywanie ceramiki tytanianu baru domieszkowanego La3+ metodą zol-żel
PL
W prezentowanej pracy z udziałem metody zol-żel wytworzono ceramikę tytanianiu baru domieszkowaną lantanem (Ba1-xLax)Ti1-x/4O3 (BLT), gdzie 0 ≤ x ≤ 0,005. Amorficzne żele kalcynowano w temperaturze 850 ºC i przy pomocy prasy hydraulicznej formowano wypraski w kształcie dysków, a następnie spiekano swobodnie w oporowym piecu silitowym HTC 1500 w temperaturze 1450 ºC przez 4 h. Proces syntezy ceramiki badano za pomocy analizy termograwimetrycznej (TG, DTG) i różnicowej analizy termicznej (DTA) przy pomocy derywatografu MOM Q-1500D. Badania mikrostruktury otrzymanej ceramiki przeprowadzono przy pomocy skaningowego mikroskopu elektronowego HITACHI S-4700. Strukturę krystaliczną i skład fazowy otrzymanych materiałów ceramicznych badano metodą dyfrakcji rentgenowskiej przy użyciu dyfraktometru rentgenowskiego Philips WP 3710.
EN
The (Ba1-xLax)Ti1-x/4O3 (BLT) ceramics with a lanthanum content of 0 ≤ x ≤ 0.005 were prepared by using the sol-gel method. Amorphous gels of BLT were calcined at a temperature of 850 ºC and pressed into pellets. The compacts were next sintered by the free sintering method at a temperature of 1450 ºC for 4 h. Simultaneous thermal analysis (STA) was used, in which both thermal analysis (DTA) and mass change effects (TG and DTG) were measured concurrently on the same sample using a derivatograph MOM Q-1500D. The morphology of BLT ceramics was studied by scanning electron microscopy (HITACHI S-4700). The crystalline structure of BLT ceramics was studied by the X-ray diffraction method.
EN
In high Tc superconductors (HTSC) the activation energy gives information about the pinning properties of a sample under applied magnetic field. Pinning of vortices determines the critical current density Jc which is of great importance for practical applications of HTSC. Instead of magnetic measurements, the activation energy may be calculated from resistivity measurements realized under magnetic field. This kind of measurement has been made in this work for yttrium doped samples of Bi2Sr2CaCu2O8+d (Bi-2212) for different values of applied magnetic field. Samples of Bi2Sr2Ca1-xYxCu2O8+d (x = 0, 0.025, 0.1, 0.25) were prepared by a sol-gel method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive analysis of X-ray. The measurements of resistivity were made using a classical four probe method and DC current. The magnetic field was applied with a constant amplitude of 0 T, 1 T, 2 T and 3 T. The obtained results show that the activation energy decreases with introduction of yttrium, but has a relative maximum when x is equal 0.1. The decrease of the activation energy is explained by the granular nature of the samples which promotes 3D transition to 2D of the vortex lattice.
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