Preparation of strontium hexaferrite film by pulsed laser deposition with in situ heating and post annealing

Strontium hexaferrite (SrFe₁₂O₁₉) films have been fabricated by pulsed laser deposition on Si(1 0 0) substrate with Pt(1 1 1) underlayer through in situ and post annealing heat treatments. C-axis perpendicular oriented SrFe₁₂O₁₉ films have been confirmed by X-ray diffraction patterns for both of the in situ heated and post annealed films. The cluster-like single domain structures are recognized by magnetic force microscopy. Higher coercivity in perpendicular direction than that for the in-plane direction shows that the films have perpendicular magnetic anisotropy. High perpendicular coercivity, around 3.8 kOe, has been achieved after post annealing at 500 °C. Higher coercivity of the post annealed SrFe₁₂O₁₉ films was found to be related to nanosized grain of about 50–80 nm.     

Development of a magnetic system for the treatment of Helicobacter pylori infections

We report a study to develop a magnetic system for local delivery of amoxicillin. Magnetite microparticles produced by coprecipitation were coated with a solution of amoxicillin and Eudragit^®S100 by spray drying. Scanning electron microscopy, optical microscopy, X-ray powder diffraction and vibrating sample magnetometry revealed that the particles were superparamagnetic, with an average diameter of 17.2 μm, and an initial susceptibility controllable by the magnetite content in the suspension feeding the sprayer. Our results suggest a possible way to treat Helicobacter pylori infections, using an oral drug delivery system, and open prospects to coat magnetic microparticles by spray drying for biomedical applications.     

Low-temperature growth of polycrystalline Ge thin film on glass by in situ deposition and ex situ solid-phase crystallization for photovoltaic applications

Poly-crystalline germanium (poly-Ge) thin films have potential for lowering the manufacturing cost of photovoltaic devices especially in tandem solar cells, but high crystalline quality would be required. This work investigates the crystallinity of sputtered Ge thin films on glass prepared by in situ growth and ex situ solid-phase crystallization (SPC). Structural properties of the films were characterized by Raman, X-ray diffraction and ultraviolet-visible reflectance measurements. The results show the transition temperature from amorphous to polycrystalline is between 255 °C and 280 °C for in situ grown poly-Ge films, whereas the transition temperature is between 400 °C and 500 °C for films produced by SPC for a 20 h annealing time. The in situ growth in situ crystallized poly-Ge films at 450 °C exhibit significantly better crystalline quality than those formed by solid-phase crystallization at 600 °C. High crystalline quality at low substrate temperature obtained in this work suggests the poly-Ge films could be promising for use in thin film solar cells on glass.     

Highly sensitive room-temperature method of non-invasive in vivo detection of magnetic nanoparticles

Methods of non-invasive in vivo quantification of magnetic nanoparticles (MP) have been proposed and realized. The methods are based on non-linear MP magnetization at two frequencies and measuring the response at combinatorial frequencies. The first method is developed for real-time study of MP dynamics and their clearance from the blood system of animals. High sensitivity of 3 ng of Fe₃O₄ in 0.1 ml was achieved for MP detection in mice tail veins. The second technique is proposed for MP detection inside animal tissues by an external probe. The proposed methods could essentially widen capabilities of biomedical research which involves magnetic nanoparticles.     

Characterization of ultrasound-mediated destruction of drug-loaded microbubbles using an improved in vitro model

Introduction

Ultrasound mediated destruction of microbubbles (MBs) has become a promising tool for site specific drug and gene delivery. One of the most important properties of drug-loaded MBs is their destructibility by ultrasound. Therefore, the aim of this study was to establish a new in vitro model that allows evaluation of the kinetics of ultrasound-mediated MB destruction at near physiological conditions.In this work, a newly developed drug-loaded MB formulation was compared with unloaded MBs in order to assess the influence of drug-loading on their acoustic destructibility. Furthermore, drug-loaded MBs were compared to acoustically active lipospheres (AALs), comprising an additional layer of triacetin, as well as to a marketed MB contrast agent (SonoVue^®, Bracco Diagnostics, USA), used as standard.

Methods

MBs with phospholipid monolayer shells were produced by mechanical agitation of liposomal dispersions and octafluoropropane gas. AALs were accordingly produced by agitation of phospholipid-stabilized aqueous triacetin microemulsions with gas.The in vitro experimental setup for acoustic destructibility testing comprised a membrane cell, pressurized and brought to 37 °C in order to imitate human blood pressure and body temperature. The optimized egg-like cell shape provided optimal flow conditions and a minimized dead volume.Ultrasound with frequencies of 1 and 3 MHz and intensities, varying from 1 to 4 W/cm², was applied through a silicone membrane window to the cell. MB size distribution and concentration were measured by light blockage in equal time intervals during the sonication.

Results

The optimized in vitro setup demonstrated differences in the ultrasound destructibility of the MB formulations used. The fastest decay upon ultrasound exposure was found for SonoVue^®. Unloaded and drug-loaded MBs appeared to be comparably destructible to SonoVue^®. AALs were about 4.5-fold more stable than SonoVue^®. MB destructibility was also found to depend on particle diameter, corresponding to theoretical models described in the literature.

Conclusion

The optimized in vitro setup has rendered a fast and reliable laboratory tool for characterization of MB formulations.     

Laser reflectometry in situ monitoring of InGaAs grown by atmospheric pressure metalorganic vapour phase epitaxy

InGaAs layers on undoped GaAs (0 0 1) substrates were grown by atmospheric pressure metalorganic vapour phase epitaxy (AP-MOVPE). In order to obtain films with different indium composition (x_In), the growth temperature as a growth parameter, was varied from 420 to 680 °C. Furthermore, high-resolution X-ray diffraction (HRXRD) measurements were used to quantify the change of x_In. Crystal quality has been also studied as a function of growth conditions. On the other hand, laser reflectometry (LR) at 632.8 nm wavelength, was employed to in situ monitor epitaxy. Reflectivity-time signal was enabled to evaluate structural and optical properties of samples. We have fitted experimental data to determine optical constants and growth rate of InGaAs at 632.8 nm. In addition, the fitting provided InGaAs thickness as a function of growth time. Based on ex situ characterization by scanning electronic microscopy (SEM) and HRXRD, we propose a practical method, relating the contrast of first reflectivity maximum with the X-ray diffraction peak angular difference between the substrate and epitaxial layer, to determine in situ the In solid composition in InGaAs alloys.     

Effect of C and SiC additions into in situ or mechanically alloyed MgB2 deformed in Ti sheath

Effect of 3.4 wt.% C and 5 wt.% SiC doping into the standard in situ (IN) process and mechanically alloyed (MA) MgB₂ was studied. Powders of IN and MA process were carried out in air and in argon filled glove box, respectively. Wire samples were prepared by two-axial rolling deformation of IN and MA powders inside the Ti tube. Titanium as sheath material allows to use higher sintering temperatures, we used 700 °C and 800 °C for 30 min in Argon. Critical current densities (J_c) were measured at variable temperatures 4.2 K, 10 K, 15 K and 20 K in the external magnetic fields ranging to 15 T. Critical temperatures, upper critical fields and irreversibility fields of IN and MA with SiC and C additions are compared and discussed. The highest transport properties were observed for wires with MA SiC doped MgB₂ in the whole scale of temperatures 4.2–20 K. Upper critical field was rapidly enhanced in the case of carbon doped MA samples at 4.2 K. MA samples have shown decreased J_c values for higher temperatures (15 K, 20 K), in some case even worse than for the not doped reference IN sample. Carbon substitution and grain connectivity of analyzed samples are compared and discussed. Presented results show that for 20 K applications some new ways (additions) have to be found for increasing the J_c substantially.     

Near room temperature magnetocaloric properties of melt-spun Gd100−xBx (x=0, 5, 10, 15, and 20 at%) alloys

The magnetocaloric properties of melt-spun Gd-B alloys were examined with the aim to explore their potential application as magnetic refrigerants near room temperature. A series of Gd_100−xB_x (x=0, 5, 10, 15, and 20 at%) alloys were prepared by melt spinning. With the decrease in Gd/B ratio, Curie temperature (T_C) remains constant at ∼293 K, and saturation magnetization, at 275 K, decreases from ∼100 to ∼78 emu/g. Negligible magnetic hysteresis was observed in these alloys. The peak value of magnetic entropy change, (−ΔS_M)_max, decreased from ∼9.9 J/kg K (0-5 T) and ∼5.5 J/kg K (0-2 T) for melt-spun Gd to ∼7.7 J/kg K (0-5 T) and ∼4.0 J/kg K (0-2 T), respectively for melt-spun Gd₈₅B₁₅ and Gd₈₀B₂₀ alloys. Similarly, the refrigeration capacity (q) decreased monotonously from ∼430 J/kg (0-5 T) for melt-spun Gd to ∼330 J/kg (0-5 T) for melt-spun Gd₈₀B₂₀ alloy. The near room temperature magnetocaloric properties of melt-spun Gd_100−xB_x (0≤x≤20) alloys were found to be comparable to few first-order transition based magnetic refrigerants.     

In situ growth stresses during the phase separation of immiscible FeCu thin films

This paper addresses the in situ growth stress evolution and post-growth stress relaxation during the phase separation of immiscible Fe_0.51Cu_0.49 thin films at various in situ deposition temperatures. Each film was sputter-deposited onto a 10 nm Si₃N₄ underlayer that was grown on top of Si [0 0 1] substrate at 25 °C, 145 °C, 205 °C, 265 °C or 325 °C. The thin film stress was measured using a wafer curvature technique. The in situ growth stress increased in compression with increasing substrate temperature. The stress relaxation of the Fe_0.51Cu_0.49 was found to have a linear increase with the inverse grain size for films deposited at temperatures greater than 205 °C. The stress state was correlated to the films’ phase and morphology by X-ray diffraction, (scanning) transmission electron microscopy and atomic force microscopy techniques.     

Structural phase transitions in Au thin films on Si (1 1 0): An in situ temperature dependent transmission electron microscopy study

We present a review on the formation of gold silicide nanostructures using in situ temperature dependent transmission electron microscopy (TEM) measurements. Thin Au films of two thicknesses (2.0 nm and 5.0 nm) were deposited on Si (1 1 0) substrate under ultra-high vacuum (UHV) conditions in a molecular beam epitaxy (MBE) system. Also a 2.0 nm thick Au film was deposited under high vacuum condition (with the native oxide at the interface of Au and Si) using thermal evaporation. In situ TEM measurements (for planar samples) were made at various temperatures (from room temperature, RT to 950 °C). We show that, in the presence of native oxide (UHV-MBE) at the interface, high aspect ratio (≈15.0) aligned gold silicide nanorods were observed. For the films that were grown with UHV conditions, a small aspect ratio (∼1.38) nanogold silicide was observed. For 5.0 nm thick gold thin film, thicker and lesser aspect ratio silicides were observed. Selected area diffraction pattern taken at RT after the sample for the case of 5.0 nm Au on Si (1 1 0)-MBE was annealed at 475 °C show the signature of gold silicide formation.     

Invert sugar formation with Saccharomyces cerevisiae cells encapsulated in magnetically responsive alginate microparticles

Invert sugar (an equimolar mixture of glucose and fructose prepared by sucrose hydrolysis) is a very important food component. We have prepared magnetically responsive alginate microbeads containing entrapped Saccharomyces cerevisiae cells and magnetite microparticles which can be easily separated in an appropriate magnetic separator. The microbeads (typical diameter between 50 and 100 μm) were prepared using the water-in-oil emulsification process. The prepared microbeads containing yeast cells with invertase activity enabled efficient sucrose conversion. The biocatalyst was quite stable; the same catalytic activity was observed after one month storage at 4 °C and the microbeads could be used at least six times.     

Rapid sequential injections of hyperpolarized [1-C]pyruvate in vivo using a sub-kelvin,multi-sample DNP polarizer

The development of hyperpolarized technology utilizing dynamic nuclear polarization (DNP) has enabled the rapid measurement of ¹³C metabolism in vivo with very high SNR. However, with traditional DNP equipment, consecutive injections of a hyperpolarized compound in an animal have been subject to a practical minimum time between injections governed by the polarization build-up time, which is on the order of an hour for [1-¹³C]pyruvate. This has precluded the monitoring of metabolic changes occurring on a faster time scale. In this study, we demonstrated the ability to acquire in vivo dynamic magnetic resonance spectroscopy (MRS) and 3D magnetic resonance spectroscopic imaging (MRSI) data in normal rats with a 5 min interval between injections of hyperpolarized [1-¹³C]pyruvate using a prototype, sub-Kelvin dynamic nuclear polarizer with the capability to simultaneously polarize up to 4 samples and dissolve them in rapid succession. There were minimal perturbations in the hyperpolarized spectra as a result of the multiple injections, suggesting that such an approach would not confound the investigation of metabolism occurring on this time scale. As an initial demonstration of the application of this technology and approach for monitoring rapid changes in metabolism as a result of a physiological intervention, we investigated the pharmacodynamics of the anti-cancer agent dichloroacetate (DCA), collecting hyperpolarized data before administration of DCA, 1 min after administration, and 6 min after administration. Dramatic increases in ¹³C-bicarbonate were detected just 1 min (as well as 6 min) after DCA administration.     

Chemomechanical properties and microstructural stability of nanocrystalline Pr-doped ceria: An in situ X-ray diffraction investigation

The chemomechanical properties and microstructural stability of nanocrystalline Pr_xCe_1 − xO_2 − δ solid solutions are studied as a function of temperature by in situ X-ray diffraction measurements under oxidizing conditions at P(O₂) ~ 200 mbar. The chemical expansion coefficient of nanocrystalline powder specimens, operative at intermediate temperatures during which Pr⁴⁺ is reduced to Pr³⁺, is found to be similar to that obtained for coarse-grained Pr_xCe_1 − xO_2 − δ. This is contrary to reports regarding variation of physical and chemical properties with crystallite size. The thermal expansion coefficient, measured under conditions for which Pr_xCe_1 − xO_2 − δ is highly oxygen deficient, was found to be greater than that measured for fully oxidized Pr_xCe_1 − xO_2 − δ, with potential sources of these changes discussed. Moreover, the microstructure of nanocrystalline Pr_xCe_1 − xO_2 − δ is observed to have excellent stability at working temperatures below 800 °C, enabled by the inherent microstrain in the structure, highlighting the potential application of this material for solid state electrochemical devices.     

FePt L10 ordering and grain growth using millisecond pulse laser processing

The structural and magnetic properties of ∼12 nm thick FePt thin films grown on Si substrates annealed using a 1064 nm wavelength laser with a 10 ms pulse have been examined. The A1 to L1₀ ordering phase transformation was confirmed by electron and X-ray diffraction. An order parameter near 50% and a maximum coercivity of 12 kOe were obtained with laser energy densities of 25-32 J/cm². Grain growth, quantified by dark field transmission electron microscopy, occurred during chemical ordering at the laser pulse widths studied.     

Preparation, characterization and in vitro cytotoxicity of BSA-based nanospheres containing nanosized magnetic particles and/or photosensitizer

This study reports on the preparation, characterization and in vitro toxicity test of a new nano-drug delivery system (NDDS) based on bovine serum albumin (BSA) nanospheres which incorporates surface-functionalized magnetic nanoparticles (MNP) and/or the silicon(IV) phthalocyanine (NzPc). The new NDDS was engineered for use in photodynamic therapy (PDT) combined with hyperthermia (HPT) to address cancer treatment. The BSA-based nanospheres, hosting NzPc, MNP or both (NzPc and MNP), present spherical shape with hydrodynamic average diameter values ranging from 170 to 450 nm and zeta potential of around −23 mV. No difference on the fluorescence spectrum of the encapsulated NzPc was found regardless of the presence of MNP. Time-dependent fluorescence measurements of the encapsulated NzPc revealed a bi-exponential decay for samples incorporating only NzPc and NzPc plus MNP, in the time window ranging from 1.70 to 5.20 ns. The in vitro assay, using human fibroblasts, revealed no cytotoxic effect in all samples investigated, demonstrating the potential of the tested system as a synergistic NDDS.     

High-k Mg-doped ZST for microwave applications

The (Zr_0.8Sn_0.2)TiO₄ material (ZST), has been prepared by solid state reaction and characterized. The samples were sintered in the temperature range of 1260-1320 °C for 2 h. The effects of sintering parameters like sintering temperature (T_s) and MgO addition (0.2 wt.%) on structural and dielectric properties were investigated. Bulk density increases from 4900 to 5050 kg/m³ with the increase of sintering temperature. The effect of MgO addition is to lower the sintering temperature in order to obtain well sintered samples with high value of bulk density. The material exhibits a dielectric constant ?_r ∼ 37 and high values of the Q × f product, greater than 45,000, at microwave frequencies. The dielectric properties make the ZST material very attractive for microwave applications such as dielectric resonators, filters, dielectric antennas, substrates for hybrid microwave integrated circuits, etc.     

Investigations of the interactions of CO2, O3 and UV light with silver surfaces by in situ IRRAS/QCM and ex situ TOF-SIMS

The characterization of the reactions occurring during the atmospheric corrosion of silver surfaces at the metal-atmosphere interface is of great importance as only the exact knowledge of the degradation mechanisms enables the development of suitable corrosion inhibiting steps. For in situ surface analysis three complementary experimental techniques have been combined in order to study the surface chemistry of silver samples exposed to humidified air, CO₂, ozone (O₃) and ultraviolet (UV) light. In situ infrared reflection absorption spectroscopy (IRRAS) combined with a quartz crystal microbalance (QCM) as well as ex situ time of flight secondary ion mass spectrometry (TOF-SIMS) provide an overall picture of the processes occurring at the metal-atmosphere interface. Investigations were carried out by exposing polycrystalline silver samples to synthetic air containing 50-90% relative humidity (RH) and 250 ppm CO₂. Additionally, the samples were exposed to UV light or O₃ for certain time periods. The formation of the main corrosion products on the sample surfaces, depending on the relative humidity, O₃ content and UV light exposure could be observed in a time resolved way. These investigations reveal the different reaction mechanisms and reaction rates occurring on a silver surface.     

Physical properties and anisotropies of the RNiGe3 series (R = Y, Ce-Nd, Sm, Gd-Lu)

We have studied RNiGe₃ (R=Y, Ce-Nd, Sm, Gd-Lu) single crystals by measuring crystal structure and stoichiometry, magnetic susceptibility, magnetization, electrical resistivity, magnetoresistance, and specific heat. Clear anisotropies as well as antiferromagnetic ordering in the RNiGe₃ series (R=Ce-Nd, Sm, Gd-Tm) have been observed above 1.8 K from the magnetic susceptibility. A metamagnetic transition in this family (except for R=Sm) was detected at 2 K for applied magnetic fields below 70 kOe. The electrical resistivity of this series follows metallic behavior in the high temperature region. Below the antiferromagnetic ordering temperature a significant anisotropy is exhibited in the resistivity and magnetoresistance for different current directions. The anisotropic magnetic, transport, and thermal properties of RNiGe₃ compounds are discussed in terms of Ni site occupancy as well as a combination of the effect of formation of a magnetic superzone gap and the crystalline electric field.     

Characterization of CdTe films with in situ CdCl2 treatment grown by a simple vapor phase deposition technique

A unique vapor phase deposition (VPD) technique was designed and built to achieve in situ CdCl₂ treatment of CdTe film. The substrate temperature was 400 °C, and the temperature of CdTe mixture with CdCl₂ source was 500 °C. The structural and morphological properties of CdTe have been studied as a function of wt.% CdCl₂ concentration by using X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM) and atomic force microscopy (AFM). XRD measurements show that the presence of CdCl₂ vapor induces (1 1 1)-oriented growth in the CdTe film. SEM measurements have shown enhance growth of grains, in the presence of CdCl₂. From AFM the roughness of the films showed a heavy dependence on CdCl₂ concentration. In the presence of 4% CdCl₂ concentration, the CdTe films roughness has a root mean square (rms) value of about 275 Å. This value is about 831 Å for the non-treated CdTe films.     

TDLAS-based in situ measurement of absolute acetylene concentrations in laminar 2D diffusion flames

We report the first quantitative and calibration-free in situ C₂H₂ measurement in a flame environment using direct Tunable Diode Laser Absorption Spectroscopy(TDLAS). Utilizing a fiber-coupled Distributed Feedback diode laser near 1535 nm we measured spatially resolved, absolute C₂H₂ concentration profiles in a laminar non-premixed CH₄/air flame supported on a modified Wolfhard-Parker slot burner with N₂ purge slots to minimize end flames. We developed a wavelength tuning scheme combining laser temperature and current modulation to record with a single diode laser a mesh of 37 overlapping spectral windows and generate an ∼7 nm (30 cm⁻¹) wide, high-resolution absorption spectrum centered at 1538 nm. Experimental C₂H₂ spectra in a reference cell showed excellent agreement with simulations using HITRAN2004 data. The enhanced wavelength coverage was needed to establish correct C₂H₂ line identification and selection in the very congested high temperature flame spectra and led to the P17e line as the only candidate for in situ detection of C₂H₂ in the flame. We used highly efficient optical disturbance correction algorithms for treating transmission and background emission fluctuations in combination with a multiple Voigt line Levenberg-Marquardt fitting algorithm and Pt/Rh thermocouple measurements to achieve fractional optical resolutions of up to 4 × 10⁻⁵ OD (1σ) in the flame (T up to 2000 K). Temperature dependent C₂H₂ detection limits for the P17e line were 60 to 480 ppm. By translating the burner through the laser beam with a DC motor we obtained spatially resolved, absolute C₂H₂ concentration profiles along the flame sheet with 0.5 mm spatial resolution as measured with a knife edge technique. The TDLAS-based, transverse C₂H₂ concentration profiles without any scaling are in excellent agreement with published mass spectrometric C₂H₂ data for the same flame supported on a similar burner, thus validating our calibration-free TDLAS measurements.