Preparation and characterization of PNIPAAm-b-PLA/Fe3O4 thermo-responsive and magnetic composite micelles

Novel magnetic micelles with the flowerlike morphology were prepared with Fe₃O₄ nanoparticles and poly(N-isopropylacrylamide)-block-polylactide (PNIPAAm-b-PLA) copolymers by a dialysis method. The diameter of flowerlike micelles was about 1 μm. The core and shell of the micelles were hydrophilic, while the other area of the micelles was hydrophobic. The lower critical solution temperature (LCST) of PNIPAAm-b-PLA was about 38 °C. The magnetic intensity of Fe₃O₄ nanoparticles decreased after they were encapsulated into PNIPAAm-b-PLA micelles. Thermo-responsive and magnetic properties of the micelles would provide useful applications in the target drug delivery and release system.     

Development of thermosensitive poly(n-isopropylacrylamide-co-((2-dimethylamino) ethyl methacrylate))-based nanoparticles for controlled drug release

Thermosensitive nanoparticles based on poly(N-isopropylacrylamide-co-((2-dimethylamino)ethylmethacrylate)) (poly(NIPA-co-DMAEMA)) copolymers were successfully fabricated by free radical polymerization. The lower critical solution temperature (LCST) of the synthesized nanoparticles was 41?°C and a temperature above which would cause the nanoparticles to undergo a volume phase transition from 140 to 100 nm, which could result in the expulsion of encapsulated drugs. Therefore, we used the poly(NIPA-co-DMAEMA) nanoparticles as a carrier for the controlled release of a hydrophobic anticancer agent, 7-ethyl-10-hydroxy-camptothecin (SN-38). The encapsulation efficiency and loading content of SN-38-loaded nanoparticles at an SN-38/poly(NIPA-co-DMAEMA) ratio of 1/10 (D/P = 1/10) were about 80% and 6.293%, respectively. Moreover, the release profile of SN-38-loaded nanoparticles revealed that the release rate at 42?°C (above LCST) was higher than that at 37?°C (below LCST), which demonstrated that the release of SN-38 could be controlled by increasing the temperature. The cytotoxicity of the SN-38-loaded poly(NIPA-co-DMAEMA) nanoparticles was investigated in human colon cancer cells (HT-29) to compare with the treatment of an anticancer drug, Irinotecan(?) (CPT-11). The antitumor efficacy evaluated in a C26 murine colon tumor model showed that the SN-38-loaded nanoparticles in combination with hyperthermia therapy efficiently suppressed tumor growth. The results indicate that these thermo-responsive nanoparticles are potential carriers for controlled drug delivery.     

Low temperature magnetic hardening in self-assembled FePt/Ag core-shell nanoparticles

The FePt/Ag core-shell nanoparticles with different Ag shell thickness have been fabricated using a seed mediated technique. The core-shell nanoparticles are annealed at temperatures ranging from 350 to 600 °C for 30 min in vacuum. The magnetic measurement demonstrates that the FePt/Ag core-shell nanoparticles show a better chemical ordering tendency with a magnetic hardening temperature of 400–450 °C, which is almost 100 °C lower than that of pure FePt nanoparticles. Negative peaks on the δM curves of the annealed FePt/Ag core-shell nanoparticles demonstrate that the predominant interparticle interactions are dipolar type rather than exchange coupling one. Besides, the FePt/Ag core-shell nanoparticles show both sensitive plasmonic and superparamagnetic properties. The present results indicate that our composite nanoparticles are very promising from the viewpoint of the optoelectronics and biomedical applications.     

Ferroelectric properties of Bi3.4Dy0.6Ti3O12 thin films crystallized in N2

Bi_3.4Dy_0.6Ti₃O₁₂ (BDT) ferroelectric thin films were deposited on Pt/Ti/SiO2/Si substrates by chemical solution deposition (CSD) and annealed in an N₂ environment after pre-annealing in air at 400 °C. The effect of crystallization temperature on the structural and electrical properties of the BDT films was studied. The BDT films annealed in N₂ in the temperature range of 600 °C to 750 °C were crystallized well and the average grain size increased with increasing crystallization temperature, while the remanent polarization of the films is not a monotonic function of the crystallization temperature. The BDT films crystallized at 650 °C have the largest remanent polarization value of 2P_r = 39.4 μC/cm², and a fatigue-free characteristic.     

Epitaxial growth of Fe3Si/CaF2/Fe3Si magnetic tunnel junction structures on CaF2/Si(111) by molecular beam epitaxy

The Fe₃Si(24 nm)/CaF₂(2 nm)/Fe₃Si(12 nm) magnetic tunnel junction (MTJ) structures were grown epitaxially on CaF₂/Si(111) by molecular beam epitaxy (MBE). The 12-nm-thick Fe₃Si underlayer was grown epitaxially on CaF_2/Si(111) at approximately 400 °C; however, the surface of the Fe₃Si film was very rough, and thus a lot of pinholes are considered to exist in the 2-nm-thick CaF₂ barrier layer. The average roughness (Ra) of the CaF₂ barrier layer was 7.8 nm. This problem was overcome by low-temperature deposition of Fe and Si at 80 °C on CaF₂/Si(111), followed by annealing at 250 °C for 30 min to form the Fe₃Si layer. The Ra roughness was significantly reduced down to approximately 0.26 nm. A hysteresis loop with coercive field H_c of approximately 25 Oe was obtained in the magnetic field dependence of Kerr rotation at room temperature (RT).     

Temperature dependence of magnetic property and photocatalytic activity of Fe3O4/hydroxyapatite nanoparticles

Fe₃O₄/hydroxyapatite (HAP) nanoparticles have been developed as a novel photocatalyst support, based on the embedment of magnetic Fe₃O₄ particles into HAP shell via homogeneous precipitation method. The resultant nanoparticles were characterized by transmission electron microscope (TEM) and X-ray diffraction (XRD). These particles were almost spherical in shape, rather monodisperse and have a unique size of about 25 nm in diameter. The effect of calcination temperature on magnetic property and photocatalytic activity of Fe₃O₄/HAP nanoparticles was investigated in detail. The obtained results showed that the Fe₃O₄/HAP nanoparticles calcined at 400 °C possessed good magnetism and photocatalytic activity in comparison with that calcined at other temperatures.     

A facile route to synthesis of superparamagnetic Fe3O4–PDVB nanoworms

Fe₃O₄–polydivinylbenzene (PDVB) nanoworms were firstly synthesized by precipitation polymerization of divinylbenzene in the presence of oleic acid coated iron oxide nanoparticles. The nanoworms had superparamagnetic properties at room temperature, but ferromagnetism at 5 K. Thermogravimetric analysis curves indicated that in comparison with magnetic nanoparticles, the weight percent of iron oxide in nanoworms was slightly declined due to the formation of Fe₃O₄–PDVB nanocomposites. The superparamagnetic nanoworms could be well dispersed in ethanol, and were capable of easy separation by an external magnetic field. Overall, this provided a valuable methodology for preparation of elongated magnetic nanoparticles with high surface-to-volume ratio, which had potential applications in drug delivery/targeting, magnetic resonance imaging, and nanoprobes for diagnosis and disease treatment.     

Fluorescent multi-responsive cross-linked P(N-isopropylacrylamide)-based nanocomposites for cisplatin delivery

Magnetic, pH and temperature-sensitive, poly(N-isopropylacrylamide) (PNIPAM)-based nanocomposites with fluorescent properties were synthesized by free radical copolymerization-cross linking of NIPAM, N,N-dimethylaminoethyl methacrylate (DMAEMA) and 4-acrylamidofluorescein (AFA). The model anti-cancer drug, cisplatin (CDDP), was loaded into the resulted nanogel. For the production of CDDP-loaded nanocomposite, Fe₃O₄ magnetic nanoparticles (MNPs) and CDDP were loaded into the nanogel. Field-emission scanning electron microscopy (FE-SEM) indicated that the size of nanogel and CDDP-loaded nanocomposite were about 90 and 160?nm, respectively. The encapsulation efficiency of CCDP was found up to 65%. The loaded CCDP showed sustained thermal and pH-responsive drug release. A high level of drug release was observed under the conditions of low pH and high temperature. The lower critical solution temperature (LCST) of synthesized nanogel was about 40?°C. CDDP-loaded nanocomposite showed a volume phase transition from 282 to 128?nm at its LCST. Accordingly, in this study, the synthesized nanocomposite can be employed as a stimuli-responsive anti-cancer drug delivery system and the pH and temperature of solution have the potential to monitor the drug release.     

Preparation of La1−xSrxMnO3 nanoparticles by sonication-assisted coprecipitation

La_1−xSr_xMnO₃ (x=0.3) (LSM) nanoparticles were prepared by a sonication-assisted coprecipitation method. The coprecipitation reaction is carried out with ultrasound radiation. Lower sintering temperatures are required for the sonication-assisted product. Fully crystallized LSM with an average particle size 24 nm is obtained after the as-prepared mixture is annealed at 900 °C for 2 h. Magnetic properties indicate that the transition temperature from the paramagnetic to ferromagnetic state of the sample is quite sharp and occurs at 366 K for samples annealed for 2 h at 900 and 1100 °C.     

Low-temperature synthesis of BiFeO3 nanoparticles by ethylenediaminetetraacetic acid complexing sol-gel process

This paper reported a novel approach to synthesize pure BiFeO₃ nanoparticles through an ethylenediaminetetraacetic acid complexing sol-gel process at low temperature. The pure BiFeO₃ nanoparticles were attained at much lower temperature as 600 °C by this process, in contrast to above 800 °C for the traditional solid-state sintering process. The SEM results showed that the prepared BiFeO₃ nanoparticles had a better homogeneity and fine grain morphology. The BiFeO₃ nanoparticles show a weak ferromagnetic order at room temperature, which is quite different from the linear M-H relationship in bulk BiFeO₃. The origin of the weak magnetic property in our samples should be attributed to the size-confinement effects of the BiFeO₃ nanostructures.     

Synthesis of nanocrystalline xCuFe2O4-(1 − x)BiFeO3 magnetoelectric composite by chemical method

xCuFe₂O₄-(1 − x)BiFeO₃ spinel-perovskite nanocomposites with x = 0.1, 0.2, 0.3 and 0.4 were prepared using citrate precursor method. X-ray diffraction (XRD) analysis showed phase formation of xCuFe₂O₄-(1 − x)BiFeO₃ calcined at 500 °C. Transmission electron microscopy (TEM) shows formation of nanocrystallites of xCuFe₂O₄-(1 − x)BiFeO₃ with an average particle size of 40 nm. Variation of dielectric constant and dielectric loss with frequency showed dispersion in the low frequency range. Coercivity, saturation magnetization and squareness have been found to vary with concentration of ferrite phase and annealing temperature due to the increase in crystallite size. Squareness and coercivity increased with an increase in annealing temperature up to 500 °C and then decreased with a further increase in temperature to 600 °C. Magnetoelectric effect of the nanocomposites was found to be strongly depending on the magnetic bias and magnetic field frequency.     

Doxorubicin loaded PVA coated iron oxide nanoparticles for targeted drug delivery

Magnetic drug targeting is a drug delivery system that can be used in locoregional cancer treatment. Coated magnetic particles, called carriers, are very useful for delivering chemotherapeutic drugs. Magnetic carriers were synthesized by coprecipitation of iron oxide followed by coating with polyvinyl alcohol (PVA). Characterization was carried out using X-ray diffraction, TEM, TGA, FTIR and VSM techniques. The magnetic core of the carriers was magnetite (Fe₃O₄), with average size of 10 nm. The room temperature VSM measurements showed that magnetic particles were superparamagnetic. The amount of PVA bound to the iron oxide nanoparticles were estimated by thermogravimetric analysis (TGA) and the attachment of PVA to the iron oxide nanoparticles was confirmed by FTIR analysis. Doxorubicin (DOX) drug loading and release profiles of PVA coated iron oxide nanoparticles showed that up to 45% of adsorbed drug was released in 80 h, the drug release followed the Fickian diffusion-controlled process. The binding of DOX to the PVA was confirmed by FTIR analysis. The present findings show that DOX loaded PVA coated iron oxide nanoparticles are promising for magnetically targeted drug delivery.     

Dark-red-emitting CdTe0.5Se0.5/Cd0.5Zn0.5S quantum dots: Effect of chemicals on properties

CdTe_0.5Se_0.5/Cd_0.5Zn_0.5S core/shell quantum dots (QDs) with a tunable photoluminescence (PL) range from yellow to dark red (up to a PL peak wavelength of 683 nm) were fabricated using various reaction systems. The core/shell QDs created in the reaction solution of trioctylamine (TOA) and oleic acid (OA) at 300 °C exhibited narrow PL spectra and a related low PL efficiency (38%). In contrast, the core/shell QDs prepared in the solution of 1-octadecene (ODE) and hexadecylamine (HDA) at 200 °C revealed a high PL efficiency (70%) and broad PL spectra. This phenomenon is ascribed that the precursor of Cd, reaction temperature, solvents, and ligands affected the formation process of the shell. The slow growth rate of the shell in the solution of ODE and HDA made QDs with a high PL efficiency. Metal acetate salts without reaction with HDA led to the core/shell QDs with a broad size distribution.     

Structural and optical studies of nanocrystalline V2O5 thin films

We report the structural and optical properties of nanocrystalline thin films of vanadium oxide prepared via evaporation technique on amorphous glass substrates. The crystallinity of the films was studied using X-ray diffraction and surface morphology of the films was studied using scanning electron microscopy and atomic force microscopy. Deposition temperature was found to have a great impact on the optical and structural properties of these films. The films deposited at room temperature show homogeneous, uniform and smooth texture but were amorphous in nature. These films remain amorphous even after postannealing at 300 °C. On the other hand the films deposited at substrate temperature T_S > 200 °C were well textured and c-axis oriented with good crystalline properties. Moreover colour of the films changes from pale yellow to light brown to black corresponding to deposition at room temperature, 300 °C and 500 °C respectively. The investigation revealed that nanocrystalline V₂O₅ films with preferred 001 orientation and with crystalline size of 17.67 nm can be grown with a layered structure onto amorphous glass substrates at temperature as low as 300 °C. The photograph of V₂O₅ films deposited at room temperature taken by scanning electron microscopy shows regular dot like features of nm size.     

Effect of glass fillers in Cu2ZnNb2O8 ceramics for advanced microwave applications

The effect of glass addition on sintering temperature and microwave dielectric properties of Cu₂ZnNb₂O₈ (CZN) is investigated for possible low temperature co-fired ceramic (LTCC) application. The CZN ceramic was prepared by the solid-state ceramic route. The phase formation, microstructure and elemental composition of the ceramics were studied using X-Ray Diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy and Energy Dispersive Analysis. The CZN sintered at 975 °C/4 h has ?_r = 15.2, tan δ = 0.0007 (at 5.1 GHz) and τ_f of −98 ppm °C⁻¹ and CTE = 1.9 ppm °C⁻¹. The addition of LBS and LMZBS glasses lowered the sintering temperature of CZN to below the melting point of silver. The 1 wt% LBS added CZN sintered at 935 °C/4 h had ?_r = 14.7, tan δ = 0.001 (at 5.1 GHz), τ_f = −19 ppm °C⁻¹ and CTE = −0.6 ppm °C⁻¹. The addition of 0.7 wt% LMZBS to CZN and sintered at 935 °C/4 h had ?_r = 14.8, tan δ = 0.002 (at 5.1 GHz), τ_f = −39 ppm °C⁻¹ and CTE = −0.9 ppm °C⁻¹.     

Temperature dependent Raman scattering of the epitaxial Sr1.9Ca0.1NaNb5O15 film

Epitaxial ferroelectric Sr_1.9Ca_0.1NaNb₅O₁₅ (SCNN) thin films have been fabricated successfully by pulsed laser deposition on (100)MgO substrates. Temperature dependency of the vibrational modes of these films was investigated for the first time using Raman scattering technique. For temperatures ranging between 50 °C and 450 °C, two strong and broad A₁(TO) phonons around 238 and 608 cm^− 1, and one weak B₁(TO) phonon around 142 cm^− 1 were observed. Changes in the temperature dependency of the peak position, the full-width at half maximum and integrated intensity of the Raman modes were observed in different temperature ranges. These changes are attributed to the structural phase transitions between 200 °C and 325 °C for the SCNN films as well as their relaxor properties.     

Deposition of WNxCy thin films for diffusion barrier application using the dimethylhydrazido (2) tungsten complex (CH3CN)Cl4W(NNMe2)

Tungsten nitride carbide (WN_xC_y) thin films were deposited by chemical vapor deposition using the dimethylhydrazido (2⁻) tungsten complex (CH₃CN)Cl₄W(NNMe₂) (1) in benzonitrile with H₂ as a co-reactant in the temperature range 300 to 700 °C. Films were characterized using X-ray diffraction (XRD), Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy and four-point probe to determine film crystallinity, composition, atomic bonding, and electrical resistivity, respectively. The lowest temperature at which growth was observed from 1 was 300 °C. For deposition between 300 and 650 °C, AES measurements indicated the presence of W, C, N, and O in the deposited film. The films deposited below 550 °C were amorphous, while those deposited at and above 550 °C were nano-crystalline (average grain size < 70 Å). The films exhibited their lowest resistivity of 840 µΩ-cm for deposition at 300 °C. WN_xC_y films were tested for diffusion barrier quality by sputter coating the film with Cu, annealing the Cu/WN_xC_y/Si stack in vacuum, and performing AES depth profile and XRD measurement to detect evidence of copper diffusion. Films deposited at 350 and 400 °C (50 and 60 nm thickness, respectively) were able to prevent bulk Cu transport after vacuum annealing at 500 °C for 30 min.     

Reactive magnetron sputtering of Inconel 690 by Ar-N2 plasma

M and M-N coatings, where M is nearly the metal composition of Inconel 690 (57 at.% Ni, 32 at.% Cr, 9.5 at.% Fe…) were sputter-deposited on glass and steel substrates in pure argon and in Ar-N₂ mixtures using a round planar magnetron. The influence of nitrogen gas flow rate inlet in argon on chemical composition and microstructure was studied. The as-deposited (T < 100 °C) M-N films containing up to 30 at.% nitrogen are a nanocrystalline supersaturated face cubic centered (fcc) solid solution (γ_N). The pure metallic films have a pronounced<111>fcc crystallographic texture, while the M-N films exhibit a strong<100>fcc crystallographic texture. The effect of temperature on the microstructure of M-N films was studied by increasing the substrate temperature during preparation and by tempering of an as-deposited M-N films. For M-N films prepared at 400 °C, the X-ray diffraction analysis reveals a magnetic γ phase with a very low nitrogen content, while electron probe microanalysis gives an overall high nitrogen content in the layer (up to 25 at.%). It is concluded that the layers consist of two phases when prepared or tempered at high temperature (T > 400 °C): an fcc CrN nitride and a γ (Ni,Fe,Cr) depleted in nitrogen.     

Stability and effect of annealing on the optical properties of plasma-deposited Ta2O5 and Nb2O5 films

Tantalum and niobium oxide optical thin films were prepared at room temperature by plasma-enhanced chemical vapor deposition using tantalum and niobium pentaethoxide (M(OC₂H₅)₅) precursors. We studied the evolution of their optical and microstructural properties as a result of annealing over a broad temperature range from room temperature up to 900 °C. The as-deposited films were amorphous; their refractive index, n, and extinction coefficient, k, at 550 nm were n = 2.13 and k < 10^− 4 for Ta₂O₅, and n = 2.24 and k < 10^− 4 for Nb₂O₅. The films contained a small amount of residual carbon (∼ 2-6 at.%) bonded mostly to oxygen. During annealing, the onset of crystallization was observed at approximately T_C1 = 650 °C for Ta₂O₅ and at T_C1 = 450 °C for Nb₂O₅. Upon annealing close to T₁ (300 °C for Nb₂O₅ and 400 °C for Ta₂O₅), n at 550 nm decreased by less than 1%. This was correlated with the decrease of carbon content, as suggested by Fourier transform infrared spectroscopy, elastic recoil detection and static secondary ion mass spectroscopy (SIMS) results. During annealing, we observed phase transition from the δ- (hexagonal) phase to the L- (orthorhombic) phase between 800 °C and 900 °C for Ta₂O₅, and between 600 °C and 700 °C for Nb₂O₅. The structural changes were also marked by silicon diffusion from the substrate into the oxide layer at annealing temperatures above 500 °C for Ta₂O₅ and above 400 °C for Nb₂O₅. As a consequence of oxygen, silicon and metal interdiffusion, the interface between the Si substrate and the metal oxide (Ta₂O₅ or Nb₂O₅) is characterized by its broadening, well documented by spectroscopic ellipsometry and SIMS data.     

Room temperature ferromagnetism in Zn0.99La0.01O and pure ZnO nanoparticles

Room temperature ferromagnetism (RTFM) was observed in both La-doped and pure ZnO nanoparticles synthesized by the sol–gel method. RTFM is intrinsic according to the results of X-ray diffraction and X-ray photoelectron spectroscopy. The saturation magnetization (M_S), the remnant magnetization at zero field and coercive field are 5 × 10⁻³, 7 × 10⁻⁴ emu g⁻¹, 100 Oe for Zn_0.99La_0.01O nanoparticles and 1.5 × 10⁻⁴, 1 × 10⁻⁵ emu g⁻¹, 50 Oe for pure ZnO nanoparticles, respectively. The magnetization is enhanced greatly by doping of La. Furthermore, the M_S of Zn_0.99La_0.01O nanoparticles decreases from 0.005 to 0.001 emu g⁻¹ as the annealing temperature increases from 500 to 700 °C. The doping of La introduces more oxygen vacancies into ZnO. The decrease of annealing temperature also produces more oxygen vacancies in La-doped ZnO. These results indicate that the origin of the RTFM is related to oxygen vacancies.