Sol-gel preparation and characterization of CoFe2O4-SiO2 nanocomposites

Magnetic nanocomposites formed by cobalt ferrite particles dispersed in a silica matrix were prepared by a sol-gel process. The effects of the thermal treatment temperature and the salt concentration on the structural and magnetic properties of the composites were investigated. By controlling these parameters, CoFe₂O₄/SiO₂ nanocomposites with different crystallite size and magnetic properties were obtained. By increasing the annealing temperature and salt concentration, composites with a progressive increase in the coercive field and of the density of magnetization were produced. In particular, a nanocomposite, with a Fe/Si molar concentration of 21%, obtained by drying the gel at 150 °C and further annealing at 800 °C, has a coercivity of 2000 Oe, which is more than twice higher than the coercivity of bulk cobalt ferrite.     

Study of reactions between HfO2 and Si in thin films with precise identification of chemical states by XPS

Reactions between HfO₂ and Si in HfSiO films during deposition and post-annealing have been studied. Intermixing of HfO₂ and Si is achieved by radio frequency sputtering with HfO₂/Si compound targets, and post-annealing is used to promote the reaction at different temperatures. The structural characteristics of the mixture, HfSiO films, are analyzed by X-ray photoelectron spectroscopy and X-ray diffraction, and a careful assessment of chemical states is performed for precise identification. XPS results show that with ratios of Si:Hf ranging from 0 to 0.3 in HfSiO films, Si fully reacts with HfO₂ to form silicate during deposition. However, SiO₂ appears when the ratio of Si:Hf rises to 1.2. When the annealing temperature reaches 600 °C, decomposition of hafnium silicate is observed and hafnium silicide forms in the bulk of the films. XRD results reveal that HfSiO films remain amorphous with the annealing temperature below 600 °C but crystallize at 800 °C.     

Microstructure and interfacial properties of HfO2-Al2O3 nanolaminate films

High-k HfO₂-Al₂O₃ composite gate dielectric thin films on Si(1 0 0) have been deposited by means of magnetron sputtering. The microstructure and interfacial characteristics of the HfO₂-Al₂O₃ films have been investigated by using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and spectroscopic ellipsometry (SE). Analysis by XRD has confirmed that an amorphous structure of the HfO₂-Al₂O₃ composite films is maintained up to an annealing temperature of 800 °C, which is much higher than that of pure HfO₂ thin films. FTIR characterization indicates that the growth of the interfacial SiO₂ layer is effectively suppressed when the annealing temperature is as low as 800 °C, which is also confirmed by spectroscopy ellipsometry measurement. These results clearly show that the crystallization temperature of the nanolaminate HfO₂-Al₂O₃ composite films has been increased compared to pure HfO₂ films. Al₂O₃ as a passivation barrier for HfO₂ high-k dielectrics prevents oxygen diffusion and the interfacial layer growth effectively.     

Enhanced emission of Er from alternately Er doped Si-rich Al2O3 multilayer film with Si nanocrystals as broadband sensitizers

Alternately Er doped Si-rich Al₂O₃ (Er:SRA) multilayer film, consisting of alternate Er-Si-codoped Al₂O₃ (Er:Si:Al₂O₃) and Si-doped Al₂O₃ (Si:Al₂O₃) sublayers, has been synthesized by co-sputtering from separated Er, Si, and Al₂O₃ targets. The dependence of Er³⁺ related photoluminescence (PL) properties on annealing temperatures over 700-1100 °C was studied. The maximum intensity of Er³⁺ PL, about 10 times higher than that of the monolayer film, was obtained from the multilayer film annealed at 950 °C. The enhancement of Er³⁺ PL intensity is attributed to the energy transfer from the silicon nanocrystals in the Si:Al₂O₃ sublayers to the neighboring Er³⁺ ions in the Er:Si:Al₂O₃ sublayers. The PL intensity exhibits a nonmonotonic temperature dependence: with increasing temperature, the integrated intensity almost remains constant from 14 to 50 K, then reaches maximum at 225 K, and slightly increases again at higher temperatures. Meanwhile, the PL integrated intensity at room temperature is about 30% higher than that at 14 K.     

The photoluminescent properties of Eu in MgO-Ga2O3-SiO2 nanocrystalline glass-ceramic

The MgO-Ga₂O₃-SiO₂ glass-ceramic (GC) containing MgGa₂O₄ nanocrystals and glasses doped with Eu³⁺ ions were prepared by the sol-gel method. The down-conversion and up-conversion luminescence (UCL) properties were studied. The results indicated that the relative intensity of f-f transitions of Eu³⁺ decreased in contrast with that of charge transfer (CT) absorption with the increase in heating temperature. Using a Xe lamp and 800 nm femtosecond (fs) laser excitation, strong red luminescence of Eu³⁺ in MgO-Ga₂O₃-SiO₂ glasses and GC was observed.     

The interface reaction of high-k La2Hf2O7/Si thin film grown by pulsed laser deposition

The La₂Hf₂O₇ films have been deposited on Si (1 0 0) substrate by using pulsed laser deposition (PLD) method. X-ray diffraction (XRD) demonstrates that the as-grown film is amorphous and crystallizes after 1000 °C annealing. The interface structure is systematically studied by Synchrotron X-ray reflectivity (XRR), Fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). Silicide, silicate and SiO_x formations from interfacial reaction are observed on the surface of the Si substrate in the as-grown film. The impact of silicide formation on the electrical properties is revealed by capacitance-voltage (C-V) measurements. By post-deposition annealing (PDA), silicide can be effectively eliminated and C-V property is obviously improved.     

An XPS study and electrical properties of Pb1.1Zr0.53Ti0.47O3/PbO/Si (MFIS) structures according to the substrate temperature of the PbO buffer layer

PbO and PZT thin films were deposited on the p-type (1 0 0) Si substrate by the rf magnetron sputtering method with PbO and Pb_1.1Zr_0.53Ti_0.47O₃ targets for the application of the metal-ferroelectric-insulator-semiconductor (MFIS) structure. The MFIS structures with the PbO buffer layer show the good electric properties including a high memory window and a low leakage current density. The maximum value of the memory window is 2.0 V under the applied voltage of 9 V for the Pt/PZT (200 nm, 400 °C)/PbO (80 nm)/Si structures with the PbO buffer layer deposited at the substrate temperature of 300 °C. From the X-ray photoelectron spectroscopy (XPS) results, we could confirm that the substrate temperature of PbO affects the chemical states of the interface between the PbO buffer layer and Si substrate, which results in the inter-diffusion of Pb and the formation of the intermediate phases (PbSiO₃). And the existence of the undesired SiO₂ layer, which is the low dielectric layer, was confirmed at the surface region of the Si substrate by the XPS depth profile analysis.     

Influence of high temperature annealing on the structure, hardness and tribological properties of diamond-like carbon and TiAlSiCN nanocomposite coatings

Diamond-like carbon (DLC) and TiAlSiCN nanocomposite coatings were synthesized and annealed at different temperatures in a vacuum environment. The microstructure, hardness and tribological properties of as-deposited and annealed DLC-TiAlSiCN nanocomposite coatings were characterized by X-ray diffraction, X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), Raman spectroscopy, nano-indentation and friction tests. The TEM results reveal that the as-deposited DLC-TiAlSiCN coating has a unique nanocomposite structure consisting of TiCN nanocrystals embedded in an amorphous matrix consisting of a-Si₃N₄, a-SiC, a-CN and DLC, and the structure changed little after annealing at 800 °C. However, XPS and Raman results show that an obvious graphitization of the DLC phase occurred during the annealing process and it worsened with annealing temperature. Because of the graphitization, the hardness of the DLC-TiAlSiCN coating after annealing at 800 °C decreased from 45 to 36 GPa. In addition, the DLC-TiAlSiCN coating after annealing at 800 °C has a similar friction coefficient to the as-deposited coating.     

The influence of substrate on the properties of Er2O3 films grown by magnetron sputtering

The structural properties and the room temperature luminescence of Er₂O₃ thin films deposited by RF magnetron sputtering have been studied. Films characterized by good morphological properties have been obtained by using a SiO₂ interlayer between the film and the Si substrate. The evolution of the properties of the Er₂O₃ films due to rapid thermal annealing processes in O₂ ambient performed at temperatures in the range 800-1200 °C has been investigated in details. The existence of well-defined annealing conditions (temperature of 1100 °C or higher) allowing to avoid the occurrence of extensive chemical reactions with the oxidized substrate has been demonstrated and an increase of the photoluminescence (PL) intensity by about a factor of 40 with respect to the as deposited material has been observed. The enhanced efficiency of the photon emission process has been correlated with the longer lifetime of the PL signal. The same annealing processes are less effective when Er₂O₃ is deposited on Si. In this latter case interfacial reactions and pit formation occur, leading to a material characterized by stronger non-radiative phenomena that limit the PL efficiency.     

Annealing temperature dependence of Raman scattering in Si/SiO2 superlattice prepared by magnetron sputtering

Si/SiO₂ superlattices were prepared by magnetron sputtering, and the deposition temperature and annealing temperature had a great influence on the superlattice structure. In terms of SEM images, the mean size of Si nanocrystals annealed at 1100 °C is larger than that of nanocrystals annealed at 850 °C. It was found that the films deposited at room temperature are amorphous. With increasing deposition temperature, the amorphous and crystalline phases coexist. With increasing annealing temperature, the Raman intensity of the peak near 470 cm⁻¹ decreases, and the intensity of that at 520 cm⁻¹ increases. Also, on increasing the annealing temperature, the Raman peak near 520 cm⁻¹ shifts and narrows, and asymmetry emerges. A spherical cluster is used to model the nanocrystals in Si/SiO₂ superlattices, and the observed Raman spectra are analyzed by combining the effects of confinement on the phonon frequencies. Raman spectra from a variety of nanocrystalline silicon structures were successfully explained in terms of the phonon confinement effect. The fitted results agreed well with the experimental observations from SEM images.     

Effects of annealing temperature on structure and magnetic properties of CoAl0.2Fe1.8O4/SiO2 nanocomposites

CoAl_0.2Fe_1.8O₄/SiO₂ nanocomposites were prepared by sol–gel method. The effects of annealing temperature on the structure and magnetic properties of the samples were studied by X-ray diffraction, transmission electron microscopy, vibrating sample magnetometer and Mössbauer spectroscopy. The results show that the CoAl_0.2Fe_1.8O₄ in the samples exhibits a spinel structure after being annealed. As annealing temperature increases from 800 to 1200 °C, the average grain size of CoAl_0.2Fe_1.8O₄ in the nanocomposites increases from 5 to 41 nm while the lattice constant decreases from 0.8397 to 0.8391 nm, the saturation magnetization increases from 21.96 to 41.53 emu/g. Coercivity reaches a maximum of 1082 Oe for the sample annealed at 1100 °C, and thereafter decreases with further increasing annealing temperature. Mössbauer spectra show that the isomer shift decreases, hyperfine field increases and the samples transfer from mixed state of superparamagnetic and magnetic order to the completely magnetic order with annealing temperature increasing from 800 to 1200 °C.     

Evolution of Si0.8Ge0.2 quantum dots during Si encapsulation

Surface structure, determined by scanning tunneling microscopy (STM), surface morphology, determined by atomic force microscopy (AFM), and surface composition, determined by X-ray photoelectron spectroscopy (XPS) of 20.0 nm Si_0.8Ge_0.2 quantum dots formed at 800 °C and encapsulated with 0-10 nm of Si at 500 °C and 800 °C are presented. It is observed that the quantum dot surface morphology changes during the Si encapsulation at 800 °C by the smoothing of the quantum dots. The height of the quantum dots decreases faster than can be accounted for from the amount of Si deposited, indicating that there is movement of material out of the quantum dots during the encapsulation process. Encapsulation at 500 °C results in a retention of the quantum dot surface morphology with increased Ge segregation compared to Si encapsulation at 800 °C. We conclude that the changing surface morphology at 800 °C is not the result of Ge segregation but due to intermixing resulting from the tensile strain of Si depositing on SiGe.     

Physical and electrical characteristics of a high-k Yb2O3 gate dielectric

High-k ytterbium oxide (Yb₂O₃) gate dielectrics were deposited on Si substrate by reactive sputtering. The structural features of these films after postdeposition annealing treatment were studied by X-ray diffraction and X-ray photoelectron spectroscopy. It is found that the Yb₂O₃ gate dielectrics annealed at 700 °C exhibit a larger capacitance value, a lower frequency dispersion and a smaller hysteresis voltage in C-V curves compared with other annealing temperatures. They also show negligible charge trapping under high constant voltage stress. This phenomenon is mainly attributed to the decrease in the amorphous silica thickness.     

Effects of annealing temperature and method on structural and optical properties of TiO2 films prepared by RF magnetron sputtering at room temperature

TiO₂ thin film was deposited on non-heated Si(1 0 0) substrate by RF magnetron sputtering. The as-deposited films were annealed by a conventional thermal annealing (CTA) and rapid thermal annealing (RTA) at 700 and 800 °C, and the effects of annealing temperature and method on optical properties of studied films were investigated by measuring the optical band gaps and FT-IR spectra. And we also compared the XRD patterns of the studied samples. The as-deposited film showed a mixed structure of anatase and brookite. Only rutile structures were found in samples annealed above 800 °C by CTA, while there are no special peaks except the weak brookite B(2 3 2) peak for the sample annealed at (or above) 800 °C by RTA. FT-IR spectra show the broad peaks due to Ti-O vibration mode in the range of 590-620 cm⁻¹ for the as-deposited film as well as samples annealed by both annealing methods at 700 °C. The studied samples all had the peaks from Si-O vibration mode, which seemed to be due to the reaction between TiO₂ and Si substrate, and the intensities of these peaks increased with increasing of annealing temperature. The optical band gap of the as-deposited film was 3.29 eV but it varied from 3.39 to 3.43 eV as the annealing temperature increased from 700 to 800 °C in the samples annealed by CTA. However, it varied from 3.38 to 3.32 eV as the annealing temperature increased from 700 to 800 °C by RTA.     

Effect of CaO-B2O3-SiO2 glass on the magnetic and dielectric properties of NiCuZn ferrites

NiCuZn ferrites with different contents of CaO-B₂O₃-SiO₂ glasses were synthesized by a conventional ceramic technology and sintered at 1050 °C. It was found that the addition of CaO-B₂O₃-SiO₂ influenced the magnetic and dielectric properties of the ferrites. The saturation magnetization increased at first and reached its maximum with the sample of 2 wt% CaO-B₂O₃-SiO₂, and then decreased. The initial permeability decreased with the content of CaO-B₂O₃-SiO₂ but the cut-off frequency increased. The quality factor decreased first and then increased; the maximum quality factor was obtained in the sample with 3 wt% CaO-B₂O₃-SiO₂. With increasing content of CaO-B₂O₃-SiO₂, the permittivity increased sharply. The possible reasons responsible for these changes are explained.     

Mechanical stress in ALD-Al2O3 films

Mechanical stress in atomic-layer deposition (ALD)-Al₂O₃ films was investigated at room temperature and during thermal cycling up to 870 °C. The films were generally under tensile stress. Thicker films (25-60 nm) showed a sharp stress increase at about 780-790 °C. X-ray diffraction (XRD)-, X-ray reflectance (XRR)- and X-ray photoelectron spectroscopy (XPS)-measurements indicate an irreversible phase transition from amorphous AlO(OH) to a mixture of different crystalline Al₂O₃-phases. Annealing at higher temperatures leads to a stress reduction as a result of diffusion and recovery processes. The stress behaviour of thinner films (<20 nm) during thermal cycling is quite different. Tensile stress increases with increasing temperature and decreases to nearly the same value during cooling down. The process is continuous and reversible.     

The properties of the Y2O3 films exposed at elevated temperature

Yttrium trioxide (Y₂O₃) thin films have been deposited on silicon (1 1 1) substrates by RF magnetron sputtering. The influences of thermal exposure at high temperature in air on the structure, the surface morphology, roughness, and the refractive index of the Y₂O₃ thin film were investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), atomic force microscopy (AFM), and spectroscopic ellipsometry (SE). The results indicate that chemical composition of the as-deposited Y₂O₃ film is apparently close to the stoichiometric ratio, and it has a cubic polycrystalline structure but the crystallinity is poor. The monoclinic and cubic phases can coexist in the Y₂O₃ film after thermal exposure to 900 °C, and the monoclinic phase disappears completely after 300 s exposure to 950 °C. The changes of the surface morphology, roughness, and the refractive index of the Y₂O₃ film are closely related to the crystal structure, the internal stress, and various defects influenced by thermal exposure temperature and time.     

Effect of annealing temperature on the decomposition of reactively sputtered Ag2Cu2O3 films

Ag₂Cu₂O₃ films were deposited on glass substrates by reactive sputtering of a composite silver-copper target. The deposited films were annealed in air at 100, 200 and 300 °C. The structure of the films was studied using X-ray diffraction (XRD), their surface morphology was characterised using scanning electron microscopy (SEM) and their electrical resistivity at room temperature was measured using the four point probe method. The 100 °C annealing did not modify either the film structure or the film morphology. On the other hand, Ag₂Cu₂O₃ films were partially decomposed into Ag and CuO after a 200 °C annealing. The decomposition was complete for a 300 °C annealing. The evolution of the film surface morphology as a function of the annealing temperature was discussed in connection to the evolution of the molar volume of the phases constituting the films.     

Structural properties and electrical characteristics of high-k Tm2Ti2O7 gate dielectrics

In this article, the structural and electrical characteristics of high-k Tm₂Ti₂O₇ gate dielectrics deposited on Si (1 0 0) by means of reactive cosputtering were reported. The Tm₂Ti₂O₇ dielectrics annealed at 800 °C exhibited excellent electrical properties such as high capacitance value, small density of interface state, almost no hysteresis voltage, and low leakage current. This phenomenon is attributed to a rather well-crystallized Tm₂Ti₂O₇ structure and composition and a smooth surface observed by X-ray diffraction, X-ray photoelectron spectroscopy, and atomic force microscopy, respectively. This film also shows almost negligible charge trapping under high constant voltage stress.     

Characteristics of sandwich-structured Al2O3/HfO2/Al2O3 gate dielectric films on ultra-thin silicon-on-insulator substrates

Sandwich-structure Al₂O₃/HfO₂/Al₂O₃ gate dielectric films were grown on ultra-thin silicon-on-insulator (SOI) substrates by vacuum electron beam evaporation (EB-PVD) method. AFM and TEM observations showed that the films remained amorphous even after post-annealing treatment at 950 °C with smooth surface and clean silicon interface. EDX- and XPS-analysis results revealed no silicate or silicide at the silicon interface. The equivalent oxide thickness was 3 nm and the dielectric constant was around 7.2, as determined by electrical measurements. A fixed charge density of 3 × 10¹⁰ cm⁻² and a leakage current of 5 × 10⁻⁷A/cm² at 2 V gate bias were achieved for Au/gate stack /Si/SiO₂/Si/Au MIS capacitors. Post-annealing treatment was found to effectively reduce trap density, but increase in annealing temperature did not made any significant difference in the electrical performance.