Improved moisture resistance of SrS:Eu phosphors with nanoscale SiO2 coating

Orange-emitting SrS:Eu²⁺ phosphors were coated with nanoscale SiO₂ and their photoluminescence (PL) degradation behavior in moist air was investigated. The SiO₂ coating was obtained by sol-gel process using diethoxydimethylsilane (DEDMS) and the coating content was varied from 0.5 to 2 wt%. The coatings were composed of a uniform, continuous, and amorphous SiO₂ layer of 30-50 nm thickness and the coating thickness was not varied significantly with the coating content. No peak shift and no decrease of PL intensity were observed after coating. The PL intensity of the coated phosphors decreased to ∼75% of the original value after 10 h exposure to moist air, while the uncoated phosphor decreased to ∼33%, which indicates the improved moisture resistance of the nanoscale SiO₂ coated SrS:Eu²⁺ phosphors.     

Effects of the surface coating of BaMgAl10O17:Eu phosphor with SiO2 nano-particles

BaMgAl₁₀O₁₇:Eu²⁺(BAM) phosphors were coated with SiO₂ nano-particles by a modified sol-gel method. In order to elucidate the effects of SiO₂ coating onto BAM phosphor, the luminescent decay time is measured before and after SiO₂ coating. It was revealed that surface coating of BAM phosphors with SiO₂ leads to an increase in luminescent decay time and quantum efficiency, due to the suppression of nonradiative decay via surface defects. The experimental results suggest that the nonradiative decay via surface defects is an important relaxation process, related to the optical properties of display devices such as plasma display panels (PDP) and lamps.     

Oxide coatings on Y3Al5O12:Tb particles

A coating method with precipitating process was developed to reduce the particle size and to improve the particle dispersion of Y₃Al₅O₁₂:Tb³⁺ phosphor prepared by sol-gel method. The particle morphology was observed by using SEM and TEM; and the particle size and its dispersion was measured by using laser scattering technique. Several coating materials were tested. Among them, Al₂(SiO₃)₃ coating not only reduced the particle size from several micrometers to ∼1 μm and improved the particle dispersion, but also well kept luminescent intensities and improved the duration of the phosphor under the bombardment of cathode ray. The mechanism of the particle size reduction was proposed.     

A potential green-emitting phosphor Ca8Mg(SiO4)4Cl2:Eu for white light emitting diodes prepared by sol-gel method

A potential green emitting phosphor Ca₈Mg(SiO₄)₄Cl₂:Eu²⁺ was prepared by modified sol-gel method. The factors those affect the photoluminescence intensity including heating temperature, the usage of the chlorine source CaCl₂ and the concentration of dopant Eu²⁺ were also investigated in detail. As comparison, the phosphor prepared by solid-state reaction was also prepared. The phosphors show intense absorption in the range of 375-450 nm, which makes it a potential candidate of green emitting phosphor used for near-UV or blue light excited white LEDs.     

Synthesis and characterization of spherical core-shell particles SiO2@AgEu(MoO4)2

Submicron spherical SiO₂ particles have been coated with AgEu(MoO₄)₂ phosphor layers by a sol-gel process, followed by surface reaction at high temperature, to get core/shell structured SiO₂@AgEu(MoO₄)₂ particles. X-ray diffraction (XRD), Fourier-transformed infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM) were used to characterize the structure and morphology of the resulted core-shell phosphors. The luminescent properties of the core-shell structured phosphors have also been measured at room temperature, and their photoluminescence (PL) spectra are similar to the pure AgEu(MoO₄)₂ phosphor prepared by the same sol-gel method exhibiting red emission.     

Surface treatment investigation and luminescence properties of SiO2-coated Ca2BO3Cl:0.02Eu2+ phosphors via sol–gel process

SiO₂-coated Ca₂BO₃Cl:Eu²⁺ phosphors were prepared by the sol–gel method in order to enhance the chemical and thermal stabilities of Ca₂BO₃Cl:Eu²⁺ phosphor. The phase structures, microstructures and luminescence properties were studied by the X-ray diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spectrometer, respectively. The emission intensity of SiO₂-coated Ca₂BO₃Cl:Eu²⁺ phosphor decreased a little compared to that of the uncoated phosphor. The moisture resistances of the phosphors were comparatively examined by the aging treatment experiment in the water, and the thermal stability was studied by the temperature dependent photoluminescence spectra. The results indicated that SiO₂ coating on the surface of the phosphor particles improved the moisture-resistance and thermal stability to a large extent.     

SiC/SiO2 coating for improving the oxidation resistive property of carbon nanofiber

The SiC/SiO₂ deposition was performed to improve the oxidation resistive properties of carbon nanofiber (CNF) from electrospinning at elevated temperatures through sol-gel process. The stabilized polyacrylonitrile (PAN) fibers were coated with SiO₂ followed by heat treatment up to 1000 and 1400 °C in an inert argon atmosphere. The chemical compositions of the CNFs surface heat-treated were characterized as C, Si and O existing as SiC and SiO₂ compounds on the surface. The uniform and continuous coating improved the oxidation resistance of the carbon nanofibers. The residual weight of the composite was 70-80% and mixture of SiC, SiO₂ and some residual carbon after exposure to air at 1000 °C.     

Evaluating Zn2SiO4:Mn phosphor for use in medical imaging radiation detectors

2 SiO₄:Mn phosphor was evaluated for use in radiation detectors of medical imaging systems. Zn₂SiO₄:Mn was used in the form of laboratory-prepared fluorescent layers (screens) with coating weights from 18 to 150 mg/cm². The phosphor was excited to luminescence by low-energy X-raysusing X-raytube voltages ranging from 15 to 50 kVp. The number of emitted optical photons per incident X-rayquantum was thus determined for various X-rayenergies and phosphor coating weights. The optical emission spectrum was also measured and it was used to evaluate the spectral compatibility of Zn₂SiO₄:Mn with radiographic films, photocathodes and the Si photodiode. Finally, phosphor optical properties were estimated by fitting a theoretical model to experimental data. Results showed that Zn₂SiO₄:Mn is more efficient for low-energy X-rays. Its intrinsic conversion efficiency was found equal to 0.08, which is comparable to that of actually used phosphors. Zn₂SiO₄:Mn was also adequately compatible with orthochromatic films and the ES-20 photocathode, thus being appropriate for low-voltage radiography and fluoroscopy. Received: 31 July 1998/Accepted: 3 August 1998     

Enhanced corrosion resistance and cellular behavior of ultrafine-grained biomedical NiTi alloy with a novel SrO-SiO2-TiO2 sol-gel coating

NiTi alloy has a unique combination of mechanical properties, shape memory effects and superelastic behavior that makes it attractive for several biomedical applications. In recent years, concerns about its biocompatibility have been aroused due to the toxic or side effect of released nickel ions, which restricts its application as an implant material. Bulk ultrafine-grained Ni50.8Ti49.2 alloy (UFG NiTi) was successfully fabricated by equal-channel angular pressing (ECAP) technique in the present study. A homogeneous and smooth SrO-SiO₂-TiO₂ sol-gel coating without cracks was fabricated on its surface by dip-coating method with the aim of increasing its corrosion resistance and cytocompatibility. Electrochemical tests in simulated body fluid (SBF) showed that the pitting corrosion potential of UFG NiTi was increased from 393 mV(SCE) to 1800 mV(SCE) after coated with SrO-SiO₂-TiO₂ film and the corrosion current density decreased from 3.41 μA/cm² to 0.629 μA/cm². Meanwhile, the sol-gel coating significantly decreased the release of nickel ions of UFG NiTi when soaked in SBF. UFG NiTi with SrO-SiO₂-TiO₂ sol-gel coating exhibited enhanced osteoblast-like cells attachment, spreading and proliferation compared with UFG NiTi without coating and CG NiTi.     

Enhanced luminescence and degradation of SiO2:Ce,Tb powder phosphors prepared by a sol-gel process

Enhanced green photoluminescence and cathodoluminescence (CL) from Tb³⁺ ions due to co-doping with Ce³⁺ ions were observed from SiO₂:Ce,Tb powder phosphors prepared by a sol-gel technique. Blue emission from the Ce³⁺ ions was completely suppressed by Tb co-doping, presumably due to energy transfer from Ce³⁺ to Tb³⁺. In addition, the green CL intensity from SiO₂:Ce,Tb degraded by ∼50% when the powders were irradiated for 10 h with a 2 keV, 54 mA/cm² beam of electrons in an ultra-high vacuum chamber containing either 1×10⁻⁸ or 1×10⁻⁷ Torr O₂. Desorption of oxygen from the surface was observed during the decrease of CL intensity. The mechanisms for energy transfer from Ce³⁺ ions to Tb³⁺ ions to enhance the green luminescence, and mechanisms for desorption of oxygen from the phosphor surface that would result in decreased CL intensity are discussed.     

Nanostructured porous SiO2 films for antireflection coatings

Thin films with a low refractive index play an important role in optics, optoelectronics, and microelectronics. In this study, we present nanostructured porous SiO₂ films fabricated by using a glancing angle deposition technique. These nanostructured porous SiO₂ films deposited at an angle of 85° show very low refractive indices of 1.08 at 633 nm. As an application, a four-layer antireflection coating for visible wavelength is designed and fabricated using SiO₂ material only. The normal incidence reflectance of the antireflection coating averaged between 400 and 800 nm is about 0.04%. The microstructure and the surface morphology are also investigated by using a scanning electron microscope.     

Degradation of Y2SiO5:Ce phosphor powders

The degradation of the cathodoluminescence (CL) intensity of cerium-doped yttrium silicate (Y₂SiO₅:Ce) phosphor powders was investigated for possible application in low voltage field emission displays (FEDs). Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and CL spectroscopy were used to monitor changes in the surface chemical composition and luminous efficiency of commercially available Y₂SiO₅:Ce phosphor powders. The degradation of the CL intensity for the powders is consistent with a well-known electron-stimulated surface chemical reaction (ESSCR) model. It was shown with XPS and CL that the electron stimulated reaction led to the formation of a luminescent silicon dioxide (SiO₂) layer on the surface of the Y₂SiO₅:Ce phosphor powder. XPS also indicated that the Ce concentration in the surface layer increased during the degradation process and the formation of CeO₂ and CeH₃ were also part of the degradation process. The CL intensity first decreased until about 300 C cm⁻² and then increased due to an extra peak arising at a wavelength of 650 nm.     

Spherical Zn2SiO4:Eu@SiO2 phosphor particles in core-shell structure: Synthesis and characterization

Spherical SiO₂ particles have been coated with Zn₂SiO₄:Eu³⁺ phosphor layers by a Pechini sol-gel process. The microstructure and luminescent properties of the obtained Zn₂SiO₄:Eu³⁺@SiO₂ particles were well characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra, and lifetime. The results demonstrate that the Zn₂SiO₄:Eu³⁺@SiO₂ particles, which have regular and uniform spherical morphology, emitted an intensive red light emission at 613 nm under excitation at 395 nm. Besides, the effects of the Eu³⁺ concentration, annealing temperature and charge compensators of Li⁺ ions on the PL emission intensities were investigated in detail.     

High-temperature oxidation behavior of SiO2 protective layer deposited on IN738LC superalloy by combustion CVD (CCVD)

A SiO₂ protective coating was deposited on an IN738LC alloy using CCVD. The physical properties of a SiO₂ protective layer are influenced by the amount of tetraethyl orthosilicate (TEOS, C₈H₂₀O₄Si). Therefore, the SiO₂ protective coating was deposited using different TEOS concentrations and deposition times to optimize the conditions. The deposited coating layer was confirmed to be a SiO₂ layer by SEM, EDX, and ESCA analyses. The oxidation resistance of the alloy was evaluated by thermo gravimetric analysis. The oxidation resistance of the SiO₂ protective coating was highest when the coating was processed at a TEOS concentration of 0.05 mol/l, which is the highest concentration of source material used. The surface roughness of the SiO₂ protective layer also increased with increasing TEOS concentration. The surface roughness of the coating had little effect on the oxidation resistance for a film thickness of approximately 1 μm.     

Synthesis and magnetic properties of carbon-coated Ni/SiO2 core/shell nanocomposites

A simple method for the synthesis of carbon-coated Ni/SiO₂ core/shell nanocomposites is reported. The Ni nanoparticles were coated with silica layers via a combined procedure of sol-gel fabrication and hydrogen reduction prior to carbon coating via acetylene decomposition at an appropriate temperature. It was found that the anti-acid ability of the Ni/SiO₂ composites was greatly enhanced after carbon coating. The results of magnetization measurement show that the real part (μ′) of complex permeability of the as-obtained sample is almost independent of frequency, and the imaginary part (μ″) stays small up to a frequency of 1 GHz. The encapsulation of Ni particles with SiO₂ results in the rise of Ni nanoparticles resistivity. The outcome is the reduction in effect of eddy current at high frequency, making the real part μ′ almost constant and the imaginary part μ″ very small. Thus, this simple method may be effective for preparing composites of soft magnetic properties, especially in the high-frequency range. Supported by the Jiangsu Postdoctoral Foundation of Jiangsu Province and the Major Project of National Basic Research Program of China (Grant No. 2005CB623605)     

Y2SiO5:Tb phosphor particles prepared from colloidal and aqueous solutions by spray pyrolysis

Green-emitting Y₂SiO₅:Tb phosphor particles with fine size, spherical shape, filled morphology, high crystallinity, and good brightness were synthesized by a spray pyrolysis process. The effect of silicon precursor type on the morphology, crystal structure, crystallinity, and photoluminescence efficiency of Y₂SiO₅:Tb phosphor particles was investigated. The particles prepared from an artificial colloidal solution obtained by dispersing fumed silica particles had a pure monoclinic X2 crystalline phase, which is more appropriate for application to displays, after post-treatment at 1300 °C. On the other hand, the particles prepared from 100% tetraethyl orthosilicate (TEOS) reagent had an X2 phase and small amounts of X1 and impurity phases such as Y₂Si₂O₇ and Y_4.67Si₃O₁₃ due to the phase-segregation characteristics of the TEOS precursor. The photoluminescence characteristics of Y₂SiO₅:Tb phosphor particles were strongly affected by the silicon source used. The photoluminescence intensities increased with the fumed silica/TEOS ratio. The particles prepared from 100% fumed silica showed the maximum photoluminescence intensity, which is 22% higher than that of particles prepared from 100% TEOS. PACS 81.20.Rg; 78.55.Hx; 78.40.Ha; 81.05.Hd; 81.40.Tv     

Low-temperature synthesis of Zn2SiO4:Mn green photoluminescence phosphor

Zn₂SiO₄:Mn green phosphor having comparable photoluminescence (PL) efficiency with commercial phosphor has been synthesized at 1000 °C using solid state reactions involving ZnO, silicic acid and manganese acetate. The water of crystallization attached to SiO₂ in silicic acid whose dissociation at 1000 °C seem to promote the sintering efficiency of Zn₂SiO₄:Mn. Incremental ZnO addition and re-firing at 1000 °C promote the diffusion rate of ZnO and SiO₂. The formation of a single crystalline phase of willemite structure in the samples was confirmed by powder XRD measurements. The phosphor exhibit an intense excitation band centered around 275 nm and a relatively weak excitation centered around 380 nm while the broad band green emission peaks at 524 nm. Other parameters studied include PL spectra, grain morphology, ZnO/SiO₂ molar ratio, Mn concentration, co-dopant/flux and the effect of chemical forms of Mn dopant as well as silica on the PL efficiency.     

Luminescence and energy transfer of white-light emitting CaAl2SiO6:Ce3+, Tb3+ phosphors

A novel white-light emitting CaAl₂SiO₆: Ce³⁺, Tb³⁺ phosphor has been prepared by a sol–gel method. X-ray diffractometry and spectrofluorometry were used to characterize structural and optical properties of the samples. The results indicate that the crystal structure of the phosphor is a single phase of CaAl₂SiO₆. The excitation band of the phosphor covers a wide region from 240 nm to 380 nm. CaAl₂SiO₆: Ce³⁺, Tb³⁺ phosphors show four emission bands: one at 400 nm for Ce³⁺ and three at 487 nm, 543 nm and 585 nm for Tb³⁺. With appropriate tuning of Tb³⁺ content, white light with different hues can be achieved under UV radiation. The energy transfer mechanism from Ce³⁺ to Tb³⁺ in CaAl₂SiO₆ host was demonstrated to be dipole–dipole interaction.     

Synthesis and VUV spectral properties of nanoscaled Zn2SiO4:Mn green phosphor

Nanoscaled Zn₂SiO₄:Mn²⁺ green phosphor with regular and uniform morphology was synthesized by hydrothermal method at a low temperature of 140 °C. The structure and morphology of the phosphor was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of the hydrothermal temperature and the time on the crystallite structure and the vacuum ultraviolet (VUV) photoluminescence (PL) properties were evaluated. The as-synthesized nanoscaled Zn₂SiO₄:Mn²⁺ phosphor exhibited intensive broad emission around 523 nm, which was attributed to the ⁴T₁→⁶A₁ transition of Mn²⁺. The PL intensity increased along with the increasing hydrothermal temperature and time. The heat-treated phosphors exhibited higher PL intensity than the corresponding samples prepared using the conventional solid-state reaction.     

XPS surface analysis of monocrystalline silicon solar cells for manufacturing control

X-ray photoelectron spectroscopy (XPS) has been applied to surfaces of silicon wafers in the different stages of the assembly line for large-scale monocrystalline silicon solar cell manufacturing (ISOFOTON, Malaga, Spain). XPS results have shown that a considerable amount of carbon is present on the pyramidal-textured monocrystalline silicon surface. This amount decreases slightly but is still present after the process of phosphor diffusion (p-n junction), as well as after subsequent calcination in humid air for SiO₂ film formation (passivation). This amount of carbon may be buried during the process of CVD coating an anti-reflection TiO₂ film. After calcination of the film in order to obtain the TiO₂ rutile phase, an even higher amount of carbon is detected on the TiO₂ anti-reflection coating surface. This indicates that not all organics from the tetra-isopropile ortho-titanate (TPT) precursor were released from the film. Furthermore, in this case phosphor is found in excess on the SiO₂ wafer surface (dead layer) and also on the rutile TiO₂ surface, indicating that an extra phosphor diffusion from the bulk silicon through the TiO₂ film has taken place during calcination. These results demonstrate how thermal treatments applied in the solar cell manufacturing assembly line can influence and may change the intended compositional distribution. These treatments may also introduce defects that act as recombination centres for charge carriers in the solar cell device. Received: 13 September 2000 / Accepted: 10 January 2001 / Published online: 3 May 2001