Phase transformation and photoluminescence properties of nanocrystalline ZrO2 powders prepared via the Pechini-type sol-gel process

Nanocrystalline ZrO2 fine powders were prepared via the Pechini-type sol-gel process followed by annealing from 500 to 1000 degrees C. The obtained ZrO2 samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), electron paramagnetic resonance (EPR), and photoluminescence spectra (PL), respectively. The phase transition process from tetragonal (T) to monoclinic (M) was observed for the nanocrystalline ZrO2 powders in the annealing process, accompanied by the change of their photoluminescence properties. The 500 degrees C annealed ZrO2, powder with tetragonal structure shows an intense whitish blue emission (lambda(max) = 425 nm) with a wide range of excitation (230-400 nm). This emission decreased in intensity after being annealed at 600 degrees C (T + M-ZrO2) and disappeared at 700 (T + M-ZrO2), 800 (T + M-ZrO2), and 900 degrees C (M-ZrO2). After further annealing at 1000 degrees C (M-ZrO2), a strong blue-green emission appeared again (lambda(max) = 470 nm).

Nanocrystalline LaAlO3:Sm3+ as a Promising Yellow Phosphor for Field Emission Displays

Nanocyrstalline LaAlO3:Sm3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. XRD results reveal that the sample begins to crystallize at 600 degrees C, and pure LaAlO3 phase can be obtained at 700 degrees C. FE-SEM images indicate that the Sm3+-doped LaAlO3 phosphors are composed of aggregated spherical particles with sizes ranging from 40 to 80 nm. Under the excitation of UV light (245 nm) and low-voltage electron beams (1-3 kV), the Sm3+-doped LaAlO3 phosphors show the characteristic emissions of the Sm3+ ((4)G(5/2)-H-6(5/2), H-6(7/2), H-6(9/2) transitions) with a yellow color. The CL intensity (brightness) of the Sm3+-doped LaAlO3 phosphor is higher than that of the commercial product [Zn(Cd)S:Ag+] (yellow) to some extent.

Growth of highly crystalline CaMoO4 : Tb3+ phosphor layers on spherical SiO2 particles via sol-gel process: Structural characterization and luminescent properties

Highly crystalline CaMoO4:Tb3+ phosphor layers were grown on monodisperse SiO2 particles through a simple sol-gel method, resulting in formation of core-shell structured SiO2@CaMoO4:Tb3+ submicrospheres. The resulting SiO2@CaMoO4: Tb3+ core-shell particles were fully characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), and kinetic decays. The XRD results demonstrate that the CaMoO4:Tb3+ layers begin to crystallize on the SiO2 spheres after annealing at 400 degrees C and the crystallinity increases with raising the annealing temperature. SEM and TEM analysis indicates that the obtained submicrospheres have a uniform size distribution and obvious core-shell structure. SiO2@CaMoO4:Tb3+ submicrospheres show strong green emission under short ultraviolet (260 nm) and low-voltage electron beam (1-3 kV) excitation, and the emission spectra are dominated by a D-5(4) -F-7(5) transition of Tb3+(544 nm, green) from the CaMoO4:Tb3+ shells.

Nanocrystalline LaGaO3 : Tm3+ as an efficient blue phosphor for field emission displays with high color purity

Nanocrystalline Tm3+-doped LaGaO3 phosphors were prepared through a Pechini-type sol-gel process [M. P. Pechini, U.S. Patent No. 3,330,697 (11 July 1967)]. X-ray diffraction, field emission scanning electron microscopy, photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. Under the excitation of ultraviolet light and low voltage electron beams (0.5-3 kV), the Tm3+-doped LaGaO3 phosphors show the characteristic emissions from the LaGaO3 host lattice and the Tm3+ (D-1(2), (1)G(4)-F-3(4), and H-3(6) transitions), respectively. The blue CL of the Tm3+-doped LaGaO3 phosphors, with a dominant wavelength of 458 nm, had better Commission International I'Eclairage chromaticity coordinates (0.1552, 0.0630) and higher emission intensity than the commercial product (Y2SiO5:Ce3+).

Sol-gel synthesis and characterization of SiO2@NaGd(WO4)(2): Eu3+ core-shell-structured spherical phosphor particles

Monodisperse, core-shell-structured SiO2@NaGd(WO4)(2):Eu3+ particles were prepared by the sol-gel method. The samples were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, photoluminescence (PL), and low-voltage cathodoluminescence (CL) as well as time-resolved PL spectra and lifetimes. PL and CL study revealed that the core-shell-structured SiO2@NaGd (WO4)(2):Eu3+ particles show strong red emission dominated by the D-5(0) - F-7(2) transition of Eu3+ at 614 nm with a lifetime of 0.74 ms. The PL and CL emission intensity can be tuned by the coating number of NaGd(WO4)(2):Eu3+ phosphor layers on SiO2 and by accelerating voltage and the filament current, respectively.

Host-sensitized luminescence of Dy3+, Pr3+, Tb3+ in polycrystalline SrIn2O4 for field emission displays

SrIn2O4:Dy3+/Pr3+/Tb3+ white/red/green phosphors were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), diffuse reflectance, photoluminescence, cathodoluminescence spectra, and lifetimes were utilized to characterize the samples. XRD reveal that the samples begin to crystallize at 800 degrees C and pure SrIn2O4 phase can be obtained at 900 degrees C. FE-SEM images indicate that the SrIn2O4:Dy3+, SrIn2O4:Pr3+, and SrIn2O4:Tb3+ samples consist of fine and spherical grains with size around 200-400 nm. Under the excitation of ultraviolet light and low-voltage electron beams (1 - 5 kV), the SrIn2O4:Dy3+, SrIn2O4: Pr3+, and SrIn2O4: Tb3+ phosphors show the characteristic emissions of Dy3+ (F-4(9/2) - H-6(15/2) at 492 nm and 4F(9/2) - 6H(13/2) at 581 nm, near white), Pr3+ (P-3(0) - H-3(4) at 493 nm, D-1(2) - H-3(4) at 606 nm, and P-3(0) - H-3(6) at 617 nm, red) and Tb3+ (D-5(4) - F-7(6,5,4,3) transitions dominated by D-5(4) - F-7(5) at 544 nm, green), respectively. All of the luminescence resulted from an efficient energy transfer from the SrIn2O4 host lattice to the doped Dy3+, Pr3+, and Tb3+ ions, and the luminescence mechanisms have been proposed.

Spherical SiO2@GdPO4 : Eu3+ core-shell phosphors: Sol-gel synthesis and characterization

Nanocrystalline GdPO4 : Eu3+ phosphor layers were coated on non-aggregated, monodisperse and spherical SiO2 particles by Pechini sol-gel method, resulting in the formation of core-shell structured SiO2@GdPO4 : Eu3+ particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), time-resolved PL spectra and lifetimes were used to characterize the core-shell structured materials. Both XRD and FT IR results indicate that GdPO4 layers have been successfully coated on the SiO2 particles, which can be further verified by the images of FESEM and TEM. Under UV light excitation, the SiO2@GdPO4: Eu3+ phosphors show orange-red luminescence with Eu(3+)sD(0)-F-7(1) (593 nm) as the most prominent group. The PL excitation and emission spectra suggest that an energy transfer occurs from Gd3+ to Eu3+ in SiO2@GdPO4: Eu3+ phosphors. The obtained core-shell phosphors have potential applications in FED and PDP devices.

Synthesis and characterization of monodisperse spherical core-shell structured SiO2@Y3Al5O12 : Ce3+/Tb3+ phosphors for field emission displays

Nanocrystalline Y3Al5O12: Ce3+/Tb3+ ( average crystalline size 30 nm) phosphor layers were coated on non-aggregated, monodisperse and spherical SiO2 particles by the sol-gel method, resulting in the formation of core-shell structured SiO2@Y3Al5O12:Ce3+/Tb3+ particles. X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, photoluminescence, cathodoluminescence spectra, as well as lifetimes were utilized to characterize the core-shell structured SiO2@Y3Al5O12: Ce3+/Tb3+ phosphor particles. The obtained core-shell structured phosphors consist of well-dispersed submicron spherical particles with a narrow size distribution. The thickness of the Y3Al5O12:Ce3+/Tb3+ shells on the SiO2 cores ( average size about 500 nm, crystalline size about 30 nm) could be easily tailored by varying the number of deposition cycles (100 nm for four deposition cycles). Under the excitation of ultraviolet and low-voltage electron beams (1-3 kV), the core-shell SiO2@Y3Al5O12:Ce3+/ Tb3+ particles show strong yellow-green and green emission corresponding to the 5d-4f emission of Ce3+ and D-5(4)-F-7(J) ( J = 6, 5, 4, 3) emission of Tb3+, respectively.

Host-sensitized luminescence of Dy3+, Pr3+ , Tb3+ in polycrystalline CaIn2O4 for field emission displays

Caln(2)O(4):Dy3+/Pr3+/Tb3+ blue-white/green/green phosphors were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), diffuse reflectance, photoluminescence (PL) and cathodoluminescencc (CL) spectra as well as lifetimes were utilized to characterize the samples. The XRD results reveal that the samples begin to crystallize at 800 degrees C 3-1 and pure CaIn2O4 phase can be obtained after annealing at 900 degrees C. The FE-SEM images indicate that the CaIn2O4:Dy3+, CaIn2O4:Pr3+ and CaIn2O4:Tb3+ samples consist of spherical grains with size around 200-400nm. Under the excitation of ultraviolet light and low electron beams (1-5kV), the CaIn2O4:Dy3+, CaIn2O4:Pr3+ and CaIn2O4:Tb3+ phosphors show the characteristic emissions of Dy3+ ((F9/2-H15/2)-F-4-H-6 and (F9/2-H13/2)-F-4-H-6 transitions, blue-white), Pr3+ ((P0-H4)-P-3-H-3, (D2-H4)-D-1-H-3 and (P1-H5)-P-3-H-3 transitions, green) and Tb3+ ((D4-F6,5,4,3)-D-5-F-7 transitions, green), respectively. All the luminescence is resulted from an efficient energy transfer from the CaIn2O4 host lattice to the doped Dy3+ ,Pr3+ and Tb3+ ions, and the corresponding luminescence mechanisms have been proposed.

Sol-gel deposition and luminescence properties of LiYF4 : Tb3+ thin films

Tb3+-doped LiYF4 films were deposited on quartz glass by a simple sol-gel method. X-ray diffraction (XRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), photoluminescence spectra, and lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 300 degrees C and fully crystallized at 400 degrees C. AFM and FESEM images of singly coated LiY0.95Tb0.05F4 annealed at 400 degrees C indicated that the film is uniform and crack-free films with average grain size of 90 nm, root mean square roughness of 11 nm and thickness of 120 nm. The doped Tb3+ ions showed its characteristic emission in crystalline LiYF4 films, i.e., D-5(3), F--7(4)J (J = 6, 5, 4, 3) emissions. The optimum doping concentration of the Tb3+ was determined to be 5.0 mol% of Y3+ in LiYF4 films.

Pechini sol-gel deposition and luminescent properties of SrLa1-xRExGa3O7 (RE = Eu, Tb) phosphor films

SrLa1-xRExGa3O7 (RE = EU3+, Tb3+) phosphor films were deposited on quartz glass substrates by a simple Pechim sol-gel method. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy, field-emission scanning electron microscopy, photoluminescence spectra, and lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 700 degrees C and crystallized fully at 900 degrees C. The results of FNR spectra were in agreement with those of XRD. Uniform and crack-free films annealed at 900 degrees C were obtained with average grain size of 80 nm, root mean square roughness of 46 nm and thickness of 130 nm The RE ions showed their characteristic emission in crystalline SrLa1-xRExGa3O7 films, i.e., Eu3+ D-0-F-7(J) (J = 0, 1, 2, 3, 4), Tb3+5D4 -(7) F-J (J = 6, 5, 4, 3) emissions, respectively. The optimum concentrations (x) of Eu3+ and Tb3+ were determined to be 50, and 80 mol% in SrLa(1-x)RE(x)GGa(3)O(7) films, respectively.

Capillary electrophoresis coupled with electrochemiluminescence detection using porous etched joint

A new setup to couple capillary electrophoresis (CE) with electrochemiluminescence (ECL) detection is described in which the electrical connection of CE is achieved through a porous section at a distance of 7 mm from the CE capillary outlet. Because the porous capillary wall allowed the CE current to pass through and there was no electric field gradient beyond that section, the influence of CE high-voltage field on the ECL procedure was eliminated. The porous section formed by etching the capillary with hydrofluoric acid after only one side of the circumference of 2-3 mm of polyimide coating of the capillary was removed, while keeping the polyimide coating on the other part to protect the capillary from HF etching makes the capillary joint much more robust since only a part of the circumference of it is etched. A standard three-electrode configuration was used in experiments with Pt wire as a counter electrode, Ag/AgCl as a reference electrode, and a 300-mum diameter Pt disk as a working electrode. Compared with CE-ECL conventional decoupler designs, the present setup with a porous joint has no added dead volume created.

Short-capillary electrophoresis with electrochemiluminescence detection using porous etched joint for fast analysis of lidocaine and ofloxacin

Fast analysis of ofloxacin and lidocaine, as bactericide and analgesic or anesthetics, is of clinic importance for understanding the patient's medical process. This paper presented a high throughput, simple analysis method of lidocaine and ofloxacin by capillary electrophoresis coupled with electrochemiluminescence (ECL) using porous etched joint. To shorten the analysis time and to improve the analytical performance, a capillary with 10 cm in length was used as the separation channel. The cyclic voltammograms of Ru(bpy)(3)(2+) with different capillary length at same field strength showed that the porous etched joint eliminated the effect of electrophoretic current on the ECL detection. Following micro total analysis systems (muTAS), some advantages of which this approach has, the fabrication of channel in chip was not needed. Compared with capillary electrophoresis with 40-cm-long capillary, the high sample throughput and low zone broadening may be the main advantage of the present system. Under optimal condition, the detection limits of lidocaine and ofloxacin based on peak height were 3.0 x 10(-8) and 5.0 x 10(-7) mot L-1 and a 60 h(-1) of sampling frequency was obtained.

Determination of reserpine in urine by capillary electrophoresis with electrochemiluminescence detection

A fast and sensitive approach to detect reserpine in urine using micellar electrokinetic capillary chromatography with electrochemiluminescence (ECL) of Ru(bpy)(3)(2+) detection is described. Using a 25 mum i.d. capillary as separation column, the ECL detector was coupled to the capillary in the absence of an electric field decoupler. Field-amplified injection was used to minimize the effect of ionic strength in the sample and to achieve high sensitivity. In this way, the sample was analyzed directly without any pretreatment. The method was validated for reserpine in the urine over the range of 1 x 10(-6) - 1 x 10(-4) mol/L with a correlation coefficient of 0.996. The RSD for reserpine at a level of 5 mumol/L was 4.3%. The LOD (S/N = 3) was estimated to be 7.0 x 10(-8) mol/L. The average recoveries for 10 mumol/L reserpine spiked in human urine were 94%.

Sol-gel-derived BPO4/Ba2+ as a new efficient and environmentally-friendly bluish-white luminescent material

In this paper, BPO4 and Ba2+-doped BPO4 powder samples were prepared by the sol-gel process using glycerol and poly(ethylene glycol) as additives. The structure and optical properties of the resulting samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), diffuse reflection spectra, photoluminescence (PL) excitation and emission spectra, quantum yield, kinetic decay, and electron paramagnetic resonance (EPR), respectively. It was found that the undoped BPO4 showed a weak purple blue emission (409 nm, lifetime 6.4 ns) due to the carbon impurities involved in the host lattice. Doping Ba2+ into BPO4 resulted in oxygen-related defects as additional emission centers which enhanced the emission intensity greatly (> 10x) and shifted the emission to a longer-wavelength region (lambda(max) = 434 nm; chromaticity coordinates: x = 0.174, y = 0. 187) with a bluish-white color. The highest emission intensity was obtained ;when doping 6 mol % Ba2+ in BPO4, which has a quantum yield as high as 31%. The luminescent mechanisms of BPO4 and Ba2+-doped BPO4 were discussed in detail according to the existing models for silica-based materials.