Preparation, patterning and luminescent properties of nanocrystalline Gd2O3 : A (A = Eu3+, Dy3+, Sm3+, Er3+) phosphor films via Pechini sol-gel soft lithography

Nanocrystalline Gd2O3:A (A = Eu3+, Dy3+, Sm3+, Er3+) phosphor films and their patterning were fabricated by a Pechini sol-gel process combined with a soft lithography. X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and optical microscopy, UV/vis transmission and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 500 degreesC and that the crystallinity increased with the elevation of annealing temperatures. Uniform and crack free non-patterned phosphor films were obtained by optimizing the composition of the coating sol, which mainly consisted of grains with an average size of 70 nm and a thickness of 550 nm. Using micro-molding in capillaries technique, we obtained homogeneous and defects-free patterned gel and crystalline phosphor films with different stripe widths (5, 10, 20 and 50 mum). Significant shrinkage (50%) was observed in the patterned films during the heat treatment process. The doped rare earth ions (A) showed their characteristic emission in crystalline Gd2O3 phosphor films due to an efficient energy transfer from Gd2O3 host to them. Both the lifetimes and PL intensity of the rare earth ions increased with increasing the annealing temperature from 500 to 900 degreesC, and the optimum concentrations for Eu3+, Dy3+, sm(3+), Er3+ were determined to be 5, 0.25, 1 and 1.5 mol% of Gd3+ in Gd2O3 films, respectively.

Fabrication, patterning, and optical properties of nanocrystalline YVO4 : A (A = Eu3+, Dy3+, Sm3+, Er3+) phosphor films via sol-gel soft lithography

Nanocrystalline YVO4:A (A = Eu3+, Dy3+, Sm3+, Er3+) phosphor films and their patterning were fabricated by a Pechini sol-gel process combined with soft lithography. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), atomic force microscopy (AFM) and optical microscopy, UV/vis transmission and absorption spectra, photoluminescence (PL) spectra, and lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 400 degreesC and the crystallinity increased with the increase of annealing temperatures. Transparent nonpatterned phosphor films were uniform and crack-free, which mainly consisted of grains with an average size of 90 nm. Patterned gel and crystalline phosphor film bands with different widths (5-60 mum) were obtained. Significant shrinkage and a few defects were observed in the patterned films during the heat treatment process. The doped rare earth ions (A) showed their characteristic emission in crystalline YVO4 phosphor films because of an efficient energy transfer from vanadate groups to them. The Sm3+ and Er3+ ions also showed upconversion luminescence in a YVO4 film host. Both the lifetimes and PL intensity of the rare earth ions increased with increasing annealing temperature from 400 to 800 degreesC, and the optimum concentration for Eu3+ was determined to be 7 mol % and those for Dy3+, Sm3-, and Er3+ were 2 Mol % of Y3- in YVO4 films, respectively.

Sol-ogel deposition and luminescence properties of lanthanide ion-doped Y2(1-x)Gd2xSiWO8 (0 <= x <= 1) phosphor films

Y2(1-x) Gd2xSiWO8 : A ( 0 <= x <= 1; A= Eu3+, Dy3+, Sm3+, Er3+) phosphor films have been prepared on silica glass substrates through the sol - gel dip-coating process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), atomic force microscope (AFM), scanning electron microscopy (SEM) and photoluminescence spectra as well as lifetimes were used to characterize the resulting films. The results of the XRD indicated that the films began to crystallize at 800 degrees C and crystallized completely at 1000 degrees C. The AFM and SEM study revealed that the phosphor films, which mainly consisted of closely packed grains with an average size of 90 - 120 nm with a thickness of 660 nm, were uniform and crack free. Owing to an efficient energy transfer from the WO42- groups to the activators, the doped lanthanide ion ( A) showed its characteristic f - f transition emissions in crystalline Y2(1-x) Gd2xSiWO8 (0 <= x <= 1) films. The optimum concentrations for Eu3+, Dy3+, Sm3+, Er3+ were determined to be 21, 5, 3 and 7 mol% of Y3+ in Y2SiWO8 films, respectively.

Preparation, patterning and luminescence properties of rare earth-doped YVO4 nanocrystalline phosphor films via sol-gel soft lithography

In this presentation, nanocrystalline YVO4:A (A=Eu3+, Dy3+, SM3+, Er3+) phosphor films and their patterning were fabricated by a Pechini sol-gel process combined with a soft lithography (micro-molding in capillaries). XRD, FT-IR, AFM and optical microscope, absorption spectra, photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 400 degrees C and the crystallinity increased with the increase of annealing temperatures. Transparent nonpattemed phosphor films were uniform and crack free, which mainly consisted of grains with an average size of 90nm. Patterned crystalline phosphor film bands with different widths (5-30 mu m) were obtained. The doped rare earth ions (A) showed their characteristic emission in crystalline YVO4 phosphor films due to an efficient energy transfer from vanadate groups to them. The Sm3+ and Er3+ ions also showed upconversion luminescence in YVO4 film host. The optimum concentration for Eu3+ was determined to be 7 mol% and those for Dy3+, Sm3+, Er3+ were 2 Mol% of Y3+ in YVO4 films, respectively.

Luminescent properties of rare-earth-doped CaWO4 phosphor films prepared by the Pechini sol-gel process

CaWO4 phosphor films doped with rare-earth ions (Eu3+, Dy-,(3+) Sm3+, Er3+) were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, thermogravimetric and differential thermal analysis, atomic force microscopy, and photoluminescence spectra, as well as lifetimes, were used to characterize the resulting powders and films. The results of the XRD analysis indicated that the films began to crystallize at 400degreesC and that the crystallinity increased with elevation of the annealing temperature. The doped rare-earth ions showed their characteristic emissions in crystalline CaWO4 phosphor films due to energy transfer from WO42- groups to them. Both the lifetimes and PL intensities of the doped rare-earth ions increased with increasing annealing temperature, from 500 to 900degreesC, and the optimum concentrations for Eu3+, Dy3+, Sm3+, Er3+ were determined as 30, 1.5, 1.5, 0.5 at.% of Ca2+ in CaWO4 films annealed at 900degreesC, respectively.

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.

Effects R3+ on the photoluminescent properties of Ca2R8(SiO4)(6)O-2 : A (R = Y, La, Gd; A= Eu3+, Tb3+) phosphor films prepared by the sol-gel process

Using CaCO3, metal oxides (all dissolved by nitric acid) and tetraethoxysilane Si(OC2H5)(4) (TEOS) as the main starting materials, Ca2R8(SiO4)(6)O-2:A (R = Y, La, Gd; A = EU3+, Tb3+) phosphor films have been dip-coated on quartz glass substrates through the sol-gel process. X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the 1000 degreesC annealed films are isomorphous and crystallize with the silicate oxyapatite structure. AFM and SEM studies revealed that the phosphor films consisted of homogeneous particles ranging from 30 to 90 nm, with an average thickness of 1.30 mum. The Eu3+ and Tb3+ show similar spectral properties independent of R 3, in the films due to their isomorphous crystal structures. However, both the emission intensity and lifetimes of Eu3+ and Tb3+ in Ca2R8(SiO4)(6)O-2 (R = Y, La, Gd) films decrease in the sequence of R = Gd > R = Y > R = La, which have been explained in accordance with the crystal structures.

Fabrication, patterning and luminescence properties of X-2-Y2SiO5 : A (A = Eu3+, Tb3+, Ce3+) phosphor films via sol-gel soft lithography

X-2-y(2)SiO(5):A (A = Eu3+, Tb3+, Ce3+) phosphor films and their patterning were fabricated by a sol-gel process combined with a soft lithography. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM), scanning electron microscopy (SEM) optical microscopy and photoluminescence (PL) were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 900 degreesC with X-1-Y2SiO5, which transformed completely to X-2-Y2SiO5 at 1250 degreesC. Patterned thin films with different band widths (5 pin spaced by 5 pm and 16 pm spaced by 24 pm) were obtained by a soft lithography technique (micromoulding in capillaries, MIMIC). The SEM and AFM study revealed that the nonpattemed phosphor films were uniform and crack free, and the films mainly consisted of closely packed grains with an average size of 350 run. The doped rare earth ions (A) showed their characteristic emissions in X-2-Y2SiO5 phosphor films, i.e., D-5(0)-F-7(J) (J = 0, 1, 2,3,4) for Eu3+, D-5(3), (4)-F-7(J) (J = 6, 5, 4, 3) for Tb3+ and 5d (D-2)-4f (F-2(2/5),(2/7)) for Ce3+, respectively. The optimum doping concentrations for EU3+, Tb3+ were determined to be 13 and 8 mol% of Y3+ in X-2-Y2SiO5 films, respectively.

Luminescent properties of Gd2Ti2O7 : Eu3+ phosphor films prepared by sol-gel process

Gd2Ti2O7: Eu3+ thin film phosphors were fabricated by a sol-gel process. X-ray diffraction (XRD), atomic force microscopy (AFM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 800 degreesC and the crystallinity increased with the elevation of annealing temperatures. Uniform and crack free phosphor films were obtained, which mainly consisted of grains with an average size of 70 nm. The doped Eu3+ showed orange-red emission in crystalline Gd2Ti2O7 phosphor films due to an energy transfer from Gd2Ti2O7 host to them. Both the lifetimes and PL intensity of the Eu3+ increased with increasing the annealing temperature from 800 to 1000 degreesC, and the optimum concentrations for Eu3+ were determined to be 9 at.%. of Gd3+ in Gd2Ti2O7 film host.

Preparation, patterning and luminescent properties of oxyapatite La-9.33(SiO6)(4)O-2 : A (A = Eu3+, Tb3+, Ce3+) phosphor films by sol-gel soft lithography

Silicate oxyapatite La-9.33 (SiO6)(4)O-2:A (A = Eu3+, Tb3+ and/or Ce3+) phosphor films and their patterning were fabricated by a sol-gel process combined with soft lithography. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, atomic force microscopy, optical microscopy and photoluminescence spectra, as well as lifetimes, were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 800degreesC and the crystallinity increased with the increase in annealing temperatures. Transparent nonpatterned phosphor films were uniform and crack-free, which mainly consisted of rodlike grains with a size between 150 and 210 nm. Patterned thin films with different bandwidths (20, 50 mum) were obtained by the micromoulding in capillaries technique. The doped rare earth ions (Eu3+, Tb3+ and Ce3+) showed their characteristic emission in crystalline La-9.33(SiO6)(4)O-2 phosphor films, i.e. Eu3+ D-5(0)-F-7(J) (J = 0, 1, 2, 3, 4), Tb3+ D-5(3,4)-F-7(J) (J = 3, 4, 5, 6) and Ce3+ 5d (D-2)-4f (F-2(2/5), F-2(2/7)) emissions, respectively. Both the lifetimes and PL intensity of the Eu3+, Tb3+ ions increased with increasing annealing temperature from 800 to 1100 degreesC, and the optimum concentrations for Eu3+, Tb3+ were determined to be 9 and 7 mol% of La3+ in La-9.33(SiO6)(4)O-2 films, respectively. An energy transfer from Ce3+ to Tb3+ was observed in the La-9.33(SiO6)(4)O-2:Ce, Tb phosphor films, and the energy transfer efficiency was estimated as a function of Tb3+ concentration.

Patterning and luminescent properties of nanocrystallineY(2)O(3): Eu3+ phosphor films by sol-gel soft lithography

Nanocrystalline Y2O3:Eu3+ phosphor films and their patterning were fabricated by a Pechini sol-gel process combined with a soft lithography. X-ray diffraction (XRD), thermogravimetric and differential thermal analysis (TG-DTA), atomic force microscopy (AFM), optical microscopy, UV/vis transmission and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 500 degreesC and the crystallinity increased with the elevation of annealing temperatures. Uniform and crack free non-patterned phosphor films were obtained, which mainly consisted of grains with an average size of 70 nm. Using micro-molding in capillaries technique, we obtained homogeneous and defects-free patterned gel and crystalline phosphor films with different stripe widths (5, 10, 20 and 50 mum). Significant shrinkage (50%) was observed in the patterned films during the heat treatment process. The doped Eu3+ showed its characteristic emission in crystalline Y2O3 phosphor films due to an efficient energy transfer from Y2O3 host to them. Both the lifetimes and PL intensity of the Eu3+ increased with increasing the annealing temperature from 500 to 900 degreesC, and the optimum concentrations for Eu3+ were determined to be 5 mol%.

Sol-gel derived silicate oxyapatite phosphor films doped with rare earth ions

Rare-earth (Eu3+, Tb3+)-doped Ca2Y8(SiO4)(6)O-2 luminescent thin films were dip-coated on silicon and quartz glass substrates through a sol-gel route. X-ray diffraction (XRD), scanning electron microscopy (SEM) and luminescence excitation and emission spectra as well as luminescence decays were used to characterize the resultant films. The results of XRD reveal that these films remain amorphous below 700 degreesC, begin to crystallize at 800 degreesC, and crystallize completely around 1000 degreesC with an oxyapatite structure. The grain structure of the film can be seen clearly from SEM micrographs, where particles with various shape and average size of 250 nm can be resolved. The Eu3+ and Tb3+ ions show their characteristic red (D-5(0)-F-7(2)) and green (D-5(4)-F-7(5)) emission in the films with a quenching concentration of 10 and 6 mol% (of Y3+), respectively. The lifetime of Eu-3divided by increases with the heat treatment temperature front 700 to 1100 degreesC.

Sol-gel deposition and luminescent properties of oxyapatite Ca-2(Y,Gd)(8)(SiO4)(6)O-2 phosphor films doped with rare earth and lead ions

Rare-earth and lead ions (Eu3+, Tb3+, Dy3+, Pb2+) doped Ca2Y8 (SiO4)(6)O-2 and Ca2Gd8(SiO4)(6)O-2 thin films have been dip- coated on silicon and quartz glass substrates through the sol- gel route. X- Ray diffraction (XRD), TG- DTA, scanning electron microscopy (SEM), atomic force microscopy (AFM), FT- IR and luminescence excitation and emission spectra as well as luminescence decays were used to characterize the resulting films. The results of XRD reveal that these films remain amorphous below 700 degreesC, begin to crystallize at 800 degreesC and crystallize completely around 1000 degreesC with an oxyapatite structure. The grain structure of the film can be seen clearly from SEM and AFM micrographs, where particles with various shapes and average size of 250 nm can be resolved. Eu3+ and Tb3+ show their characteristic red (D-5(0)-F-7(2)) and green (D-5(4) - F-7(5)) emission in the films with a quenching concentration of 10 and 6 mol% (of Y3+), respectively. The lifetime and emission intensity of Eu3+ increase with the temperature treatment from 700 to 1100 degreesC, while those of Tb3+ show a maximum at 800 degreesC. Energy transfer phenomena have been observed by activating the oxyapatite film host- lattice Ca2Gd8(SiO4)(6)O-2 with Tb3+ (Dy3+). In addition, Pb2+ can sensitize the Gd3+ sublattice in Ca2Gd8(SiO4)(6)O-2.

Multiform oxide optical materials via the versatile Pechini-type sol-gel process: Synthesis and characteristics

This feature article highlights work from the authors' laboratories on the various kinds of oxide optical materials, mainly luminescence and pigment materials with different forms (powder, core-shell structures, thin film and patterning) prepared by the Pechini-type sol-gel (PSG) process. The PSG process, which uses the common metal salts (nitrates, acetates, chlorides, etc.) as precursors and citric acid (CA) as chelating ligands of metal ions and polyhydroxy alcohol (such as ethylene glycol or poly ethylene glycol) as a cross-linking agent to form a polymeric resin on molecular level, reduces segregation of particular metal ions and ensures compositional homogeneity. This process can overcome most of the difficulties and disadvantages that frequently occur in the alkoxides based sol-gel process.

Sol-gel fabrication and photoluminescence properties of SiO2@Gd2O3 : Eu3+ core-shell particles

A uniform nanolayer of europium-doped Gd2O3 was coated on the surface of preformed submicron silica spheres by a Pechini sol-gel process. The resulted SiO2@Gd2O3:Eu3+ core-shell structured phosphors were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays. The XRD results show that the Gd2O3:Eu3+ layers start to crystallize on the SiO2 spheres after annealing at 400 degrees C and the crystallinity increases with raising the annealing temperature. The core-shell phosphors possess perfect spherical shape with narrow size distribution (average size: 640 nm) and non-agglomeration. The thickness of the Gd2O3:Eu3+ shells on the SiO2 cores can be adjusted by changing the deposition cycles (70 nm for three deposition cycles). Under short UV excitation, the obtained SiO2@Gd2O3:Eu3+ particles show a strong red emission with D-5(0)-F-7(2) (610 nm) of Eu3+ as the most prominent group.The PL intensity of Eu3+ increases with increasing the annealing temperature and the number of coating cycles.