RESUMO
We described the novel nanocomposite of silver doped ZrO2 combined graphene-based mesoporous silica (ZrO2-Ag-G-SiO2,) in bases of low-cost and self-assembly strategy. Synthesized ZrO2-Ag-G-SiO2 were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, Nitrogen adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS), and Diffuse Reflectance Spectroscopy (DRS). The ZrO2-Ag-G-SiO2 as an enzyme-free glucose sensor active material toward coordinate electro-oxidation of glucose was considered through cyclic voltammetry in significant electrolytes, such as phosphate buffer (PBS) at pH 7.4 and commercial urine. Utilizing ZrO2-Ag-G-SiO2, glucose detecting may well be finished with effective electrocatalytic performance toward organically important concentrations with the current reaction of 9.0 × 10-3 mAcm-2 and 0.05 mmol/L at the lowest potential of +0.2 V, thus fulfilling the elemental prerequisites for glucose detecting within the urine. Likewise, the ZrO2-Ag-G-SiO2 electrode can be worked for glucose detecting within the interferometer substances (e.g., ascorbic corrosive, lactose, fructose, and starch) in urine at proper pH conditions. Our results highlight the potential usages for qualitative and quantitative electrochemical investigation of glucose through the ZrO2-Ag-G-SiO2 sensor for glucose detecting within the urine concentration.
RESUMO
A set of new triple molybdates, LixNa1-xCaGd0.5(MoO4)3:Ho3+0.05/Yb3+0.45, was successfully manufactured by the microwave-accompanied sol-gel-based process (MAS). Yellow molybdate phosphors LixNa1-xCaGd0.5(MoO4)3:Ho3+0.05/Yb3+0.45 with variation of the LixNa1-x (x = 0, 0.05, 0.1, 0.2, 0.3) ratio under constant doping amounts of Ho3+ = 0.05 and Yb3+ = 0.45 were obtained, and the effect of Li+ on their spectroscopic features was investigated. The crystal structures of LixNa1-xCaGd0.5(MoO4)3:Ho3+0.05/Yb3+0.45 (x = 0, 0.05, 0.1, 0.2, 0.3) at room temperature were determined in space group I41/a by Rietveld analysis. Pure NaCaGd0.5Ho0.05Yb0.45(MoO4)3 has a scheelite-type structure with cell parameters a = 5.2077 (2) and c = 11.3657 (5) Å, V = 308.24 (3) Å3, Z = 4. In Li-doped samples, big cation sites are occupied by a mixture of (Li,Na,Gd,Ho,Yb) ions, and this provides a linear cell volume decrease with increasing Li doping level. The evaluated upconversion (UC) behavior and Raman spectroscopic results of the phosphors are discussed in detail. Under excitation at 980 nm, the phosphors provide yellow color emission based on the 5S2/5F4 â 5I8 green emission and the 5F5 â 5I8 red emission. The incorporated Li+ ions gave rise to local symmetry distortion (LSD) around the cations in the substituted crystalline structure by the Ho3+ and Yb3+ ions, and they further affected the UC transition probabilities in triple molybdates LixNa1-xCaGd0.5(MoO4)3:Ho3+0.05/Yb3+0.45. The complex UC intensity dependence on the Li content is explained by the specificity of unit cell distortion in a disordered large ion system within the scheelite crystal structure. The Raman spectra of LixNa1-xCaGd0.5(MoO4)3 doped with Ho3+ and Yb3+ ions were totally superimposed with the luminescence signal of Ho3+ ions in the range of Mo-O stretching vibrations, and increasing the Li+ content resulted in a change in the Ho3+ multiplet intensity. The individual chromaticity points (ICP) for the LiNaCaGd(MoO4)3:Ho3+,Yb3+ phosphors correspond to the equal-energy point in the standard CIE (Commission Internationale de L'Eclairage) coordinates.
RESUMO
Triple molybdate NaCaLa(1-x-y)(MoO4)3:xEr3+,yYb3+ (x = y = 0, x = 0.05 and y = 0.45, x = 0.1 and y = 0.2, x = 0.2 and y = 0) phosphors were successfully synthesized for the first time by the microwave sol-gel method. Well-crystallized particles formed after heat treatment at 900 °C for 16 h showed a fine and homogeneous morphology with particle sizes of 2-3 µm. The structures were refined by the Rietveld method in the space group I41/a. The optical properties were examined comparatively using photoluminescence emission and Raman spectroscopy. Under excitation at 980 nm, the NaCaLa0.7(MoO4)3:0.1Er3+,0.2Yb3+ and NaCaLa0.5(MoO4)3:0.05Er3+,0.45Yb3+ particles exhibited a strong 525 nm emission band, a weaker 550 nm emission band in the green region, and three weak 655 nm, 490 nm and 410 nm emission bands in the red, blue and violet regions. The pump power dependence and Commission Internationale de L'Eclairage chromaticity of the upconversion emission intensity were evaluated in detail.
RESUMO
CaLa2-x(MoO4)4:Ho(3+)/Yb(3+) phosphors with the doping concentrations of Ho(3+) and Yb(3+) (x = Ho(3+) + Yb(3+), Ho(3+) = 0.05; Yb(3+) = 0.35, 0.40, 0.45 and 0.50) have been successfully synthesized by the microwave sol-gel method. The modulated and averaged crystal structures of CaLa2-x(MoO4)4:Ho(3+)/Yb(3+) molybdates have been found by the Rietveld method, and the upconversion photoluminescence properties have been investigated. The synthesized particles, being formed after the heat-treatment at 900 °C for 16 h, showed a highly crystallized state. Under the excitation at 980 nm, CaLa2-x(MoO4)4:Ho(3+)/Yb(3+) particles exhibited strong 545 and 655 nm emission bands in the green and red regions. When the Yb(3+) : Ho(3+) ratios are 9 : 1 and 10 : 1, the UC intensity of CaLa1.5(MoO4)4:Yb0.45/Ho0.05 and CaLa1.45(MoO4)4:Yb0.50/Ho0.05 particles is the highest for different bands. The CIE coordinates calculated for CaLa2-x(MoO4)4:Ho(3+)/Yb(3+) phosphors are related to the yellow color field. The Raman spectrum of undoped CaLa2(MoO4)4 has revealed about 13 narrow lines. The strongest band observed at 906 cm(-1) was assigned to the ν1 symmetric stretching vibration of MoO4 tetrahedra. The spectra of the samples doped with Ho and Yb, as obtained under the 514.5 nm excitation, were dominated by Ho(3+) luminescence over the wavenumber range of >700 cm(-1) preventing the recording of the Raman spectra.
