A powder diffraction method was applied to the quantitative analysis of amorphous silica in several quartz powders. Two calibration methods, i.e., direct analysis and the standard addition method were examined. Calibration mixtures were made by mixing a standard silica gel powder ground to under 5 μm particle size with a matrix quartz powder which was ground to 10 to 40 μm particle size and treated with NaOH solution to remove the amorphous phase caused by grinding. Intensity of the amorphous halo was measured at 23.0° 2θ, and the background intensity at 53.0° 2θ was subtracted. Linear calibration curves were obtained over the ranges of 0 to 50 wt% by direct analysis and 0 to 20 wt% by standard addition methods, respectively. The analytical results obtained by the two calibration methods were in good agreement with each other. The relative standard deviations for 4.3 wt% of amorphous silica were 4.6% by the direct analysis and 5.4% by the standard addition method. These methods were successfully applied to a correction of reference intensity ratios (RIR) for several quartz powders containing amorphous silica. After the correction for amorphous content, the relative standard deviations of the RIR values for quartz powders became smaller.
(Pb, La)(Zr, Ti)O3 (PLZT) thin films were deposited on 6-inch Pt/Ti/SiO2/Si substrates by rf magnetron sputtering using a multichamber production system. The Pb content in PLZT films deposited at low temperature was measured by inductively coupled plasma (ICP) spectroscopy, and the structural properties of crystallized PLZT films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). A novel method for Pb content control was developed and it was found that Pb content in PLZT film could be changed by changing the electric potential of the substrate. For ferroelectric properties, only small differences were observed between the rapid thermally annealed PLZT film and furnace- annealed ones. Good uniformities of film thickness, Pb content and remanent polarization were achieved on 6-inch wafers.
Surface morphology of lead-zirconate-titanate [PZT(52/48)] thin films prepared by sol-gel processing on Pt/Ti/ SiO2/Si substrates was studied. When the atomic ratio [Pb/(Zr+Ti)] of PZT gel films was 1, rosette structure was observed in the films after annealing at 600° C for one hour. The crystal structure of the rosette was identified as perovskite and that of the other area was nonperovskite, by electron diffraction analysis. Lead deficiency in the non-perovskite phase caused by lead diffusion into the bottom electrode was detected by energy dispersive X-ray spectroscopy and Auger electron spectroscopy. In order to prepare PZT films with a smooth surface, the following four means were efficient: addition of lead excess, rapid thermal annealing (RTA), adoption of buffer layer, and preparation of crystal nucleus on the substrate.
The photo sensitivity of sol-gel solution of PbZr
x
Ti1-x
O3 (PZT) was studied. A coated film of the sol-gel solution on Pt/Ti/SiO2/Si substrates was exposed to an excimer laser and developed with water. The film was finally annealed at 700°C for 60 s by rapid thermal annealing (RTA). Ferroelectric perovskite phase was observed in the PZT thin films. The 130-nm-thick film showed P
r of 11.2 µ C/cm2 and E
c of 93.8 kV/cm. From this process, half-micron patterns of PZT films were obtained.
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