The influence of optical bleaching on lifetimes and luminescence intensity in the slow component of optically stimulated luminescence of natural quartz from Nigeria

The intensity of optically stimulated luminescence may be decreased to a slow or medium component of its decay curve by optical bleaching, that is, by prolonged exposure of the luminescent sample to stimulating light. In this paper, we report on the influence of irradiation and measurement temperature on luminescence lifetimes as well as on the effect of measurement temperature on luminescence intensity in annealed natural quartz from Nigeria. Measurements were carried out in the slow component region using time-resolved optical stimulation at 470 nm on samples annealed at 500 and 600 °C. Luminescence lifetimes were determined from the resultant time-resolved luminescence spectra by analysing the portion of each spectrum after the stimulating light pulse of duration 11 μs. In preparatory tests, the influence of the duration of optical bleaching on lifetimes was investigated. It was found that lifetimes in samples annealed at 500 °C are independent of the duration of optical bleaching, whereas lifetimes in quartz annealed at 600 °C are affected, decreasing towards a constant value with duration of bleaching. Concerning measurements in the slow-component region, lifetimes were found to decrease with irradiation dose for samples annealed at either 500 or 600 °C. The temperature dependence of lifetimes in both sets of quartz is similar with lifetimes constant at about 36 μs between 20 and 120 °C, but decreasing consistently from then on to about 5 μs at 200 °C, the maximum measurement temperature used in experiments. The luminescence intensity was observed to typically go through a peak as the stimulation temperature was increased from 20 to 200 °C, following a brief initial decrease, a change better exemplified in the quartz annealed at 600 °C. The initial decrease in luminescence intensity is attributed to the dominance of optical stimulation over thermal stimulation. On the other hand, the subsequent change of luminescence intensity with temperature is discussed as evidence of thermal assistance to optical stimulation, initially with activation energy of 0.27±0.07 eV and of thermal quenching subsequently with activation energy equal to 0.93±0.23 eV for samples annealed at either 500 or 600 °C. The temperature dependence of lifetimes is explained as showing increased thermal effect on lifetimes with activation energy values within 0.83±0.01 eV. On the other hand, the influence of irradiation on lifetimes is accounted for in terms of an energy band model for quartz consisting of three luminescence centres and one non-radiative recombination centre.     

The influence of ingot annealing on the corrosion resistance of a PrFeCoBNbP alloy

The influence of the annealing time on the corrosion resistance of a Pr–Fe–Co–B–Nb alloy with the addition of 0.1 wt% P was investigated here using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The cast ingot alloys were annealed at 1100 °C for 10, 15 and 20 h. The specimens were immersed for 30 days in naturally aerated 0.02 M Na₂HPO₄ solution at room temperature, during which period the evolution of the electrochemical behavior was assessed using EIS. The results indicated that the corrosion resistance of the Pr₁₄Fe_balCo₁₆B₆Nb_0.1P_0.25 alloy was related to the annealing time and, hence, to its microstructure. Annealing at 1100 °C for 10 h was insufficient to eliminate the Fe- phase from the alloy microstructure, whereas annealing for 15 and 20 h removed an increasing amount of Fe- phase, thereby increasing the alloy's corrosion resistance.     

RF-sputtered CrB2 diffusion barrier for Ni/Au Ohmic contacts on p-CuCrO2

Ohmic contacts to p-type CuCrO₂ using Ni/Au/CrB₂/Ti/Au contact metallurgy are reported. The samples were annealed in the 200–700 °C range for 60 s in flowing oxygen ambient. A minimum specific contact resistance of 2 × 10⁻⁵ Ω cm² was obtained after annealing at 400 °C. Further increase in the annealing temperature (>400 °C) resulted in the degradation of contact resistance. Auger Electron Spectroscopy (AES) depth profiling showed that out-diffusion of Ti to the surface of the contact stacks was evident by 400 °C, followed by Cr at higher temperature. The CrB₂ diffusion barrier decreases the specific contact resistance by almost two orders of magnitude relative to Ni/Au alone.     

Temperature dependence of luminescence time-resolved spectra from quartz

Pulsed optical stimulation of luminescence has been used to study the thermal dependence of luminescence lifetimes in quartz over the temperature range 20–200°C. Time-resolved spectra for lifetime analysis were recorded from samples of quartz over a dynamic range of 64 μs following stimulation of luminescence by pulsed 525 nm green light emitting diodes (LEDs) using an 11 μs pulse and 12% duty cycle. It has been demonstrated that an increase in measurement temperature generally leads to a decrease in lifetimes from about 30 μs at 20°C to about 7 μs at 200°C. The form of the decrease is influenced by the initial optical or thermal pre-treatment of samples.     

New experimental evidence of the structural modification in single crystal Bi2Sr2CaCu2Oy by X-ray diffraction observation

The variations of the high angle 00 peak-shape by means of X-ray l scans of the 00l fundamental reflections were investigated in detail for a highly oriented Bi₂Sr₂CaCu₂O_y (Bi2212) crystal with sufficiently small intrinsic mosaicity and the same crystal annealed in air at 250, 300, 400, 600, and 750°C for 20 h in consequence. For the first time, we observed a new additional reflection almost overlapped original 00l fundamental reflection at annealing temperature below 400°C by X-ray diffraction measurement, which shows that there coexisted two sets of lattice periodicity in the c-direction of the annealed crystal. The new additional reflection appeared at 250°C and disappeared at 400°C. Its intensity was increased at 300°C. The measurements of the AC susceptibility, c-axis parameter and full width at half maximum (FWHM) of the 00 peaks showed that the new additional reflection was associated with the oxygen diffusion in CuO₂ planes and the changes of strain field. The results provide the new experimental evidence that the structural distortion is more sensitive to the oxygen diffusion in CuO₂ planes than to that in Bi–O layers.     

Defect versus nanocrystal luminescence emitted from room temperature and hot-implanted SiO2 layers

Silicon nanocrystals have been synthesized in SiO₂ matrix using Si ion implantation. Si ions were implanted into 300-nm-thick SiO₂ films grown on crystalline Si at energies of 30–55 keV, and with doses of 5×10¹⁵, 3×10¹⁶, and 1×10¹⁷ cm⁻². Implanted samples were subsequently annealed in an N₂ ambient at 500–1100°C during various periods. Photoluminescence spectra for the sample implanted with 1×10¹⁷ cm⁻² at 55 keV show that red luminescence (750 nm) related to Si-nanocrystals clearly increases with annealing temperature and time in intensity, and that weak orange luminescence (600 nm) is observed after annealing at low temperatures of 500°C and 800°C. The luminescence around 600 nm becomes very intense when a thin SiO₂ sample is implanted at a substrate temperature of 400°C with an energy of 30 keV and a low dose of 5×10¹⁵ cm⁻². It vanishes after annealing at 800°C for 30 min. We conclude that this luminescence observed around 600 nm is caused by some radiative defects formed in Si-implanted SiO₂.     

Soft X-ray emission study of thermally treated Ni(film)/4H–SiC(substrate) interface

Deposition of Ni as contact on 4H–SiC has been investigated. Ni/4H–SiC samples were annealed at temperatures of 600, 800 and 950 °C for 30 min and were non-destructively characterized by soft X-ray emission spectroscopy (SXES) using synchrotron radiation as excitation. Si L_2,3 SXE showed the formation of Ni₂Si for all annealing temperatures. The C K SXE indicated the formation of graphite and graphitic carbons at annealing temperatures of 950 °C and below 800 °C, respectively.     

TL and PTTL in natural fluorite previously irradiated with gamma rays and heavy ions

The effect of annealing temperature on the phototransfer thermoluminescence (PTTL) signal was studied to determine the appropriate annealing temperature for treating the natural powder before irradiation. The temperatures used to anneal virgin natural fluorite samples (only natural dose without giving the samples any artificial doses) were 150, 250, 350, 450, 550, 650 and 750°C for a duration of 1 h in each case. The results show that the PTTL response did not change for anneal temperatures up to 450°C, but at higher temperatures the signal decreased rapidly. The height of the 90°C peak decreased by two orders of magnitude as the anneal temperature increased from 450 to 750°C, whilst the height of the 180°C peak decreased by three orders of magnitude between the same two annealing temperatures. In order to investigate the effect of previous gamma rays and heavy ion irradiation on thermoluminescence (TL) and PTTL signals, powdered samples of natural fluorite from Cornwall, England, were annealed at 500°C and then irradiated (at GSI, Darmstadt, Germany) with ¹⁶¹Dy ions of energy 13 Mev/n; the range of fluences used was from 10⁴ to 10¹² ion cm⁻². Identical samples were given gamma doses in the range 1 Gy to 2.6 × 10⁴ Gy in order to compare the effects of gamma rays and heavy ions. The sensitivities of TL and PTTL were studied by giving the samples a gamma test dose of 1 Gy after annealing the samples at 500°C for 30 min in order to eliminate the TL resulting from previous gamma or heavy ion irradiation.     

Annealing effects on structure and laser-induced damage threshold of Ta2O5/SiO2 dielectric mirrors

The effects of annealing on structure and laser-induced damage threshold (LIDT) of Ta₂O₅/SiO₂ dielectric mirrors were investigated. Ta₂O₅/SiO₂ multilayer was prepared by ion beam sputtering (IBS), then annealed in air under the temperature from 100 to 400 °C. Microstructure of the samples was characterized by X-ray diffraction (XRD). Absorption of the multilayer was measured by surface thermal lensing (STL) technique. The laser-induced damage threshold was assessed using 1064 nm free pulsed laser at a pulse length of 220 μs.

It was found that the center wavelength shifted to long wavelength gradually as the annealing temperature increased, and kept its non-crystalline structure even after annealing. The absorbance of the reflectors decreased after annealing. A remarkable increase of the laser-induced damage threshold was found when the annealing temperature was above 250 °C.     

Superconductivity, Ca content and oxygen deficiency of Ga(Sr,Ca)2(Yb,Ca)Cu2O7

Superconducting transition temperature (T_c), Ca content and oxygen deficiency are studied on GaSr_1.8Ca_0.2Yb_1−xCa_xCu₂O₇ (x≤0.35). Superconducting samples with T_c=52 K are prepared after the annealing at 20 MPa of oxygen. The T_c is reduced through a slight oxygen loss accompanied by annealing in air above 650°C. The oxygen loss suggests the presence of short Cu–O chains in the GaO₄ slab. The formal valence of planar Cu required for the appearance of superconductivity depends on oxygen and Ca contents. The critical formal Cu valences are 2.105 and 2.125 for the samples annealed in air at 600°C and at 835°C, respectively. The values are higher than those of usual high-T_c superconductors. This can be explained by a high concentration of localized holes in the CuO₅ slab.     

The origin of photoluminescence in Ge-implanted SiO2 layers

Ge ions were implanted at 100 keV with 3×10¹⁶ cm⁻² into a 300  nm thick SiO₂ layer on Si. Visible photoluminescence (PL) around 2.1 eV from an as-implanted sample is observed, and faded out by subsequent annealing at 900°C for 2 h. However, PL shows up again after annealing above 900°C at the same peak position. Compared with the as-implanted sample, significant increase of Ge–Ge bonds is measured in X-ray photoelectron spectroscopy, and the formation of Ge nanocrystals with a diameter of 5 nm are observed in transmission electron microscopy from the sample annealed at 1100°C. We conclude that the PL peak from the sample annealed above 900°C is caused by the quantum confinement effects from Ge nanocrystals, while the luminescence from the as-implanted sample is due to some radiative defects formed by Ge implantation.     

Kinetics of isolated peak 5 in TLD-100 following 165°C post-irradiation annealing

Peak 5 in the glow curve of TLD-100 (at a temperature of approximately 200°C) was studied as a function of post-irradiation annealing at 165°C. Computerized glow peak analysis shows that the order of kinetics of peak 5 increases from 1.2 ± 0.05 (1 SD) following 165°C annealing for five minutes to 1.72 ± 0.07 (1 SD) following annealing at 165°C for thirty minutes. Extrapolation of the results to zero annealing time yields a value of kinetic order consistent with unity. The glow curve analysis also indicates that peak 4 (the satellite peak at approximately 175°C) is undetectable even at the lowest annealing duration of 5 minutes. The high temperature satellite of peak 5 (peak 6 at approximately 225°C) grows with increasing annealing time to 10% of the intensity of peak 5 after annealing for 30 min. Glow curve analysis including peak 6, however, does not significantly change the conclusions regarding the increase in the order of kinetics of peak 5 as a function of annealing time or the consistency of the extrapolated results with kinetic order unity at zero annealing time. Analysis of isothermal decay curves at 165°C shows that the relative intensity of peak 4 to peak 5 decreases with increasing annealing time, from 8% after 5 min annealing to 0.5% after 30 min annealing.     

Development of cube textured Ni–5 at.%W alloy substrates for coated conductor application using a melting process

Biaxially textured Ni–5 at.%W substrates have been prepared by cold rolling, followed by three different annealing routes. In this paper, the processes of melting Ni and W metals, flat rolling, various annealing methods are described in detail. The Ni–5 at.%W tapes annealed under either high vacuum or flowing Ar (7% H₂) gas were characterized by X-ray pole figures, ODF, EBSD as well as AFM analysis. The texture analysis indicated that as fabricated tapes have a sharp cube texture formed after annealing at a wide temperature range of 800–1100 °C. The high quality of cube orientation on tapes was obtained after a two-step annealing (TSA), where the percentage of the cube texture component was as high as 93.5% within a misorientation angle smaller than 8° from EBSD analysis. Furthermore, it was also observed that the number of twin boundaries in this tape decreased with respect to that of tapes annealed both in vacuum and one-step gas annealing. From AFM on 1 μm² areas, it was concluded that the roughness (RMS) on the tape surface reached 0.98 nm.     

Effect of Co layer thickness on structural and magnetic properties of C/Co/C films

Granular C/Co/C films have been prepared by magnetron sputtering from C and Co onto glass substrates at room temperature and subsequent in situ annealing. It has been found that the structure and magnetic properties of the C/Co/C films depend strongly on the Co layer thickness. Vibrating sample magnetometer measurements indicate that the in-plane coercivities reach maximum in 20 nm Co thickness of both as-deposited and annealed films. The squareness ratio of annealed films was more than 0.8. X-ray diffraction shows that majority Co nanograins are formed as the hexagonal-close-packed (HCP) structure in 20 nm Co thickness with annealing at 400 °C. Scanning probe microscope was used to scan surface morphology and magnetic domain structures. The values of the surface roughness were lower than 0.6 nm in all annealed samples. The average magnetic cluster size was estimated to be about 10 nm in annealed 20 nm Co thickness films.     

Enhanced magnetic properties of Nd–Fe–B thin films crystallized by heat treatment

Nd₂Fe₁₄B Φ phase crystallites were formed in Nd_16.7Fe_65.5B_17.8 thin films prepared by RF sputtering with subsequent heat treatment. The 2 μm-thick films were deposited onto 0.1 mm Mo sheets at an average substrate temperature (T_s) of 365°C. The enhanced magnetic properties of the magnetically anisotropic thin films were investigated using different heating rates (h_r) of 10°C, 20°C, 50°C and 100°C/min in an annealing experiment. Transformation from the amorphous phase to the crystalline phase is clearly manifested by the formation of fine crystallites embedded as a columnar matrix of Nd₂Fe₁₄B phase. High-resolution scanning electron microscope data of the cross-section of the annealed films show columnar stacking of Nd₂Fe₁₄B crystallites with sizes <500 nm. Transmission electron microscope observations revealed that the microstructure of these films having out-of-plane magnetization consists of uniformly distributed Φ phase with grain size around 400 nm together with small Nd rich particles. This grain size of Φ phase is comparable to the single domain particle diameter of Nd₂Fe₁₄B. Significant change in _iH_c, 4πM_r and 4πM_s with h_r was confirmed. Annealing conditions with a heating rate of 50°C/min to an annealing temperature (T_a) of 650°C for 30 min was consequently found to give optimum properties for the NdFeB thin films. The resulting magnetic properties, considered to be the effect of varying h_r were _iH_c= 1307–1357 kA/m, 4πM_r=0.78–1.06 T and 4πM_s=0.81–1.07 T.     

Ultrathin amorphous Ni-Ti film as diffusion barrier for Cu interconnection

5-nm-thick amorphous Ni-Ti films deposited on Si by magnetron sputtering, annealed at various temperatures in high vacuum, have been studied as diffusion barriers for Cu interconnection using X-ray diffraction, atomic force microscopy and four-probe methods. Although no Cu silicide peaks are found from X-ray diffraction patterns of the samples annealed up to 750 °C, it is found that the sheet resistance of Cu/Ni-Ti/Si decreases with the increase of annealing temperature and then slightly increases when the annealing temperature is higher than 700 °C. Root mean square roughness of Cu/Ni-Ti/Si increases with the increase of annealing temperature and many island-like grains present on the surface of the 750 °C annealed sample, which is ascribed to dewetting and agglomeration.     

Low-temperature ordering of L10 FePt phase in FePt thin film with AgCu underlayer

FePt (20 nm) films with AgCu (20 nm) underlayer were prepared on thermally oxidized Si (0 0 1) substrates at room temperature by using dc magnetron sputtering, and the films annealed at different temperature to examine the disorder–order transformation of the FePt films. It is found that the ordered L1₀ FePt phase can form at low annealing temperature. Even after annealing at 300 °C, the in-plane coercivity of 5.2 kOe can be obtained in the film. With increase in annealing temperature, both the ordering degree and coercivity of the films increase. The low-temperature ordering of the films may result from the dynamic stress produced by phase separation in AgCu underlayer and Cu diffusion into FePt phase during annealing.     

Structure and optical properties of sol–gel derived Gd2O3 waveguide films

Pure and rare earth doped gadolinium oxide (Gd₂O₃) waveguide films were prepared by a simple sol–gel process and dip-coating method. Gd₂O₃ was successfully synthesized by hydrolysis of gadolinium acetate. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were used to study the thermal chemistry properties of dried gel. Structure of Gd₂O₃ films annealed at different temperature ranging from 400 to 750 °C were investigated by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that Gd₂O₃ starts crystallizing at about 400 °C and the crystallite size increases with annealing temperature. Oriented growth of (4 0 0) face of Gd₂O₃ has been observed when the films were deposited on (1 0 0) Si substrate and annealed at 750 °C. The laser beam (λ=632.8 nm) was coupled into the film by a prism coupler and propagation loss of the film measured by scattering-detection method is about 2 dB/cm. Luminescence properties of europium ions doped films were measured and are discussed.     

Structural evolution of Co clusters on Cu90Co10 upon annealing

A granular alloy, composed of cobalt embedded in a copper matrix, was studied by using EXAFS and magnetotransport measurements as function of annealing parameters (temperature and annealing time). The results suggest that different annealing routes can reach the same final state. For annealing temperatures up to 450°C, the results indicate the coalescence of cobalt atoms, resulting in magnetic particles with increasing size. On the other hand, the annealing at 500°C shows a rapid formation of cobalt particles and then the re-dissolution of cobalt atoms in the copper matrix.     

Effects of annealing temperature on YAG:Ce synthesized by spray-drying method

In this report, YAG:Ce phosphors were synthesized by spray-drying method. The effects of annealing temperature on crystal structure, morphology and photoluminescence property (PL) of as-prepared samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and spectrofluorometer, respectively. The XRD patterns showed all the samples are in consistence with a single garnet phase, and the location of strongest peak shifts to smaller angle with increasing the annealing temperature. The SEM micrographs revealed the sample annealed at 1200 °C appears to be a spherical polycrystalline aggregate; as the samples were annealed at 1300?1400 °C, spherical grains obviously grow up; but the sample annealed at over 1400 °C forms an irregular bulk. The emission spectra of samples indicated the PL of samples annealed at 1200?1400 °C improve with increasing the annealing temperature because of the diffusion of Si⁴⁺ ions; whereas the PL of sample annealed at the temperature over 1400 °C decreases likely resulting from inflection effects of multiangular shape of grains. Therefore, the samples annealed at 1400 °C are suitable for gaining phosphor with high brightness and good morphology.