Improvement of optical properties of Nd:YAG transparent ceramics by post-annealing and post hot isostatic pressing

The Nd:YAG transparent ceramics were fabricated by vacuum sintering. The Nd:YAG samples were annealed at 1450 °C for 20 h in air and followed by hot isostatic pressing (HIP) at 1700 °C for 2 h in 200 MPa Ar and then re-annealed at 1250–1450 °C for 10 h in air. The experimental results showed that the optical properties of Nd:YAG samples varied markedly with different post treatments. After air annealing at 1450 °C for 20 h and HIP at 1700 °C for 2 h under 200 MPa of Ar and then air re-annealing at 1250 °C for 10 h, the transmittances of the samples increased from 51.2% to 77.2% (at 400 nm) and 78.4% to 83.6% (at 1064 nm), respectively. The annealing and HIP are effective post treatments to reduce oxygen vacancies and intergranular pores respectively in Nd:YAG transparent ceramics.     

Mechanism of nanostructure bredigite formation by mechanical activation with thermal treatment

This paper reports the successful synthesis of nanostructure bredigite powder by mechanical activation with subsequent annealing. Talc, calcium carbonate, and amorphous silica were used as initial reactants. The initial materials were milled for various times and then annealed in order to obtain single-phase nanostructure bredigite powder. The results showed that during the formation of bredigite powder some intermediate compounds such as wollastonite and larnite were formed. Single-phase nanostructure bredigite powder was synthesized by 10–60 h of mechanical activation with subsequent annealing at 1200 °C for 1 h. The bredigite powder obtained after 60 h milling and subsequent annealing at 1200 °C for 1 h had a mean crystallite size of about 50 nm and mean particle size of about 779 nm.     

Annealing effect on the microstructure and photoluminescence of ZnO thin films

Zinc oxide thin films have been obtained by pulsed laser ablation of a ZnO target in O₂ ambient at a pressure of 0.13 Pa using a pulsed Nd:YAG laser. ZnO thin films deposited on Si (1 1 1) substrates were treated at annealing temperatures from 400 °C up to 800 °C after deposition. The structural and optical properties of deposited thin films have been characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, photoluminescence spectra, resistivity and IR absorption spectra. The results show that the obtained thin films possess good single crystalline with hexagonal structure at annealing temperature 600 °C. Two emission peaks have been observed in photoluminescence spectra. As the post-annealing temperature increase, the UV emission peaks at 368 nm is improved and the intensity of blue emission at 462 nm decreases, which corresponds to the increasing of the optical quality of ZnO film and the decreasing of Zn interstitial defect, respectively. The best optical quality for ZnO thin films emerge at post-annealing temperature 600 °C in our experiment. The measurement of resistivity also proves the decrease of defects of ZnO films. The IR absorption spectra of sample show the typical Zn–O bond bending vibration absorption at wavenumber 418 cm⁻¹.     

Influence of thermal annealing on optical properties and structure of aluminium oxide thin films by filtered cathodic vacuum arc

Optical and structural properties of aluminium oxide thin films are investigated in the annealing temperature range of 200–900 °C. The changes in optical properties and film structure show the great dependence on the temperature. For the film annealed at low temperatures (from 200 °C to 600 °C), the film optical properties, such as transmittance and optical constants, could be improved by thermal annealing with amorphous structure and smooth surface. However, for the film annealed at higher temperature (e.g. 900 °C), the poor performance of optical properties indicates undesirable application for precise use in optics due to significant changes in both structure and surface roughness. At optimum annealing temperature of 600 °C, the transmittance could reach as high as that of substrate and the film possesses better optical constants (refractive index was 1.73 and extinction coefficient was ∼10⁻⁴ at 550 nm) with remaining amorphous structure and smooth surface.     

Synthesis,mechanical properties and bioactivity of nanostructured zirconia

Yttria stabilized zirconia 3Y – TZP nanopowders (10–30 nm) are prepared through direct precursor calcination of mixed zirconium oxychloride and yttrium nitrate solutions at 600 °C for 2 h. Cuboid(50 × 25 × 20 mm³) zirconia blanks are fabricated through centrifuge casting and followed by sintering at 1350 °C for 2 h. Sintered zirconia blanks exhibit 24% volume shrinkage and 98% relative density with average grain size of 250 nm. Vickers hardness and indented fracture toughness of sintered blanks are measured as 13.5 GPa and 3.5 MPa.m^1/2, respectively. Bioactivity of nanostructured zirconia originates after four weeks incubation in simulated body fluid solution. An optimum time is required for the deposition of hydroxyapatite nanoparticles on stress-induced nucleation site of nanostructured zirconia.     

Photoluminescence and thermoluminescence studies of Tb3+ doped ZnO nanorods

Here in, the synthesis of the terbium doped zinc oxide (ZnO:Tb³⁺) nanorods via room temperature chemical co-precipitation was explored and their structural, photoluminescence (PL) and thermoluminescence (TL) studies were investigated in detail. The present samples were found to have pure hexagonal wurtzite crystal structure. The as obtained samples were broadly composed of nanoflakes while the highly crystalline nanorods have been formed due to low temperature annealing of the as synthesized samples. The diameters of the nanoflakes are found to be in the range 50–60 nm whereas the nanorods have diameter 60–90 nm and length 700–900 nm. FTIR study shows ZnO stretching band at 475 cm^?1 showing improved crystal quality with annealing. The bands at 1545 and 1431 cm^?1 are attributed to asymmetric and symmetric CO stretching vibration modes. The diffuse reflectance spectra show band edge emission near 390 nm and a blue shift of the absorption edge with higher concentration of Tb doping. The PL spectra of the Tb³⁺-doped sample exhibited bright bluish green and green emissions at 490 nm (⁵D₄ → ⁷F₆) and 544 nm (⁵D₄ → ⁷F₅) respectively which is much more intense then the blue (450 nm), bluish green (472 nm) and broad green emission (532 nm) for the undoped sample. An efficient energy transfer process from ZnO host to Tb³⁺ is observed in PL emission and excitation spectra of Tb³⁺-doped ZnO ions. The doped sample exhibits a strong TL glow peak at 255 °C compared to the prominent glow peak at 190 °C for the undoped sample. The higher temperature peaks are found to obey first order kinetics whereas the lower temperature peaks obey 2nd order kinetics. The glow peak at 255 °C for the Tb³⁺ doped sample has an activation energy 0.98 eV and frequency factor 2.77 × 10⁸ s^?1.     

Spectroscopic characterizations of Er doped LaPO4 submicron phosphors prepared by homogeneous precipitation method

Hexagonal shaped LaPO₄ submicron particles doped with various concentrations of Er were successfully prepared by homogenous precipitation method using metal nitrates and ammonium phosphate. Particles of approximate particle size 125 nm and size distribution of 85 nm are obtained with good crystallinity. After heat treatment at 1200 °C for 2 h, the particles are characterized for their various optical properties such as absorption, emission, fluorescence decay and optical band gap. Optical absorption and emission data are numerically analyzed with the help of Judd–Ofelt model to evaluate various radiative spectral properties such as radiative decay rates, radiative quantum yield, emission cross-section and fluorescence branching ratios of various emission transitions. Though the radiative quantum yield of 1554 nm emission approaches the theoretical limit of 100%, the experimentally measured quantum yield is only 11% at 12 W/cm² at 980 nm excitation power density in 2% Er doped LaPO₄.     

Formation of nanotubes in Cz Si wafers using He+ implantation and subsequent O+- or N+-plasma treatment

Standard 4.5 Ω cm n-type and 12 Ω cm p-type Cz Si wafers were implanted with helium ions of 300 keV energy and the fluences of 1 × 10¹⁵, 5 × 10¹⁵, 1 × 10¹⁶ or 2 × 10¹⁶ at/cm² at room temperature. The implanted wafers were then annealed in vacuum at 650, 700, 750 or 800 °C. Then oxygen or nitrogen ions of the fluence of 2 × 10¹⁷ cm^?2 were introduced to the silicon wafers from a plasma source followed by annealing the samples in vacuum at 900 °C.The structural properties of the samples were investigated using SEM. To control the treatment's influence on the electrical properties of the wafers, the measurements of charge carriers' lifetime were carried out.1D defects (nanotubes) normal to the sample surface with defect's length equal to the projected range of the implanted ions were formed in the Cz Si wafers following He⁺ implantation with subsequent vacuum annealing and plasma treatment. The surfaces of wafers contained a small density of defects.     

Synthesis and photoluminescence study of La1.8Eu0.2O3 coating on nanometric α-Al2O3

In this work the La_1.8Eu_0.2O₃ coating on nanometric alpha-alumina, α-Al₂O₃@La_1.8Eu_0.2O₃, was prepared for the first time by a soft chemical method. The powder was heat-treated at 100, 400, 800 and 1200 °C for 2 h. X-ray powder diffraction patterns (XRD), transmission electronic microscopy (TEM), emission and excitation spectra, as well as Eu³⁺ lifetime were used to characterize the material and to follow the changes in structure as the heating temperature increases. The Eu³⁺ luminescence data revealed the characteristic transitions ⁵D₀ → ⁷F_J (J = 0, 1 and 3) of Eu³⁺ at around 580, 591 and 613 nm, respectively, when the powders were excited by 393 nm. The red color of the samples changed to yellow when the powder was annealed at 1200 °C. The decrease in the (⁵D₀ → ⁷F₂)/(⁵D₀ → ⁷F₁) ratio from around 5.0 for samples heated at lower temperatures to 3.1 for samples annealed at 1200 °C is consistent with a higher symmetry of the Eu³⁺ at higher temperature. The excitation spectra of the samples also confirms this change by the presence of a more intense and broad band at around 317 nm, instead of the presence of the characteristic peak at 393 nm, which corresponds to the ⁷F₀ → ⁵L₆ transition of the Eu³⁺. The lifetimes of the ⁵D₀ → ⁷F₂ transition of Eu³⁺ for the samples heat-treated at 100, 400, 800 and 1200 °C was evaluated as 0.57, 0.72, 0.43 and 0.31 ms, respectively.     

Synthesis of the CaAl2O4 nanoceramic compound using high-energy ball milling with subsequent annealing

Monocalcium aluminate, CaAl₂O₄, is the main constituent of calcium alumina cements which have found wide applications in refractory industries. In the present work, CaAl₂O₄ nanoceramic compound was produced by high-energy ball milling of the oxide powders followed by annealing. The phase evolution and microstructural changes of the powders during the process were investigated by means of X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that no CaAl₂O₄ was formed during ball milling even after 100 h. By subsequent annealing, the nucleation and growth of CaAl₂O₄ took place at 1000 °C after 2 h. Depending on milling time, the amount of CaAl₂O₄ increased with increasing annealing temperature. The CaAl₂O₄ single phase was obtained by milling the sample for 100 h and subsequently annealing at 1200 °C for 2 h. The quantitative phase analysis was used to measure CaAl₂O₄ phases in these processes. The average particle diameter of the sample milled for 100 h and annealed at 1200 °C was found to be less than 100 nm as measured by transmission electron microscopy.     

A study of manufacturing tubes with nano/ultrafine grain structure by stagger spinning

A new method of manufacturing tubes with nano/ultrafine grain structure by stagger spinning and recrystallization annealing is proposed in this study. Two methods of the stagger spinning process are developed, the corresponding macroforming quality, microstructural evolution and mechanical properties of the spun tubes made of ASTM 1020 steel are analysed. The results reveal that a good surface smoothness and an improved spin-formability of spun parts can be obtained by the process combining of 3-pass spinning followed by a 580 °C × 0.5 h static recrystallization and 2-pass spinning with a 580 °C × 1 h static recrystallization annealing under the severe thinning ratio of wall thickness reduction. The ferritic grains with an average initial size of 50 μm are refined to 500 nm after stagger spinning under the 87% thinning ratio of wall thickness reduction. The equiaxial ferritic grains with an average size of 600 nm are generated through re-nucleation and grain growth by subsequent recrystallization annealing at 580 °C for 1 h heat preservation. The tensile strength of spun tubes has been founded to be proportional to the reciprocal of layer spacing of pearlite (LSP), and the elongation is inversely proportional to the reciprocal of LSP. This study shows that the developed method of stagger power spinning has the potential to be used to manufacture bulk metal components with nano/ultrafine grain structure.     

Low temperature preparation and characterization of CdTiO3 nanoplates

An alternative low cost method was proposed for the low temperature (600 °C) preparation of CdTiO₃ nanoplates, using low-melting-point Cd(NO₃)₂ · 4H₂O and high-reactive-activity TiO₂ nanocrystals as the reactants. The structure, composition, specific surface area, thermal stability and optical properties of the as-synthesized products were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy, field emission scanning electron microscopy, Brunauer–Emmett–Teller surface area analysis, UV–vis absorption and room temperature photoluminescence spectra. The as-synthesized CdTiO₃ nanoplates were thermally stable at temperatures ≤ 900 °C, and their phase changed from ilmenite to perovskite when heated in air at 1000 °C for 2 h. Besides, they exhibited a strong and broad visible light emission in the range of about 470–750 nm upon laser excitation at 325 nm, enabling their use as a luminescent material.     

Photoluminescent properties of nanostructured Y2O3:Eu3+ powders obtained through aerosol synthesis

Red emitting Y₂O₃:Eu³⁺ (5 and 10 at.%) submicronic particles were synthesized through ultrasonic spray pyrolysis method from the pure nitrate solutions at 900 °C. The employed synthesis conditions (gradual increase of temperature within triple zone reactor and extended residence time) assured formation of spherical, dense, non-agglomerated particles that are nanostructured (crystallite size ∼20 nm). The as-prepared powders were additionally thermally treated at temperatures up to 1200 °C. A bcc Ia-3 cubic phase presence and exceptional powder morphological features were maintained with heating and are followed with particle structural changes (crystallite growth up to 130 nm). Emission spectra were studied after excitation with 393 nm wavelength and together with the decay lifetimes for Eu³⁺ ion ⁵D₀ and ⁵D₁ levels revealed the effect of powder nanocrystalline nature on its luminescent properties. The emission spectra showed typical Eu^{3+ 5}D₀ → ⁷F_i (i = 0, 1, 2, 3, 4) transitions with dominant red emission at 611 nm, while the lifetime measurements revealed the quenching effect with the rise of dopant concentration and its more consistent distribution into host lattice due to the thermal treatment.     

Effects of high-temperature annealing on the microstructure and properties of C/SiC–ZrB2 composites

C/SiC–ZrB₂ composites prepared via precursor infiltration and pyrolysis (PIP) were treated at high temperatures ranging from 1200 °C to 1800 °C. The mass loss rate of the composites increased with increasing annealing temperature and the flexural properties of the composites increased initially and then decreased reversely. Out of the four samples, the flexural strength and the modulus of the specimen treated at 1400 °C are maximal at 216.9 MPa and 35.5 GPa, suggesting the optimal annealing temperature for mechanical properties is 1400 °C. The fiber microstructure evolution during high-temperature annealing would not cause the decrease of fiber strength, and moderate annealing temperature enhanced the thermal stress whereas weakened the interface bonding, thus boosting the mechanical properties. However, once the annealing temperature exceeded 1600 °C, element diffusion and carbothermal reduction between ZrO₂ impurity and carbon fibers led to fiber erosion and a strong interface, jeopardizing the mechanical properties of the composites. The mass loss rate and linear recession rate of composites treated at 1800 °C are merely 0.0141 g/s and 0.0161 mm/s, respectively.     

Green light-emitting Lu3Al5O12:Ce phosphor powders prepared by spray pyrolysis

Green light-emitting Lu_2.985Al₅O₁₂:Ce_0.015 (LuAG:Ce) phosphor powders are prepared by spray pyrolysis. The only crystallized phase in the precursor powders and post-treated powders at temperatures below 800 °C is Lu₂O₃ and the other components are amorphous. Phase pure cubic garnet LuAG:Ce phosphor powders are obtained by post-treatment at 1000 °C. Phosphor powders post-treated at temperatures below 1400 °C retain the spherical shape of the precursor powders. The mean crystallite sizes of phosphor powders post-treated at 1200, 1400, and 1500 °C are 30, 46, and 54 nm, respectively. The excitation spectra contain two bands: a weak band with the maximum peak at 345 nm and a strong broad band in the spectral range from 400 to 490 nm with the maximum peak at 455 nm. The LuAG:Ce phosphor powders have broad emission spectra between 480 and 600 nm, with the maximum peak intensity located at 507 nm. The photoluminescence intensity of the phosphor powders post-treated at 1400 °C is 84.2% of that of the powders post-treated at 1500 °C.     

(101)-oriented ZnO nanoparticles fabricated in Si (100) by Zn ion implantation and thermal oxidation

ZnO nanoparticles (NPs) embedded in Si (100) substrate have been created by Zn ion implantation and post thermal annealing in oxygen atmosphere. Several techniques have been employed to investigate the formation of Zn NPs and their thermal evolution at elevated temperatures. Grazing X-ray diffraction results clearly show that ZnO NPs are effectively formed after 600 °C annealing, and they show a (101) preferential orientation. Cross-sectional transmission electron microscopy observations confirm that ZnO NPs with a narrow size distribution of 2–7 nm are formed within the near-surface region of about 35 nm in thickness. Photoluminescence measurement displays a strong emission band centered at 387 nm in the sample annealed at 600 °C.     

Thermal stability of MgO nanoparticles

Thermal stability of nanocrystalline MgO particles with average diameter of 11 nm was investigated by annealing of the cold isostatically pressed compacts between 600 °C and 900 °C for various durations. Sintering time versus grain radius at 800 °C demonstrated a linear line with the slope of ∼ 4 similar to that expected for surface diffusion. High resolution scanning electron microscope images from different specimens showed a porous microstructure of interconnected particles typical for initial sintering. Arrhenius plot of the grain size data revealed the activation energy of 161 ± 11 kJ mol^− 1 for the growth process in agreement with those reported for grain boundary grooving experiments. It was found that MgO particles undergo coarsening already at temperatures as low as 0.31 of the MgO melting point (3125 K). Increase in the particle diameter and decrease in the surface area were associated with surface diffusion mechanism that leads to initial sintering between the particles.     

Mechanical properties of hot pressed CoCrMo alloy compacts for biomedical applications

This study aimed at investigating the influence of the processing conditions on the mechanical properties of hot pressed compacts of a CoCrMo biomedical alloy.Several hot pressed CoCrMo compacts were processed in vacuum (10⁻² mbar), at a pressure of 60 MPa with different temperatures (900 °C, 1000 °C and 1100 °C) and different times (10 min, 30 min and 60 min). Compacts were examined by SEM/EDS. The transverse rupture strength, Young’s Moduli and hardness were determined. The fracture surface of compacts were also examined.The compacts hot pressed at 900 °C exhibited lower TRS than those processed at 1000 °C and 1100 °C, which showed similar strength values, regardless the sintering time. The 900 °C compacts showed also lower YM and higher porosity. Lower hardness values were registered for 900 °C compacts while 1000 °C compacts exhibited the highest values. The fracture surface analyses revealed fragile fracture for 900 °C compacts (10 min and 30 min) and 1000 °C (10 min). The remaining compacts exhibited ductile fracture.A full characterization of the mechanical properties of hot pressed CoCrMo compacts has been made and the selection of the processing parameters according to the desired mechanical properties is now possible.     

Growth and characterization of new semiorganic nonlinear optical single crystal L-Phenylalanine L-Phenylalaninium perchlorate (LPPAPC)

The new semi-organic nonlinear optical crystal, L-Phenylalanine L-Phenylalaninium perchlorate (LPPAPC) has been grown through synthesis between L-Phenylalanine and perchloric acid. The bulk crystals of dimension 5.5 × 0.4 × 0.3 cm³ were obtained by submerged seed solution method. The new compound was characterized by UV–Vis-NIR spectroscopic technique. In addition to that the solid-state structure of the crystal has been determined by single crystal X-ray diffraction technique. LPPAPC was thermally stable up to 272 °C as determined by TG/DTA studies. Also, the second harmonic generation (SHG) of the LPPAPC crystal was observed using Nd: YAG laser with a fundamental wavelength of 1064 nm.     

Photoluminescence properties of Y3Al5O12:Eu nanocrystallites prepared by co-precipitation method using a mixed precipitator of NH4HCO3 and NH3·H2O

Europium-doped yttrium aluminum garnet (Y₃Al₅O₁₂:Eu, YAG:Eu) nanocrystallites were prepared by calcining the precursors obtained via a co-precipitation method using a mixed solution of NH₄HCO₃ and NH₃·H₂O as the precipitator. The results of XRD, FTIR and thermal analysis showed that phase-pure YAG:Eu without any other phases was obtained at 900 °C. TEM results indicated that the particle sizes are 50–100 nm. YAG:Eu nanocrystallites showed four emission bands ascribed to ⁵D₀ → ⁷F₁ transition (592 and 597 nm) and ⁵D₀ → ⁷F₂ transition (611 and 633 nm) of Eu³⁺, respectively. The intensity of the magnetic dipole transition (⁵D₀ → ⁷F₁) is stronger than that of the electric dipole transition (⁵D₀ → ⁷F₂). The influence of the precipitators with different molar ratios of NH₄HCO₃ to NH₃·H₂O on the thermal properties of the as-prepared precursors and luminescent properties of the resulting YAG:Eu nanocrystallites was also investigated.