On the exothermic peak during annealing of electrodeposited nanocrystalline nickel

Nanocrystalline metals frequently exhibit poor thermal stability, and the exothermic peak in differential scanning calorimetry is usually attributed to grain growth. We show from experiments on electrodeposited nano-Ni with varying levels of S, and tests with microcrystalline Ni and S powders, that the exothermic peak is associated with the formation of a nickel sulfide phase and concurrent grain growth. Analysis suggests that segregation plays a more important role in limiting grain growth than second-phase particles in nano-Ni. (C) 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Microstructure evolution and hardness variation during annealing of equal channel angular pressed ultra-fine grained nickel subjected to 12 passes

The microstructure, thermal stability and hardness of ultra-fine grained (UFG) Ni produced by 12 passes of equal channel angular pressing (ECAP) through the route Bc were studied. Comparing the microstructure and hardness of the as-ECAPed samples with the published data on UFG Ni obtained after 8 passes of ECAP through the route Bc reveals a smaller average grain size (230 nm in the present case compared with 270 nm in 8-pass Ni), significantly lower dislocation density (1.08 x 10(14) m(-2) compared with 9 x 10(14) m(-2) in 8-pass Ni) and lower hardness (2 GPa compared with 2.45 GPa for 8-pass Ni). Study of the thermal stability of the 12-pass UFG Ni revealed that recovery is dominant in the temperature range 150-250A degrees C and recrystallisation occurred at temperatures > 250 A degrees C. The UFG microstructure is relatively stable up to about 400 A degrees C. Due to the lower dislocation density and consequently a lower stored energy, the recrystallisation of 12-pass ECAP Ni occurred at a higher temperature (similar to 250 A degrees C) compared with the 8-pass Ni (similar to 200 A degrees C). In the 12-pass Nickel, hardness variation shows that its dependence on grain size is inversely linear rather than the common grain size(-0.5) dependence.

Crack formation due to annealing of Al2O3 films grown on Si(100) by MOCVD

We report crack formation in alumina films grown on Si(100), caused by annealing in a controlled oxidizing ambient. The films were grown in a low-pressure CVD reactor, using aluminium acetylacetonate as precursor. High purity argon and nitrous oxide were employed as carrier and oxidizing gas, respectively. The films were characterized by optical microscopy and SEM/EDAX. The proportion and chemical nature of the heteroatoms, namely C and H, incorporated into the films from the precursor, were characterized by XPS, and FTIR. As-deposited films do not exhibit any cracks, while post-deposition annealing results in cracks. Apart from the delamination of the films, annealing in nitrous oxide ambient leads to an unusual crack geometry, which we term the “railway-track”. These twin cracks are very straight and run parallel to each other for as much as several millimeters. Often, two such linear tracks meet at exactly 90°. Between some of these tracks lie bullet-like structures with very sharp tips, oriented in a specific direction. As cracks are generally activated by residual stress, both thermal and intrinsic, the origins of the stresses that generate these linear cracks are discussed. The redistribution of stress, arising from the removal of C and H during annealing, will also be discussed. An attempt has been made to correlate the formation of cracks with the crystal structure of the film.

Investigating thermal stability of structural defects and its effect on d(0) ferromagnetism in undoped SnO2

The effect of annealing on structural defects and d(0) ferromagnetism in SnO2 nanoparticles prepared by solution combustion method is investigated. The as-synthesized SnO2 nanoparticles were annealed at 400-800 degrees C for 2 h, in ambient conditions. The crystallinity, size, and morphology of the samples were studied using x-ray diffraction and transmission electron microscopy studies. The annealing results in grain growth due to coarsening as well as reduction in oxygen vacancies as confirmed by Raman spectroscopy, photoluminescence spectroscopy, and x-ray photoelectron spectroscopy. All the as synthesized and annealed samples exhibit room temperature ferromagnetism (RTFM) with distinct hysteresis loops and the saturation magnetization as high as similar to 0.02 emu/g in as-synthesized samples. However, the saturation magnetization is drastically reduced with increasing annealing temperature. Further the presence of singly charged oxygen vacancies (V-o(-) signal at g-value 1.99) is confirmed by electron paramagnetic resonance studies, which also diminish with increasing annealing temperature. The observed diminishing RTFM and simultaneous evidences of diminishing O vacancies clearly indicate that RTFM is driven by defects in oxide lattice and confirms primary role of oxygen vacancies in inducing ferromagnetic ordering in metal oxide semiconductors. The study also provides improved fundamental understanding regarding the ambiguity in the origin of intrinsic RTFM in semiconducting metal oxides and projects their technological application in the field of spintronics. (C) 2013 AIP Publishing LLC.

Thermal Response on the Microstructure and Texture of ECAP and Cold-Rolled Pure Magnesium

This paper deals with dynamic recrystallization (DRX), static recrystallization, and grain growth phenomena of pure magnesium after equal channel angular pressing (ECAP) by route A and B-C at 523 K (250 A degrees C) followed by 80 pct cold rolling. The ECAP-deformed and the subsequently rolled samples were annealed at 373 K and 773 K (100 A degrees C and 500 A degrees C). The associated changes in the microstructure and texture were studied using electron back-scattered diffraction. ECAP produced an average grain size of 12 to 18 A mu m with B and C-2 fiber textures. Subsequent rolling led to an average grain size 8 to 10 A mu m with basal texture fiber parallel to ND. There was no noticeable increase in the average grain size on annealing at 373 K (100 A degrees C). However, significant increase in the average grain size occurred at 773 K (500 A degrees C). The occurrence of different DRX mechanisms was detected: discontinuous dynamic recrystallization was attributed to basal slip activity and continuous dynamic recovery and recrystallization to prismatic/pyramidal slip systems. Only continuous static recrystallization could be observed on annealing.

Thermal stability and spectroscopic properties of Er3+-doped niobium tellurite glasses for broadband amplifiers

Three Er3+-doped tellurite glasses with compositions of 70TeO(2)-30ZnO, 70TeO(2)-20ZnO-10Nb(2)O(5) and 70TeO(2)-20ZnO-5BaO-5Nb(2)O(5) have been investigated for developing fiber and planar broadband amplifiers and lasers. The optical spectroscopic properties and thermal stability of Er3+-doped tellurite glasses have been discussed. The results show that the incorporation of Nb2O5 increases the thermal stability of Er3+-doped tellurite glasses significantly, Er3+-doped niobium tellurite glasses 70TeO(2)-20ZnO-10Nb(2)O(5) and 70TeO(2)-20ZnO-5BaO-5Nb(2)O(5) exhibit the good thermal stability (DeltaT > 150degreesC), the large emission cross-section (>10 x 10(-21) cm(2)) and broad full width at half maximum (similar to65 nm), will be preferable for broadband Er3+-doped fiber amplifiers. (C) 2004 Elsevier B.V. All rights reserved.

Microstructure and laser-induced damage threshold of ZrO2 coatings dependence on annealing temperature

ZrO2 coatings were deposited on different substrates of Yb:YAG and fused silica by electron beam evaporation. After annealed for 12 h at 673 and 1073 K, respectively, weak absorption of coatings was measured by surface thermal lensing (STL) technique, and then laser-induced damage threshold (LIDT) was determined also. The crystalline phase of ZrO2 coatings and the size of the crystal grain were investigated by X-ray diffraction. It was found that microstructure of ZrO2 coatings was dependent on both annealing temperature and substrate structure, and coatings containing monoclinic phases had higher damage threshold than others. Due to the strong absorption of Yb:YAG, damage threshold of coatings on Yb:YAG was much less than that on fused silica. (C) 2004 Elsevier B.V. All rights reserved.

Structure and UV emission of nanocrystal ZnO films by thermal oxidation of ZnS films

ZnO films prepared by the thermal oxidation of the ZnS films through thermal evaporation are reported. The as-deposited ZnS films have transformed to ZnO films completely at 400 degrees C. The 400-700 degrees C annealed films with a preferential c-axis (002) orientation have a hexagonal wurtzite structure. The band gap of ZnO films shifts towards longer wavelength with the increase of the annealing temperature. The relationship between the band gap energy of ZnO films and the grain size is discussed. The shift of the band gap energy can be ascribed to the quantum confinement effect in nanocrystal ZnO films. The photoluminescence spectra of ZnO films show a dominant ultraviolet emission and no deep level or trap state defect emission in the green region. It confirms the absence of interstitial zinc or oxygen vacancies in ZnO films. These results indicate that ZnO film prepared by this simple thermal oxidation method is a promising candidate for optoelectronic devices and UV laser. (c) 2005 Elsevier BN. All rights reserved.

Influence of annealing temperature on structure, optical loss and laser-induced damage threshold of TiO2 thin films

TiO2 thin films are prepared on fused silica with conventional electron beam evaporation deposition. After annealed at different temperatures for 4h, the spectra and XRD patterns of the TiO2 thin film are obtained. Weak absorption of coatings is measured by the surface thermal lensing technique, and laser-induced damage threshold (LIDT) is determined. It is found that with the increasing annealing temperature, the transmittance of TiO2 films decreases. Especially when coatings are annealed at high temperature over 1173K, the optical loss is very serious. Weak absorption detection indicates that the absorption of coatings decreases firstly and then increases, and the absorption and defects play major roles in the LIDT of TiO2 thin films.

Influences of CO2 laser annealing on mechanical and laser-induced damage properties of ZrO2 thin films

Zirconium dioxide (ZrO2) thin films were deposited on BK7 glass substrates by the electron beam evaporation method. A continuous wave CO2 laser was used to anneal the ZrO2 thin films to investigate whether beneficial changes could be produced. After annealing at different laser scanning speeds by CO2 laser, weak absorption of the coatings was measured by the surface thermal lensing (STL) technique, and then laser-induced damage threshold (LIDT) was also determined. It was found that the weak absorption decreased first, while the laser scanning speed is below some value, then increased. The LIDT of the ZrO2 coatings decreased greatly when the laser scanning speeds were below some value. A Nomarski microscope was employed to map the damage morphology, and it was found that the damage behavior was defect-initiated both for annealed and as-deposited samples. The influences of post-deposition CO2 laser annealing on the structural and mechanical properties of the films have also been investigated by X-ray diffraction and ZYGO interferometer. It was found that the microstructure of the ZrO2 films did not change. The residual stress in ZrO2 films showed a tendency from tensile to compressive after CO, laser annealing, and the variation quantity of the residual stress increased with decreasing laser scanning speed. The residual stress may be mitigated to some extent at proper treatment parameters. (c) 2007 Elsevier GmbH. All rights reserved.

Investigation of annealing effects on the laser-induced damage threshold of amorphous Ta2O5 films

Ta2O5 films were deposited using the conventional electron beam evaporation method and then annealed at temperatures in the range 373-673 K. Chemical composition, scattering and absorption were examined by X-ray photoelectron spectroscopy (XPS), total integrated scattering (TIS) measurement and the surface thermal lensing (m) technique, respectively. The laser-induced damage threshold (LIDT) was assessed using the output from an Nd:YAG laser with a pulse length of 12 ns. The results showed that the improvement of the LIDT after annealing was due to the reduced substoichiometric and structural defects present in the film. The LIDT increased slightly below 573K and then increased significantly with increase in annealing temperature, which could be attributed to different dominant defects. Moreover, the root mean square (RMS) roughness and scattering had little effect on the LIDT, while the absorption and the LIDT were in accord with a general relation. (c) 2008 Elsevier Ltd. All rights reserved.

Investigation on thermal stability of TiO2 films for application at high temperature

The thermal stability of electron beam deposited TiO2 monolayers and TiO2/SiO2 high reflectors (HR) during 300 to 1100 degrees C annealing is studied. It is found that the optical loss of film increases with the increase in annealing temperature, due to the phase change, crystallisation and deoxidising of film. Scattering loss dominates the optical property degradation of film below 900 degrees C, while the absorption is another factor at 1100 degrees C. The increase in refractive index and decrease in physical thickness of TiO2 layer shift the spectra of HR above 900 degrees C. The possible crack mechanism on the surface of HR during annealing is discussed. Guidance for application on high temperature stable optical coatings is given.

Spontaneous formation of highly ordered nanostructures: thermal instability and mode selection in surface-capped polymer films.

We demonstrate a controllable formation process of wave-like patterns in thermally unstable surface-capped polymer films on a rigid substrate. Self-ordered wave-like structures over a large area can be created by applying a small lateral tension to the film, whereupon it becomes unstable. A clear mode selection process which includes creation, decay and interference between coexisting waves at different annealing conditions has been observed, which makes it possible to restrain the patterns which are formed finally. Our results provide a clear and new evidence of spinodal behaviour in such a film due to thermal instability. Furthermore, we show that the well-controlled patterns generated in such a process can be used to fabricate nanostructures for various applications.

Application of electron beams in thermal processing of semiconductor materials and devices

Rapid and effective thermal processing methods using electron beams are described in this paper. Heating times ranging from a fraction of a second to several seconds and temperatures up to 1400°C are attainable. Applications such as the annealing of ion implanted material, both without significant dopant diffusion and with highly controlled diffusion of impurities, are described. The technique has been used successfully to activate source/drain regions for fine geometry NMOS transistors. It is shown that electron beams can produce localised heating of semiconductor substrates and a resolution of approximately 1 μm has been achieved. Electron beam heating has been applied to improving the crystalline quality of silicon-on sapphire used in CMOS device fabrication. Silicon layers with defect levels approaching bulk material have been obtained. Finally, the combination of isothermal and selective annealing is shown to have application in recrystallisation of polysilicon films on an insulating layer. The approach provides the opportunity of producing a silicon-on-insulator substrate with improved crystalline quality compared to silicon-on-sapphire at a potentially lower cost. It is suggested that rapid heating methods are expected to provide a real alternative to conventional furnace processing of semiconductor devices in the development of fabrication technology. © 1984 Benn electronics Publications Ltd, Luton.

TIME RESOLVED REFLECTIVITY MEASUREMENTS APPLIED TO RAPID ISOTHERMAL ANNEALING OF ION IMPLANTED SILICON.

The annealing of ion implantation damage in silicon by rapid isothermal heating has been monitored by the time resolved reflectivity (TRR) method. This technique was applied simultaneously at a wavelength of 632. 8nm and also at 1152nm, where the optical absorption coefficient of silicon is less. The two wavelength method simplifies the interpretation of TRR results, extends the measurement depth and allows good resolution of the position of the interface between amorphous and crystalline silicon. The regrowth of amorphous layers in silicon, created by self implantation and implanted with electrically active impurities, was observed. Regrowth in rapid isothermal annealing occurs during the heating up stage of typical thermal cycles. Impurities such as B, P, and As increase the regrowth rate in a manner consistent with a vacancy model for regrowth. The maximum regrowth rate in boron implanted silicon is limited by the solid solubility.