Characteristics of molecular beam epitaxy-grown GaFeAs

Diluted magnetic semiconductors GaFeAs were grown by molecular beam epitaxy and characterized. Ga_1−xFe_xAs ternary alloys were obtained at the growth temperature T_s=200 °C ranging from x=0.005 to 0.03. The effects of thermal treatment on behaviors of defects, affecting to the magnetic properties of GaFeAs layer were particularly elucidated. As-grown samples were annealed at temperatures varying from 400 to 600 °C. From the measurement of double crystal X-ray diffraction, we observed Fe-related peak which shifted to a higher diffraction angle as the Fe content increased, indicating that the lattice constant decreases with increasing Fe content. In contrast, above the annealing temperature 500 °C, the lattice constant becomes smaller than that of GaAs. Using the deep level transient spectroscopy, various defects in GaFeAs layer were observed and identified in conjunction with magnetic properties.     

Effect of Annealing Poly(4-Methylpentene) and of Oxidative Degradation during Annealing

Injection molded specimens of a poly(4-methylpentene) (TPX) were annealed at temperatures between 140 and 220°C for times up to 500 min in air, and the annealed TPX specimens were characterized by the differential scanning calorimeter, UV–visible spectrometry, FT-IR, and X-ray diffraction. The annealing of the TPX specimens at 140–180°C for 50 min showed little effect on their thermal properties. However, the thermal properties were significantly affected by annealing at 200–220°C, and the change was dependent on the annealing time. Besides the annealing effect, the thermal properties were also affected by oxidative degradation. Severe oxidative degradation can destroy the crystalline structure and thus decreases the crystallinity. The oxidative degradation phenomenon of the TPX specimens during annealing can be simulated by isothermal scanning of the weight loss in air by thermal gravimetric analysis.     

The Structure and Properties of Polyamide/Liquid Crystal Polymer Blends

Melt blended polyamide (PA)/liquid crystal polymer (LCP) blends were prepared and their structures and properties were studied. The tensile strength and impact strength of the PA/LCP blends increased with increasing small amount of LCP content. Compared with a pure PA sample, there was a 17.7% increase in the tensile strength and a 45.5% increase in the impact strength when the LCP content was less than 10%. On the other hand, the Vicat softening temperature decreased with increasing the LCP content. Differential scanning calorimetry (DSC) showed that small addition of LCP was beneficial to increase the crystallinity of PA component for PA/LCP blends and the melting peak for the PA component of PA/LCP blends shifted to lower temperature with increasing LCP content. Scanning electron microscopy (SEM) displayed a layered structure existing in the injection moldings of PA/LCP blends with the LCP crystals having a preferred orientation along the melt flow direction in the sub-skin, shearing layer, and core region. The increased crystallinity of PA component and preferred orientation structure of LCP phase were beneficial to increase the mechanical properties of the PA/LCP blends.     

Investigations of thermoluminescence properties of multicrystalline LiF: Mg,Cu, Si phosphor prepared by edge defined film fed growth technique

Thermoluminescence (TL) properties of LiF: Mg, Cu, Si phosphor prepared in multicrystalline form using edge defined film fed growth (EFG) technique has been investigated. The effect of preparation route on TL properties and thermal stability has been studied. To improve the TL dosimetry properties, phosphor is subjected to different annealing temperatures ranging from 250 °C to 450 °C. The shape of the glow curve structure and peak temperature remains similar at different annealing temperatures, however peak intensities vary. The consistency in the glow curve structure with annealing temperature elucidate that TL trapping states are stable in nature. Thermal annealing at 300 °C for 10 min gives maximum TL intensity with main dosimetry peak at 209 °C. The TL intensity of the main dosimetry peak is increased by a factor of five as compared to as-grown crystal. The thermal stability of LiF: Mg, Cu, Si is found to be better than LiF: Mg, Cu, P. Trapping parameters are calculated to have an insight study of defect states. A simple glow curve structure, tissue equivalency, thermal stability, low residual signal, linear response and reusability makes LiF: Mg, Cu, Si a suitable phosphor for radiation therapy, radio diagnostics and personnel dosimetry applications.     

Thermal stability of organic layered systems based on lead stearate

The structural variation in multilayer Langmuir-Blodgett films of lead stearate caused by heat treatment under different conditions in the temperature range 20–100°C is investigated by X-ray reflectometry and high-resolution electron diffraction. Successive annealing of the samples is shown to not alter the initial layered structure at temperatures of 60, 80, and 100°C; partial disturbance of the layered structure occurs upon successive annealing at 80°C and 100°C. Significant disturbance of the structure is observed when the films are heated immediately to 100°C. In all these cases, the orthorhombic (pseudomonoclinic) lattice, with the lattice constants: a = 0.496, b = 0.738, c = 9.60 nm, α = β = γ = 90°, space group P2/1b, formed by transferring monolayers onto the substrate is retained in the crystalline domains of the film.     

Poly(3-Hydroxybutyrate) Matrices Modified with Iron(III) Complexes with Tetraphenylporphyrin. Analysis of the Structural Dynamic Parameters

The effect of small additions of the iron(III) complex with tetraphenylporphyrin (0–5%) on the structure and properties of ultrathin fibers based on poly(3-hydroxybutyrate) (PHB) was studied by differential scanning calorimetry (DSC), X-ray diffraction analysis (XRD), EPR probe method, and scanning electron microscopy. When tetramethylporphyrin was added to the PHB fibers, the crystallinity significantly increased, and the molecular mobility in the amorphous regions of the polymer decreased. The thermal treatment of the fibers (annealing at 140°C) led to significantly increased crystallinity and decreased molecular mobility in the amorphous regions of the PHB fibers. The addition of tetramethylporphyrin to the PHB fibers led to a sharp decrease in crystallinity. Ozonolysis of the fibers at small treatment times caused a considerable decrease in their molecular mobility (to 5 h), while prolonged ozonolysis led to increased mobility. The obtained fibrous materials have bactericidal properties and will find use in the development of antibacterial and antitumor therapeutic systems.     

Raman active lattice spectrum of single crystal 2,4,6-triphenyltriazine

The Raman spectra of single crystal 2,4,6-triphenyltriazine have been recorded in the lattice region at 300 and 30°K. The interpretation of the results was based on assuming that the molecular structure is D_3h (i.e. complete planarity) instead of the most probable non-planar conformation of C₁ symmetry. Assignment of the lattice vibrations was based on a rigid-body approximation. Considerable temperature effect was observed in the spectrum when the crystal was cooled to 30°K. This seemed to indicate large anisotropic thermal motions in the crystalline solid.     

Shape-memorizable styrene-butadiene block copolymer. I. Thermal and mechanical behaviors and structural change with deformation

Thermal properties in the range from room temperature to 150°C, mechanical properties from room temperature to 80°C, and structural changes by drawing and contraction at 80°C followed by crystallization have been studied in a crystalline styrene-butadiene block copolymer, which has the property of shape memory, using differential scanning calorimetry (DSC), mechanical analysis, wide-angle x-ray diffraction (WAXD), and smallangle x-ray scattering (SAXS). This copolymer has the crystal transformation temperature, the melting temperature of the trans- 1,4-polybutadiene domains, and the higher glass transition temperature of the polystyrene domains. When a high strain is adopted for the deformation at 80°C (i.e., between the melting temperature of the polybutadiene [PB] domains and the glass transition temperature of the polystyrene regions) and crystallization conditions with fixed ends are employed, a fibrillar structure with a better regularity of long spacings and a high orientation of crystals forms. When the drawn sample is allowed to contract at 80°C, the high contraction or the shape recovery appears. Nevertheless, crystallization after contraction presents essentially the same supermolecular structure as that before contraction. It is suggested that the molecular chains of polybutadiene were inhibited from flowing freely by the glassy polystyrene molecules and that there must be some structural units separated by amorphous domains that contribute to the elongation and contraction at the high temperature.     

Effect of annealing on the structure and morphology of nylon 6 fibers

Changes in the structure of nylon 6 fibers annealed in dry and wet atmospheres were studied by small-and wide-angle x-ray diffraction. In the presence of water or saturated steam, fibers can be annealed to the same strucutral state at temperatures 70°C lower than in dry atmosphere. This is due to the enhanced mobility of the molecular segments in the amorphous region, a mechanism which is also known to lower the T_g by the same amount. Upon annealing under unconstrained conditions, lamellar spacing, crystallite size in the equatorial plane, crystalline as well as fiber density, and the chain-axis repeat increase with annealing-temperature; whereas crystalline orientation and the Van der Waals separation of the hydrogen-bonded sheets decrease. The monoclinic angle 8 remains constant at 66.7° (σ = 0.3°) and might depend on the starting fiber rather than on the treatment of the fiber. Most of these changes occur above a critical temperature of 170°C if dry, or 100°C if wet; rate of crystallization is also the highest under these conditions in nylon. The effect of these changes on such fiber properties as dyeing and the role of micro voids in dye diffusion and in dye uptake are discussed. Surface premelting and the accompanying changes in the surface structure of the lamellae, selective melting, and more importantly, the longitudinal motion of the nylon 6 chains and the resulting folding of interfibrillar extended amorphous chains are invoked to explain the shrinkage of the fiber, disorientation of the crystallites, increase in crystalline perfection, and the increase in lamellar spacing.     

Curie temperatures of CoPt ultrathin continuous films

The effects of layer thickness and thermal annealing on Curie temperature have been studied for CoPt ultrathin continuous layers in AlN/CoPt multilayer structures. It is found that there exists a critical thickness below which Curie temperature rapidly decreases due to the loss of spin-spin interactions in the vicinity of interface. After high temperature annealing, the in-plane lattice constant of CoPt film is increased and the exchange coupling parameter is decreased. Consequently, Curie temperatures decrease for some films with large thickness, compared with as-deposited state. Upon annealing at 600?^°C, CoPt undergoes ordering transformation, which also contributes to the degradation of the Curie temperature. However, when the CoPt film thickness is below 2?nm, the Curie temperature is increased after annealing. Especially for 1?nm thick film, the Curie temperature is strikingly increased from 173?^°C to 343?^°C after annealing at 600?^°C. This effect is attributed to the out-of-plane lattice deformation of CoPt thin layers in AlN/CoPt multilayer structures.     

Complex dynamics of a particle in an oscillating potential field

In this paper, Mg-doped ZnO nanoparticles were synthesized by the facile sol–gel method. The crystalline structure, characteristic absorption bands and morphology of the obtained Mg-doped ZnO nanoparticles were studied by XRD, FTIR and TEM. The thermal degradation behaviour of the samples was investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The effect of Mg concentrations and annealing temperatures on the antibacterial properties of the obtained nanoparticles was investigated in detail. The results indicated that doping Mg ions into ZnO lattice could enhance its antibacterial activity. Antibacterial assay demonstrated that Mg-doped ZnO with 7% Mg content annealed at 400 ^°C had the strongest antibacterial activity against Listeria monocytogenes (98.7%). This study indicated that the inhibition rate of ZnO nanoparticles increased with the formation of granular structure and the decrease of ZnO size due to the doping of Mg ions into the ZnO lattice.     

Crystal recovery from Al‐implantation induced damaging in 3C‐SiC films

Damaging in Al‐implanted 3C‐SiC and subsequent crystal recovery due to thermal treatments up to 1350 °C are evaluated by X‐ray diffraction and micro‐Raman spectroscopy. Reciprocal space mapping of (004) 3C‐SiC planes shows a low‐intensity implantation‐induced secondary peak at higher interplanar spacing in the as‐implanted 3C‐SiC sample, with a generated misfit between the implanted and the epitaxial region of about 0.6%. Increasing the annealing temperature from 950 °C to 1350 °C, the secondary peak is gradually re‐absorbed within the epitaxial 3C‐SiC reciprocal lattice point. Finally, the disappearance of the secondary peak after a 1350 °C thermal treatment is observed. Thus, implantation‐induced average strain, resulting in a severe 3C‐SiC deforma‐ tion, has been totally relieved at the highest annealing temperature. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Phase change and pyroelectricity in natural hemimorphite

The phase change of a natural hemimorphite sample from Minas Gerais (Brazil) was investigated by two X-ray diffraction (XRD) methods and by near-infrared reflectance spectroscopy. Applying successive thermal treatments, the crystal structure undergoes two orientation conversions. The first one occurs at about 550 °C, and it was revealed by the Laue method. Below 500 °C, the water molecules were partially expelled without changing the crystal structure. A fact that supports this statement is the sequential disappearance of the water bands at 1400 and 1900 nm by thermal treatment. The second conversion takes place below 939 °C. Moreover, at 972 °C a phase change to the willemite mineral (α-Zn₂SiO₄) has been observed. This last conversion was confirmed by the power XRD. In addition, natural hemimorphite displayed a high pyroelectricity, which is related both to the absence of inverse centre and to the presence of molecular water and hydroxyl groups in the crystal structure.     

KTN thin films prepared by pulsed laser deposition on transparent single crystal quartz(100)

Using the Sol-Gel method to produce the KTN ultrafine powder and the sintering technique with K2O atmosphere to prepare KTN ceramics as the targets instead of the KTN single crystal, highly oriented KTN thin films were produced on the transparent single crystal quartz (100) by the pulsed laser deposition (PLD). Since the thermal stress sustained by the quartz is relatively small, the limit temperature of the quartz substrates (300℃) is much lower than that of the P-Si substrates (560℃); the prepared thin film is at amorphous state. Increasing the pulsed laser energy density in the process incorporated with annealing the film after deposition at different temperatures converts the amorphous films into crystal. The optimal pulsed laser energy density and annealing temperature were 2.0 J/cm2 and 600℃, respectively. A discussion was made to understand the mechanism of film production at relatively low substrate temperature by PLD and effects of the annealing temperatures on the forming of the perovskite p     

Study of structural and electrical properties of thin NiO<Subscript>x</Subscript> films prepared by ion beam sputtering of Ni and subsequent thermo-oxidation

Nickel oxide thin films were prepared by thermal annealing of thin Ni films (thickness ca 47?nm) deposited by ion beam sputtering. The thermal annealing was performed at 350 °C and 400 °C with elected time (1–7 hours) in a quartz furnace opened to air. During annealing the samples underwent structural changes, as well as changes of their electrical properties. The structural properties (surface morphology and occurrence of crystalline phases) were analyzed by the AFM and XRD methods, O and Ni depth concentration profiles by the NRA method, and electrical properties (sheet resistance) by the van der Pauw 4-point technique. The sheet resistance (R _S ) of the as-deposited sample was found to be 12.03 Ω/□; after open air thermal annealing at 350 °C for 1 h the value was found to be almost the same, 11.67 Ω/□. After 2 h of annealing, however, a sharp increase in the sheet resistance (R _S = 1.46 MΩ/□) was observed. At this stage the deposit formed largely oxidized Ni layer with a distinct polycrystalline structure. The sharp increase of sheet resistance was ascribed to the oxidation of the Ni layer, leaving only a smaller amount of isolated Ni particles unoxidized. Almost complete oxidation was found after 7 h of annealing at 350 °C. At 400 °C was almost complete oxidation recorded already after 1 h of annealing.     

In-situ and ex-situ study of crystallization behaviour of magnetron sputtered Ni63Zr37 amorphous thin film

ABSTRACT

The stages of crystallization of magnetron sputter-deposited Ni₆₃Zr₃₇ film with mostly amorphous structure have been investigated by differential scanning calorimetry (DSC) and in-situ annealing at 300°C by use of heating stage on a high-resolution transmission electron microscope (HRTEM). These results have been further confirmed by grazing incidence X-ray diffraction analyses of thin film specimens annealed ex-situ at 300°C for various durations. The temperature for crystallization found by DSC has been found to increase from 371°C to 434°C with an increase in heating rate from 3°C/min to 10°C/min, and the apparent activation energy for amorphous to crystalline transformation has been found as ～260.2?kJ/mol from the Kissinger plot. Studies on HRTEM using in-situ heating stage have shown the crystallization to occur on annealing at 300°C for ～10?min. Crystallization at a temperature lower than that found by DSC is attributed to structural relaxation with reduction of free volume due to thermal activation. It has been observed that Ni₃Zr forms first due to its large negative enthalpy of formation, and is followed by the formation of Ni-rich solid solution (Ni_ss) grains. HRTEM studies have shown grain rotation with the formation of partial dislocations at Ni₃Zr-Ni_ss interfaces as well as twinning followed by detwinning with dislocation formation in the Ni_ss matrix possibly to reduce the interfacial energy.     

Phase transformation of ZrO2 nanoparticles produced from zircon

This article focuses on the phase transformation of zirconia (ZrO₂) nanoparticles produced from zircon using a bottom-up approach. The influence of mechanical milling and thermal annealing on crystalline phase transformation of ZrO₂ nanoparticles was explored. It was found that the iron oxide, as an inherent impurity present in ZrO₂ nanoparticles, produced from zircon stabilises the cubic phase after calcination at 600°C. The stabilised cubic phase of ZrO₂ nanoparticles was disappeared and transformed into partial tetragonal and monoclinic phases after mechanical milling. The phase transformation occurred on account of the crystal defect induced by high-energy mechanical milling. The destabilisation of cubic phase into monoclinic phase was observed after the thermal annealing of ZrO₂ nanoparticles at 1000°C. The phase transitions observed are correlated to the exclusion of iron oxide from the zirconia crystal structure.     

On the formation of lamellae during annealing of extended chain crystals of radiation-polymerized trioxane

The structure changes of radiation-polymerized trioxane taking place during annealing have been studied by means of electron microscopy, X-ray small- and wide-angle scattering, and differential thermal analysis. The original fibrillar crystals, supposedly consisting of extended chains, change into lamellar crystals due to annealing at temperatures between 150° and 190°C. Lamella formation can be connected with the appearance of a long period of about 200A which is not observed in the unannealed sample.

During annealing within the same temperature range the X-ray reflections due to the twin structure of the original polytrioxane disappear, whereas the orientation of the fraction with its c-axis parallel to the c-axis of the parent trioxane remains unaltered.

The melting point of the lamellar crystals obtained by annealing is 186°-187°C and, therefore, considerably higher than the melting point (175°C) of crystals grown during cooling of a polytrioxane melt. The equilibrium melting point of an undisturbed extended-chain poly-oxymethylene single crystal must be still higher and may even approach 200°C.

On the basis of the electron-microscopical observations and the X-ray results, it is supposed that the process of lamella formation takes place continuously by reorganization of the whole structure including the already grown lamellae. The rate of this process is the faster the higher the annealing temperature. Some possible mechanisms are discussed but the final reasons for the observed structure changes are not known.     

The study of gamma irradiation effects on poly (glycolic acid)

We have investigated the effects of gamma irradiation on chemical structure, thermal and morphological properties of biodegradable semi-crystalline poly (glycolic acid) (PGA). PGA samples were subjected to irradiation treatment using a ⁶⁰Co gamma source with a delivered dose of 30, 60 and 90?kGy, respectively. Gamma irradiation induces cleavage of PGA main chains forming ～O?H₂ and ?H₂COO～ radicals in both amorphous and crystalline regions. The free radicals formed in the amorphous region abstract atmospheric oxygen and convert them to peroxy radicals. The peroxy radical causes chain scission at the crystal interface through hydrogen abstraction from methylene groups forming the ～?HCOO～ (I) radical. Consequently, the observed electron spin resonance (ESR) doublet of irradiated PGA is assigned to (I). The disappearance of the ESR signal above 190°C indicates that free radicals are formed in the amorphous region and decay below the melting temperature of PGA. Fourier transform infrared and optical absorption studies confirm that the groups are not influenced by gamma irradiation. Differential scanning calorimetry (DSC) studies showed that the melting temperature of PGA decreased from 212°C to 202°C upon irradiation. Degree of crystallinity increased initially and then decreased with an increase in radiation as per DSC and X-ray diffraction studies. Irradiation produced changes in the physical properties of PGA as well as affecting the morphology of the material.     

Growth kinetics and polysilicon formation by aluminium-induced crystallization on glass-ceramic substrates

In this work, we present extended structural properties of poly-Si thin films fabricated by aluminium-induced crystallization (AIC) of amorphous silicon (a-Si) on high-temperature glass-ceramic substrates. The silicon nucleation kinetics on glass-ceramic substrates was investigated by optical microscopy. The crystalline quality of the films was studied by micro-Raman spectroscopy as a function of exchange annealing conditions. By means of electron backscattering diffraction (EBSD), we have analyzed the effect of thermal annealing on silicon grain size and its distribution, intra- and inter-grains defects, and on the grains preferential crystallographic orientation. The optimal thermal annealing condition, allowing 100% crystallized polysilicon large grains with an average grain size of 26 μm and 〈100〉 oriented, acquired a thermal budget of 475°C and 8 h.