The freezing and supercooling of garlic (Allium sativum L.)

This work shows that peeled garlic cloves demonstrate significant supercooling during freezing under standard conditions and can be stored at temperatures well below their freezing point (?2.7 °C) without freezing. The nucleation point or ‘metastable limit temperature’ (the point at which ice crystal nucleation is initiated) of peeled garlic cloves was found to be between ?7.7 and ?14.6 °C. Peeled garlic cloves were stored under static air conditions at temperatures between ?6 and ?9 °C for up to 69 h without freezing, and unpeeled whole garlic bulbs and cloves were stored for 1 week at ?6 °C without freezing.     

Containerless processing of a lithium disilicate glass

Glasses of Li₂O · 2SiO₂ (LS₂), and LS₂ doped with 0.001 wt% platinum (LS₂ + 0.001 wt% Pt) compositions were melted, cooled and reheated at controlled rates while levitated (containerless) inside an electrostatic levitator (ESL) furnace at the NASA Marshall Space Flight Center. The experiments were conducted in vacuum using spherical, 2.5–3 mm diameter, glass samples. The measured critical cooling rate for glass formation, R _c, for the LS₂ and LS₂ + 0.001 wt% Pt glasses processed at ESL were 14 ± 2 °C/min and 130 ± 5 °C/min, respectively. The values of R _c for the same LS₂ and LS₂ + 0.001 wt% Pt glasses processed in a container were 62 ± 3 °C/min and 162 ± 5 °C/min, respectively. The effective activation energy for crystallization, E, for this LS₂ glass processed without a container at ESL, was higher than that for an identical glass processed in a container. These results suggest that the glass formation tendency for a containerless LS₂ melt is significantly increased compared to an identical melt in contact with a container. The absence of heterogeneous nucleation sites that are inherently present in all melts held in containers is believed to be the reason for the increased glass forming tendency of this containerless melt.     

Effect of Oleic Acid and Oleylamine Surfactants on the Size of FePt Nanoparticles

FePt magnetic nanoparticles have been synthesized by superhydride reduction of FeCl₂ and Pt(acac)₂ at high temperature. Adding superhydride (LiBEt3H) to the phenyl ether solution of FeCl₂ and Pt(acac)₂ in the presence of oleic acid, oleylamine, and 1,2-hexadecanediol at 190?^°C, followed by refluxing at 245?^°C, led to monodisperse 3.5?nm FePt nanoparticles. The effect of oleylamine and oleic acid surfactants on the nucleation and growth of FePt nanoparticles were studied. The size of Pt was controlled by oleylamine surfactant in nucleation stage. To prevent sintering of the FePt nanoparticles, oleic acid surfactant was used in growth stage. The energy dispersive spectroscopy results revealed that the particle composition was first Fe₁₁Pt₈₉ in nucleation stage and after adding superhydride the composition changed to Fe₆₃Pt₃₇ in growth stage. The structural and magnetic measurements indicated that the L1₀ structure of FePt nanoparticles is formed after annealing and the coercivity of superlattice FePt nanoparticles increases to 7.5?kOe after heat treatments.     

Effects of nitrogen content and weld cooling time on the simulated heat-affected zone toughness in a Ti-containing steel

An increase of nitrogen content in a 0.02 wt% Ti-containing carbon-manganese steel resulted in a low coarsening rate of TiN particles in the heat-affected zone (HAZ), which led to an accelerated ferrite transformation instead of ferrite side plates during weld cooling cycle. The mixed microstructure of ferrite side plate, acicular ferrite and grain boundary polygonal ferrite in the simulated HAZ produced higher toughness. However, the increase of nitrogen content gradually increased the free nitrogen content in the HAZ and deteriorated HAZ toughness. Impact energy of the simulated HAZ (with Δt_8/5 ∼60 s) at –20 °C deteriorated by about 97 J per 0.001 wt% free nitrogen, in the free nitrogen range from 0.0009 wt% to 0.0034 wt%, even though the HAZ has the tough mixed microstructure. Cooling time after welding influenced the HAZ microstructure and toughness as well, and maximum toughness was obtained when cooling produced the tough mixed microstructure. Therefore, for a high HAZ toughness, both nitrogen content and cooling time should be controlled to obtain the tough mixed microstructure and to keep the free nitrogen content low. The optimal nitrogen content and cooling time from 800 °C to 500 °C were 0.006 wt% and between 60 s and 100 s, respectively, in this experiment.     

Synthesis and characterization of highly dispersed TiO2 nanocrystal colloids by microwave-assisted hydrothermal method

Anatase TiO₂ nanocrystal colloids with high dispersion and photocatalytic activity were rapidly synthesized from peroxo-titanium-acid precursor by microwave-assisted hydrothermal method within 30?min at low temperature (120–180?°C). The transmission electron microscopy results indicate that the as-prepared TiO₂ have a narrow particle size distribution (25–29?nm) and high dispersion. The crystal structure of all these products are pure anatase phase (XRD, Raman), and they show good crystallinity and large surface area (N₂ adsorption–desorption measurements BET). The results of the UV–Visible absorbance and Fourier transform infrared spectra indicate that the surface peroxo group Ti(O₂) still remains in TiO₂ nanoparticles prepared by microwave-assisted hydrothermal method at 120?°C, and this surface peroxo group can be decomposed effectively by drying at 140?°C. The photocatalytic activity of the as-prepared TiO₂ were evaluated by the degradation of reactive brilliant red X-3B, it is found that the as-prepared TiO₂ exhibited good photocatalytic performance. Moreover, the existence of surface peroxo group greatly suppressed the photocatalytic activity of the TiO₂ nanoparticles.     

Preparation of bilayer graphene utilizing CuO as nucleation sites by CVD method

Graphene is an attractive 2D material for optoelectronics applications. However, due to the spontaneous nucleation characteristics of graphene growth on the metal substrates using chemical vapor deposition method, the polycrystalline graphene exhibited many crystal defects, leading to poor crystal quality. Properly controlling the density of nucleation sites is an important and necessary mean to increase the quality of graphene material. In this work, a new method to synthesize high-quality graphene on Cu substrate was reported by utilizing the CuO nanoparticles as nucleation sites. It was found that when annealing the copper substrate at 300 °C for 30 min with Ar:O₂ flow ratio of 64:1, the copper substrate showed the lowest roughness and the density of CuO nucleation sites after hydrogen etching (H₂ 21 sccm at 1035 °C). Bilayer graphene with diagonal length of ~?3 µm was successfully prepared centering on the CuO nucleation sites. This work supplied a new clue for high quality and monocrystalline graphene preparation.     

Fractography and transmission electron microscopy analysis of an Al-Li-Cu-Mg-Zr alloy displaying an improved fracture toughness

Al-2.3 wt% Li-1.8 wt% Mg-0.15 wt% Zr alloys with 0.1 and 0.45 wt% Cu were studied. The materials were cast, homogenized at 530°C for 24 h, extruded at 400°C with a reduction ratio of 30 : 1, solution treated at 528°C for 0.5 h and then artificially aged at 190°C to an overaged condition. The concerted application of light-, transmission electron- and scanning electron microscopy together with short rod fracture toughness measurements allowed the influence of low level Cu together with 0.15 wt% Zr on the fracture toughness of this alloy system to be studied. It was found that the addition of 0.1 wt% Cu together with 0.15 wt% Zr not only affected the δ′ precipitate nucleation and their size and size distribution through Li-Cu-v triple complexes but also affected the β′ dispersoid nucleation through Zr-Cu-v triple complexes. This in turn affected the size and size distribution of the δ′/β′ duplex precipitates. This causes an increase in the fracture toughness in underaged material artificially aged at 190°C. This effect was probed in an SEM fractographic investigation and by mechanical testing. This revised version was published online in November 2006 with corrections to the Cover Date.     

The Lyophilization of Dispersed Systems: Influence of Freezing Process,Freezing time,Freezing Temperature and RBCs Concentration on RBCs Hemolysis

ABSTRACT

In this work, we studied the influence of different parameters controlling cooling stage on biological dispersed system injury. The human red blood cell (RBCs) was chosen as work model. The study examined the influence of two freezing processes on RBCs hemolysis, one process producing big crystals, the other producing small crystals. Using both processes, we examined the effect of freezing temperature, freezing time, and RBCs concentration on injuries to RBCs. Freezing damage was assessed by the hematocrite measure before freezing and after thawing. The process producing a small number of big ice crystals (Pa) seems—in relation to the one producing a large number of small ice crystals (Pb)—to be less traumatic for the RBC, although the two are not statistically different. Freezing temperature and freezing time influence the preservation of RBCs. At 0 and ?20°C there were high preservation and total hemolysis, respectively. At ?5°C and ?10°C, the RBC hemolysis depends on freezing temperature and freezing time. The RBCs hemolysis rates increases when freezing time increases and when freezing temperature decreases. The rates of RBCs preserved decreases with RBCs concentration some with either the freezing process used (Pa or Pb). More, an accentuation of the difference between the two used freezing processes on RBCs hemolysis was retrieved. The analysis of the conductivity evolution within the RBCs suspension frozen showed that the destruction of the RBCs is had essentially to the solution effects. When the crystallization eutectic takes place, the RBCs are already completely destroyed.     

Low-temperature calcination of convenient micro-sized copper ink with surface activation and synchronous protection by in-situ chemisorbed cupric formate

The main problem of copper nanoparticle inks is the oxidation of copper nanoparticles because of the high reactivity. Therefore, less oxidable micro-sized copper particles become an ideal alternative copper source. However, micro-sized copper particles cannot sinter at low temperatures. In this study, with the combination of formic acid treatment and complexation with amine, the low-temperature calcination of micro-sized copper ink is achieved. Formic acid treatment can activate the surface of micro-sized copper particles, immediately followed by in situ chemisorbed cupric formate (CuF) on the surface to protect it from oxidation. 3-Dimethylamino-1,2-propanediol (DMAPD) can coordinate with the chemisorbed CuF on the surface and serve as a reducing agent during the calcination process. When the chemisorbed CuF–DMAPD decomposes to generate copper nanoparticles, the activated copper surface is exposed and serves as nucleation sites to form nano-channels. Finally a copper film with the resistivity of 19?±?2 μΩ cm was obtained after calcined at 180 °C for 10 min under N₂ atmosphere.

     

Dissolution and precipitation behavior of ternary solid dispersions of ezetimibe in biorelevant media

Abstract

The effects of different formulations and processes on inducing and maintaining the supersaturation of ternary solid dispersions of ezetimibe (EZ) in two biorelevant media fasted-state simulated intestinal fluid (FaSSIF) and fasted-state simulated gastric fluid (FaSSGF) at different temperatures (25?°C and 37?°C) were investigated in this work.

Ternary solid dispersions of EZ were prepared by adding polymer PVP-K30 and surfactant poloxamer 188 using melt-quenching and spray-drying methods. The resulting solid dispersions were characterized using scanning electron microscopy, differential scanning calorimetry (DSC), modulated DSC, powder X-ray diffraction and Fourier transformation infrared spectroscopy. The dissolution of all the ternary solid dispersions was tested in vitro under non-sink conditions.

All the prepared solid dispersions were amorphous in nature. In FaSSIF at 25?°C, the melt-quenched (MQ) solid dispersions of EZ were more soluble than the spray-dried (SD) solid dispersions and supersaturation was maintained. However, at 37?°C, rapid and variable precipitation behavior was observed for all the MQ and SD formulations. In FaSSGF, the melting method resulted in better solubility than the spray-drying method at both temperatures.

Ternary solid dispersions show potential for improving solubility and supersaturation. However, powder dissolution experiments of these solid dispersions of EZ at 25?°C may not predict the supersaturation behavior at physiologically relevant temperatures.     

Evaporative Drying of Aqueous Dispersions of Solid Lipid Nanoparticles

Solid lipid nanoparticles (SLNs) have been proposed as alternative colloidal drug carriers. SLNs are obtained by dispersing warm oil-in-water microemulsions into cold water. The aim of this research was to investigate an evaporative drying process for aqueous dispersions of SLNs. For this purpose, a special apparatus, namely, a thermostatic minidesiccator having alumina as the drying medium, was designed to carry out the evaporative drying at a controlled temperature. Besides the water removal kinetics, the mean particle size and the size distribution of SLNs were measured during the drying with the aim of detecting the highest temperature at which the drying process can be carried out without significantly affecting the SLN average diameter. The SLN dispersions were evaluated with and without a hydrophilic excipient, commonly used as a cryoprotector (trehalose). The drying temperature of 10°C was found to be the most suitable for obtaining SLNs as a powder, maintaining almost the same size as that of the SLNs in dispersion.     

A facile and green approach to prepare monodispersion nanonickel nanofluids

This paper first develops a novel approach to prepare solvent-free nanonickel (Ni) nanofluids via hydrogen bonding between poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) and 3-(Trimethoxysilyl)-1-propanethiol-modified Ni powder with average diameter of 80?nm to solve the problem of nanoparticles agglomerating due to the anisotropic dipolar attraction. It is interestingly found that Ni nanofluid is solid at room temperature while it undergoes solid–liquid transition without solvent at 50.7°C. The content of Ni is up to 12.1?wt%. The average diameter of core-shell structure of Ni nanofluids is 182?nm without agglomerations. It is worth noting that incorporation of Ni powder can elevate remarkably initial decomposition temperature of block copolymer due to high dispersity of Ni powder after modification. In addition, the viscosity of Ni nanofluids is found to be less than 10?Pa?·?s at 100°C, which is between that of water and honey, 0.001 and 10?Pa?·?s, respectively, at 20°C. More importantly, the Ni nanofluids exhibit excellent dispersion in water and other organic solvents for 2 months due to amphiphilic properties of the modifier molecule. These unique properties of Ni nanofluids may offer new scientific and technical opportunities for application of Ni powder in the form of liquid-like status.     

Reactions in frozen foods; the reactions of myosin and single amino acids with some aldehydesRéactions dans les aliments congelés; les réactions de la myosine et des acides aminés simples avec des aldéhydes

Malonaldehyde and related substances occur in foods as secondary decomposition products of oxidized polyunsaturated fatty acids. The reaction of malonaldehyde (and glycoaldehyde) with rabbit myosin or single amino acids (glycine, lysine methionine or asparagine) was studied in vitro for its potential to cause protein denaturation in muscle. The reactions were followed at nine temperatures between 45°C and ?40°C. At each temperature the influence of pH (5.2, 7.0, 9.2) and ionic strength (0.3, 0.6) was examined, and the influence of the freezing rate on the reaction rates was also investigated. The decrease of malonaldehyde concentration in the reaction mixture was followed by the TBA-test.The temperature-dependence of reaction rates was very similar for all the reactions. As expected, the rate of reaction decreases when the temperature is reduced from 45°C to freezing point. However, when the mixture is frozen the reaction rate increases with decreasing temperature down to ?24°C. Further lowering of the temperature to ?40°C showed a reduction again in the reaction rate. There was no difference in the reaction rate for different ionic strengths. Lowering of pH gave an increase in reaction rate. A low freezing rate gave a higher reaction rate than was obtained with a fast freezing rate.The observed increase in the rate of reaction between malonaldehyde and protein components when lowering the temperature from the freezing point to the eutectic point is explained on the basis of the so-called ‘freeze concentration effect’ and a consequent pH-shift to values more favourable to the reactions.     

Effect of interfacial compounds on mechanical properties of titanium–steel vacuum roll-cladding plates

The titanium–steel clad plates were prepared by vacuum roll cladding. Ti–Fe compounds and TiC were observed at different cooling rates after rolling. Optical microscopy, electron microprobe analyser, X-ray diffraction and shear test studies were carried out to study the effect of Ti–Fe compounds and TiC on the ultimate microstructure and mechanical properties of titanium–steel clad plates. At a cooling rate of 6.2°C/min, TiC and Ti–Fe compounds seriously impacted the mechanical properties of the clad plate. At a cooling rate of 1.8°C/min, the thickness of the TiC layer was optimal much that the maximum shear strength of 296?MPa was obtained. At a cooling rate of 0.6°C/min, the thickness of the TiC layer was relatively thick, which affected the mechanical properties of clad plates.     

Preparation and properties of glass-ceramic materials obtained by recycling goethite industrial waste

The recycling of toxic goethite waste, originated in the hydrometallurgy of zinc ores, in glass-ceramic matrices has been studied. Oxide compositions suitable to form glasses were prepared by mixing the goethite waste with granite scraps and glass cullet, yielding the following oxide composition (wt%): SiO₂, 44.6; Al₂O₃, 3.3; Fe₂O₃, 25.5; MgO, 1.6; CaO, 4.5; Na₂O, 5.9; PbO, 3.1; ZnO, 6.5; K₂O, 1.0; TiO₂, 2.0; other 2.0. By proper addition of carbon powder, the initial Fe³⁺/Fe²⁺ ratio (12) of glasses melted in air at 1450 °C was approximated to the stoichiometric value of magnetite (2) to obtain high nucleation and crystallization rates. The heat treatment of iron supersaturated goethite glasses above 630 °C led to the formation of magnetite nuclei with a high tendency to grow and coalesce with time. The crystallization of pyroxene, occurring on the magnetite crystals above 800 °C, was found to be influenced by the nucleation period, so that the highest crystalline volume fraction, V _f (0.80–0.85), was obtained for 90–120 min nucleation time at 670 °C and 120 min crystallization at 860 °C. This revised version was published online in November 2006 with corrections to the Cover Date.     

Low indium content In–Zn–O system towards transparent conductive films: structure,properties and comparison with AZO and GZO

In this work, low content indium doped zinc oxide (IZO) thin films were deposited on glass substrates by RF magnetron sputtering using IZO ceramic targets with the In₂O₃ doping content of 2, 6, and 10 wt%, respectively. The influences of In₂O₃ doping content and substrate temperature on the structure and morphology, electrical and optical properties, and environmental stability of IZO thin films were investigated. It was found that the 6 wt% doped IZO thin film deposited at 150?°C exhibited the best crystal quality and the lowest resistivity of 9.87?×?10^?4 Ω cm. The corresponding Hall mobility and carrier densities were 9.20 cm² V^?1 s^?1 and 6.90?×?10²⁰ cm^?3, respectively. Compared with 2 wt% Al₂O₃ doped ZnO and 5 wt% Ga₂O₃ doped ZnO thin films, IZO thin film with the In₂O₃ doping content of 6 wt% featured the lowest surface roughness of 1.3 nm. It also showed the smallest degradation with the sheet resistance increased only about 4.4% at a temperature of 121?°C, a relative humidity of 97% for 30 h. IZO thin film with 6 wt% In₂O₃ doping also showed the smallest deterioration with the sheet resistance increased only about 2.8 times after heating at 500?°C for 30 min in air. The results suggested that low indium content doped ZnO thin films might meet practical requirement in environmental stability needed optoelectronic devices.     

Effect of temperature on the fracture behaviour of heat‐treated Al–Cu–Li alloy laser welds under low‐cycle fatigue loading

The paper presents the results of the studies of the effect of temperature on the fracture behaviour of Al–Cu–Li alloy laser welds under low‐cycle fatigue loading. The mechanical properties and the microstructure of the welded joints without and after postweld heat treatment (PWHT) were investigated. The tensile strength and the low‐cycle fatigue resistance of the welded joints were studied at various test temperatures (20°C, 85°C and ? 60°C). It was been found that heating up to 85°C and cooling down to ?60°C reduced the maximum number of loading cycles of the welded joints after PWHT by 1.5–2.0 times compared with that at a test temperature of 20°C.     

Acalypha indica–mediated green synthesis of ZnO nanostructures under differential thermal treatment: Effect on textile coating,hydrophobicity, UV resistance,and antibacterial activity

In this study, ZnO nanoparticles were green-synthesized from Acalypha indica leaf extract using zinc acetate as a precursor. The prepared ZnO nanoparticles were calcined at three different temperatures, namely 100, 300, and 600?°C. The structure/morphology of the green-synthesized ZnO nanoparticles was ascertained through X-ray diffraction, particle size analysis, scanning electron microscopy, transmission electron microscopy, and surface area analysis techniques. It was observed from the physico-chemical and biological characterization studies that ZnO nanoparticles calcined at high temperature (600?°C) exhibit high surface area (230?m²?g^?1) and small particle size (20?nm) with good antibacterial activity against Escherichia coli (22.89?±?0.06?mm) and Staphylococcus aureus (24.62?±?0.08?mm). In addition, cotton fabrics coated with these nanoparticles showed higher UV-protection (87.8?UPF), hydrophobicity (155°), and maximum zone of bacterial inhibition against E. coli and S. aureus (25.13?±?0.05 mm and 30.17?±?0.03?mm) than those coated with particles calcined at 100?°C and 300?°C. High temperature calcination has a vital role in the crystallization of the particles towards nanoscale with increased resistivity to UV exposure, washing treatments, and microbial infection in fabrics. Thus, the cost-effective ZnO nanoparticles obtained through green synthesis method proves their potential applications in the field of biomedical, textile, and cosmetic applications.     

Synthesis of platinum single-crystal nanoparticles in water vapor

Platinum (Pt) nanoparticles have broad application in automobile pollution control, sensors, and fuel cells. Single-crystal platinum particles over the range of nano- to micron-meters were synthesized at the Pt/SiC interface in high pressure water vapor at 1200 °C. These particles exhibited a cube–octahedral shape with predominant (111) facets. Formation of the Pt particles is likely due to water vapor-facilitated oxidation of the platinum silicide, resulting from the interaction between SiC and Pt. Well-aligned Pt single-crystal particles with sizes of tens to hundreds nanometers were obtained on the surface of arc-melted Pt₂Si after exposure in flowing water vapor (90 cm/min) at 1200 °C for 5 min. The potential applications of this finding are discussed.     

Photoelectrochemical properties of TiO2 nanotube arrays: effect of electrolyte pH and annealing temperature

The effect of electrolyte pH and annealing temperature on the formation of TiO₂ nanotube arrays in connection with the photoelectrochemical response was investigated in this article. Well-aligned TiO₂ nanotube arrays were fabricated by anodisation of Ti foil in an electrolyte consisting of 1?M of glycerol (85?wt% of glycerol and 15?wt% of water) with 0.5?wt% of NH₄F at 30?V for 30?min. The pH of the electrolyte was varied from pH 1 to 7. With the increase of electrolyte pH to neutral condition, the length of the nanotube arrays was increased from ～320 to 1100?nm. As-anodised TiO₂ nanotube arrays were amorphous in nature. However, anatase phase was observed after annealing at 400°C and polycrystalline anatase and rutile phase could be observed by heating up to 500°C in air atmosphere. Based on the results obtained, the length and crystalline phases of TiO₂ nanotube arrays affect the performance of photoelectrochemical response and photoconversion efficiency significantly.