• Textile Coloration and Finishing
• /
• v.3 no.1
• /
• pp.8-16
• /
• 1991

In order to investigate the fine structure of PET films, PET films were stretchd at various draw ratios (2, 3, 4, 5) below $T_g$ ($72^{\circ}C$) and then annealed at various temperatures (125, 150, 175, $200^{\circ}C$) under free-annealed (FA) and taut-annealed (TA) conditions. Such changes as thermal shrinkage, crystallinity, crystallite size, dynamic viscoelasticity and thermal behaviour were measured in relation to the draw ratio and annealing condition.The following results were obtained. 1. Thermal shirinkage increased with increasing annealing temperature and draw ratio, but decreased in case of draw ratio 4 (draw ratio 3 at $200^{\circ}C$) and above it. 2. The degree of crystallinity of FA samples were higher than those of TA samples. 3. Tan 5 of TA samples were less than those of FA samples, and storage moduli (E') and loss moduli (E") of FA samples were less than those of TA samples; moreover, maximum tan '||'&'||' temperature of FA samples were shifted toward higher temperature than those of TA samples. 4. The melting endotherm ($T_m$) and heat of fusion $(\DeltaH)$ of the PET film increased with the draw ratio and annealing temperature; in addition, premelting endotherm ($T_m$) and heat of fusion $(\DeltaH)$ of the local crystallization in the FA samples were larger than those of TA samples. 5. The X-ray diffraction pattern displayed sharp peaks gradually with the draw ratio and annealing temperature. 6. Crystallite sizes of FA samples were larger than those of TA samples.

• Journal of the Korean Ceramic Society
• /
• v.24 no.2
• /
• pp.123-132
• /
• 1987

Yttria-stabilized zirconia with erbia-lanthana were investigated with respect to the amount of Ln2O3 (Ln; Er, La) addition in the range of 0.5∼5 mol% to the base composition of 8 mol% yttriazirconia. Following analysis and measurement were adopted for the characterization of synthesizes of solid electrolyte; phase transformation, lattice parameter, crystallite size, relative density, chemical composition and SEM/EDS. Electrical conductivity by two-probe method versus temperature from 350$^{\circ}C$ to 800$^{\circ}C$ and frequency in the range of 5Hz∼13MHz by complex impedance method was also conducted together with the determination of oxygen ion transference number by EMF method for the evaluation of their electrical properties. The results were as followsing; Electrical conductivity were decreased with increase in Ln2O3 content, but their activation energies increased. In the case of La2O3 addition, espicially, its electrical conductivity was decreased owing to the segregation of second phases at the grain-boundary. Grain-boundary conductivity of the specimen contained 0.5 mol% Er2O3 exhibited a maximum conductivity among thecompositions experimented. However, their bulk conductivities decreased in both case. Oxygen ion transference number was also reduced with decrease in oxygen partial pressure. For example, in the case of Er2O3 addition it retained value in the range of 0.97∼0.94 abvove 4.74${\times}$10-2in oxygen partial pressure. With the increase in the quantities of the evaporation of additive components, the crystallite size of stabilized zirconia decreased, and their relative density also reduced owing to the formation of porosity in their matrices. In the case of La2O3 the sinterbility was improved in the limited amount of addition up to 0.5 mol%, in the same range of addition the strength of sintered bodies were improved perhaps owing to the precipitation of metastable tetragonal phase in the fully stabilized zirconia.

• Bulletin of the Korean Chemical Society
• /
• v.31 no.1
• /
• pp.47-51
• /
• 2010

A powder, containing 80 percent of blue cobalt aluminate $(CoAl_2O_4)$ crystallites, was synthesized at $210 ^{\circ}C$ using a (metal nitrate-malonic acid-ammonium hydroxide-ammonium nitrate) system. The optimal amount of concentrated ammonia water and initial decomposition temperature were determined for the blue $CoAl_2O_4$ crystallites preparation. Three $CoAl_2O_4$ precursor pastes, corresponding to the various amounts of concentrated ammonia water, were prepared by evaporating the initial solutions in an electric furnace fixed at $80 ^{\circ}C$ under a vacuum of 25 torr. The initial solution was used to dissolve the starting materials. The powder with the maximum content (80%) of blue $CoAl_2O_4$ crystallites was prepared when the prepared precursor was decomposed at $210 ^{\circ}C$. The blue $CoAl_2O_4$ crystallite content in the prepared sample decreased with increasing initial decomposition temperature. For 0.2 mole of the $Al^{3+}$ ion, the chemical compositions of the precursor corresponded to molar ratios of 0.4, 1.40, 2.56 and 2.00 for the $Co^{2+}$ ion, malonic acid, ammonia and ammonium nitrate per mole of the $Al^{3+}$ ion, respectively. The blue $CoAl_2O_4$ crystallite content in the sample decreased with the amount of ammonia deviated from the optimal value. The characteristics of the powders were examined using X-ray diffraction, optical microscopy, Fourier transformation infrared spectroscopy and the Brunauer-Emmett-Teller technique.

• Journal of the Korean Chemical Society
• /
• v.62 no.2
• /
• pp.118-123
• /
• 2018

The hexagonal tungsten bronze $Cs_xWO_3$ nanoparticle was synthesized by a chemical coprecipitation method of ammonium tungstate and $Cs_2CO_3$ in acidic condition. This synthetic method for cesium tungsten bronze is reported for the first time as far as we know. The synthesized $Cs_xWO_3$ as precipitated showed a weak crystallinity of hexagonal unit cell with a crystallite size of about 4 nm without annealing. When the synthesized $Cs_xWO_3$ was annealed in $N_2$ atmosphere, the crystallinity and crystallite size systematically increased maintaining the typical hexagonal tungsten bronze structure as the annealing temperature increased. The analyzed Cs content in the bronze was about 0.3 vs W, which is very close to the theoretical maximum value, 1/3 in cesium tungsten bronze. According to XPS analysis, the reduced tungsten ions existed as both the forms of $W^{5+}$ and $W^{4+}$ and the contents systematically increased as the annealing temperature increased up to $800^{\circ}C$. The $Cs_xWO_3$ thin films on PET substrate were also prepared by a wet-coating method using the ball-milled solution of the annealed $Cs_xWO_3$ nanoparticles at various temperatures. The near-infrared shielding property of these thin films increased systematically as the annealing temperature increased up to $800^{\circ}C$ as expected with the increased contents of reduced tungsten ions.

• Journal of Powder Materials
• /
• v.27 no.3
• /
• pp.226-232
• /
• 2020

Bismuth vanadate (BiVO₄) is considered a potentially attractive candidate for the visible-light-driven photodegradation of organic pollutants. In an effort to enhance their photocatalytic activities, BiVO₄ nanofibers with controlled microstructures, grain sizes, and crystallinities are successfully prepared by electrospinning followed by a precisely controlled heat treatment. The structural features, morphologies, and photo-absorption performances of the asprepared samples are systematically investigated and can be readily controlled by varying the calcination temperature. From the physicochemical analysis results of the synthesized nanofiber, it is found that the nanofiber calcines at a lower temperature, shows a smaller crystallite size, and lower crystallinity. The photocatalytic degradation of rhodamine-B (RhB) reveals that the photocatalytic activity of the BiVO₄ nanofibers can be improved by a thermal treatment at a relatively low temperature because of the optimization of the conflicting characteristics, crystallinity, crystallite size, and microstructure. The photocatalytic activity of the nanofiber calcined at 350℃ for the degradation of RhB under visible-light irradiation exhibits a greater photocatalytic activity than the nanofibers synthesized at 400℃ and 450℃.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.2
• /
• pp.622-628
• /
• 2013

Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.33 no.6
• /
• pp.483-489
• /
• 2020

BaTiO₃ powder was synthesized by a solid-state reaction using BaCO₃ and TiO₂. Different calcination temperatures (800℃, 850℃, 900℃, and 950℃) were set to investigate their effects on the properties of BaTiO₃ powder. The synthesized BaTiO₃ phase was confirmed to be a single phase by XRD, and the tetragonality (c/a) and crystallite size were calculated. Thereafter, each calcinated BaTiO₃ was sintered at five different sintering temperatures (1,100℃, 1,150℃, 1,200℃, 1,250℃, and 1,300℃), and the tetragonality, density, porosity, dielectric constant, and grain size were measured. As the calcination temperature increased, the tetragonality and crystallite size also increased, to 1.008 and 66 nm, respectively, at 950℃. Moreover, most pellets showed increased density, dielectric constant, and tetragonality as the sintering temperature increased up to 1,250℃; the same parameters slightly decreased at 1,300℃. It is noteworthy that the tetragonality of BaTiO₃ at 1,250℃ exhibits a very high c/a value of 1.0084. In addition, the grain size and dielectric constant measured near the Curie temperature increased as the sintering temperature increased.

• Applied Chemistry for Engineering
• /
• v.23 no.2
• /
• pp.169-175
• /
• 2012

In the study, the effects of $130{\sim}150^{\circ}C$ annealing condition and 1~10 wt% isopropylphenyl diphenyl phosphate (IPPP) on crystallization behavior and flame retardancy of a full name (PLA) film were determined. The crystallization kinetics of PLA films with adding 1, 5, and 10 wt% IPPP at $140^{\circ}C$ were higher than those at 130 and $150^{\circ}C$. The average crystallinity and crystallite size of PLA film with 1 wt% IPPP were 21.3% and 24.8 nm, respectively. With an increasing IPPP content, the crystallinity of PLA film increased and the crystallite size decreased. The burning rate lowered with an increasing IPPP content as well.

• Advances in nano research
• /
• v.7 no.4
• /
• pp.233-240
• /
• 2019

The present research work reports in-vitro anti-cancer activity of biologically synthesized ZnO nanoparticles (ZnO NPs) against human carcinoma cells viz SCC-40, SK-MEL-2 and SCC-29B using Sulforhodamine-B (SRB) Assay. ZnO NPs were synthesized by a unique and novel biological route using Temperature-gradient phenomenon where the extract of combination of Catharanthus roseus (L.) G. Don (C. roseus), Azadirachta indica (A. indica), Ficus religiosa (F. religiosa) and NaOH solution were used as synthesis medium. The morphology of the ZnO NPs was characterized by Transmission Electron Microscopy (TEM). TEM images reveal that particle size of the samples reduces from 76 nm to 53 nm with the increase in reaction temperature and 68 nm to 38 nm with the increase in molar concentration of NaOH respectively. XRD study confirms the presence of elements and reduction in crystallite size with increase in reaction temperature and NaOH concentration. The diffraction peaks show broadening and a slight shift towards lower Bragg angle ($2{\theta}$) which represents the reduction in crystallite size as well as presence of uniform strain. The FTIR spectra of the extract show transmittance peak fingerprint of Zn-O bond and presence of bioactive molecules These NPs exhibit inhibition greater than 50% for SCC-40, SK-MEL-2 and SCC-29B cell lines and more than 50% cell kill for SCC-29B cells at concentrations < $80{\mu}g/ml$. Nanoparticles with smallest size have shown better anti-cancer activity and peculiar cell-selectivity. The combination of extracts of these plants with ZnO NPs can be used in targeted drug delivery as an effective anti-cancer agent, a potential application in cancer treatment.

• Journal of Ceramic Processing Research
• /
• v.20 no.2
• /
• pp.158-163
• /
• 2019

Er3+/Yb3+-codoped NaLa(MoO4)2 colloidal nanocrystals were synthesized by pulsed laser ablations in de-ionized water and sodium dodecyl sulfate (NaC12H25SO4, SDS) aqueous solution for up-conversion (UC) luminescence bio-labeling applications. The influences of the SDS molecules on the crystallinities, crystal morphologies, crystallite sizes, and UC luminescence properties of the prepared Er3+/Yb3+-codoped NaLa(MoO4)2 colloidal nanocrystals were investigated in detail. Under a 980-nm excitation, the Er3+/Yb3+-codoped nanocolloidal NaLa(MoO4)2 suspension exhibited a weak red emission near 670 nm and strong green UC emissions at 530 and 550 nm, corresponding to the intra 4f transitions of Er3+ (4F9/2, 2H11/2, 4S3/2) → Er3+ (4I15/2). When the SDS solution was used, a smaller average crystallite size, narrower size distribution, and enhanced UC luminescence were observed. These characteristics were attributed to the amphoteric SDS molecules attached to the positively charged Er3+/Yb3+-codoped NaLa(MoO4)2 colloidal nanocrystals, effectively occupying the oxygen defect on their surfaces. The Er3+/Yb3+-codoped nanocrystalline NaLa(MoO4)2 suspension prepared in the SDS solution exhibited a remarkably strong green emission visible to the naked eyes.