• Journal of Powder Materials
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• v.22 no.6
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• pp.396-402
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• 2015

The organic binder-free paste for dye-sensitized solar cell (DSSC) has been investigated using peroxo titanium complex. The crystal structure of $TiO_2$ nanoparticles, morphology of $TiO_2$ film and electrical properties are analyzed by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Electrochemical Impedance Spectra (EIS), and solar simulator. The synthesized $TiO_2$ nanopowders by the peroxo titanium complex at 150, 300, $400^{\circ}C$, and $450^{\circ}C$ have anatase phase and average crystal sizes are calculated to be 4.2, 13.7, 16.9, and 20.9 nm, respectively. The DSSC prepared by the peroxo titanium complex binder have higher $V_{oc}$ and lower $J_{sc}$ values than that of the organic binder. It can be attributed to improvement of sintering properties of $TCO/TiO_2$ and $TiO_2/TiO_2$ interface and to formation of agglomerate by the nanoparticles. As a result, we have investigated the organic binder-free paste and 3.178% conversion efficiency of the DSSC at $450^{\circ}C$.

• Journal of Powder Materials
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• v.23 no.2
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

• Journal of Powder Materials
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• v.23 no.4
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• pp.325-330
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• 2016

Owing to increasing demand of rare metals present in ICT products, it is necessary to promote the rare metal recycling industry from an environmental viewpoint and to prevent climate change. Despite the fact that information for toxic substances is partly indicated, a legal basis and an international standard indicating usage of rare metals is insufficient. In order to address this issue, a newly created study group of environment and climate change at the ITU (International Telecommunication Union) is doing research to develop methodologies for recycling rare metals from ICT products in an eco-friendly way. Under this group, the Republic of Korea has established two international standards related to rare metals present in ICT products. The first is 'Release of rare metal information for ICT products (ITU-T L.1100)' and the other is 'Quantitative and qualitative analysis methods for rare metals (ITU-T L.1101)'. A new proposal for recommending the provision of rare metal information through a label by manufacturers and consumer/recycling businesses has been approved recently and is supposed to be published later in 2016. Moreover, these recommendations are also being extended to IEC, ISO and other standardization organizations and a strategy to reinforce the ability for domestic standardization is being established in accordance with industrial requirements. This will promote efficient recycling of rare metals from ICT products and will help improve the domestic supply of rare metals.

• Journal of Powder Materials
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• v.22 no.6
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• pp.385-390
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• 2015

We report a synthesis of non-toxic InP nanocrystals using non-pyrolytic precursors instead of pyrolytic and unstable tris(trimethylsilyl)phosphine, a popular precursor for synthesis of InP nanocrystals. In this study, InP nanocrystals are successfully synthesized using hexaethyl phosphorous triamide (HPT) and the synthesized InP nanocrystals showed a broad and weak photoluminescence (PL) spectrum. As synthesized InP nanocrystals are subjected to further surface modification process to enhance their stability and photoluminescence. Surface modification of InP nanocrystals is done at $230^{\circ}C$ using 1-dodecanethiol, zinc acetate and fatty acid as sources of ZnS shell. After surface modification, the synthesized InP/ZnS nanocrystals show intense PL spectra centered at the emission wavelength 612 nm through 633 nm. The synthesized InP/ZnS core/shell structure is confirmed with X-ray diffraction (XRD) and Inductively Coupled Plasma - Atomic Emission Spectrometer (ICP-AES). After surface modification, InP/ZnS nanocrystals having narrow particle size distribution are observed by Field Emission Transmission Electron Microscope (FE-TEM). In contrast to uncapped InP nanocrystals, InP/ZnS nanocrystals treated with a newly developed surface modified procedure show highly enhanced PL spectra with quantum yield of 47%.

• Journal of Powder Materials
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• v.23 no.4
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• pp.311-316
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• 2016

$Ni(OH)_2$ hollow spheres have been prepared by solvent displacement crystallization using a micro-injection device, and the effect of process parameters such as concentration and the relative ratio of the injection speed of the precursor solution, which is an aqueous solution of $NiSO_4{\cdot}6H_2O$, to isopropyl alcohol of displacement solvent have been investigated. The crystal phases after NaOH treatment are in the ${\beta}-phase$ for all process parameters. A higher concentration of $NiSO_4{\cdot}6H_2O$ aqueous solution is injected by a micro-injection device and bigger $Ni(OH)_2$ hollow spheres with a narrower particle size distribution are formed. The crystallinity and hardness of the as-obtained powder are so poor that hydrothermal treatment of the as-obtained $Ni(OH)_2$ at $120^{\circ}C$ for 24 h in distilled water is performed in order to greatly improve the crystallinity. It is thought that a relative ratio of the injection speed of $NiSO_4{\cdot}6H_2O$ to that of isopropyl alcohol of at least more than 1 is preferable to synthesize Ni(OH)2 hollow spheres. It is confirmed that this solution-based process is very effective in synthesizing ceramic hollow spheres by simple adjustment of the process parameters such as the concentration and the injection speed.

• Journal of Powder Materials
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• v.23 no.2
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• pp.108-111
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• 2016

$Y_2O_3-H_3BO_3:Eu^{3+}$ powders are synthesized using a mechanical alloying method, and their photoluminescence (PL) properties are investigated through luminescence spectrophotometry. For samples milled for 300 min, some $Y_2O_3$ peaks ([222], [440], and [622]) and amorphous formations are observed. The 300-min-milled mixture annealed at $800^{\circ}C$ for 1 h with Eu = 8 mol% has the strongest PL intensity at every temperature increase of $100^{\circ}C$ (increasing from 700 to $1200^{\circ}C$ in $100^{\circ}C$ increments). PL peaks of the powder mixture, as excited by a xenon discharge lamp (20 kW) at 240 nm, are detected at approximately 592 nm (orange light, $^5D_o{\rightarrow}^7F_1$), 613 nm, 628 nm (red light, $^5D_o{\rightarrow}^7F_2$), and 650 nm. The PL intensity of powder mixtures milled for 120 min is generally lower than that of powder mixtures milled for 300 min under the same conditions. PL peaks due to $YBO_3$ and $Y_2O_3$ are observed for 300-min-milled $Y_2O_3-H_3BO_3$ with Eu = 8 mol% after annealing at $800^{\circ}C$ for 1 h.

• Journal of Powder Materials
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• v.23 no.4
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• pp.303-306
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• 2016

An optimum route to synthesize Ti-Mo system powders is investigated by analyzing the effect of the heat treatment atmosphere on the formation of the reaction phase by dehydrogenation and hydrogen reduction of ball-milled $TiH_2-MoO_3$ powder mixtures. Homogeneous powder mixtures with refined particles are prepared by ball milling for 24 h. XRD analysis of the heat-treated powder in a hydrogen atmosphere shows $TiH_2$ and $MoO_3$ peaks in the initial powders as well as the peaks corresponding to the reaction phase species, such as $TiH_{0.7}$, TiO, $MoO_2$, Mo. In contrast, powder mixtures heated in an argon atmosphere are composed of Ti, TiO, Mo and $MoO_3$ phases. The formation of reaction phases dependent on the atmosphere is explained by the partial pressure of $H_2$ and the reaction temperature, based on thermodynamic considerations for the dehydrogenation reaction of $TiH_2$ and the reduction behavior of $MoO_3$.

• Journal of Powder Materials
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• v.23 no.2
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• pp.95-101
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• 2016

Carbon nanofiber (CNF) composites coated with spindle-shaped $Fe_2O_3$ nanoparticles (NPs) are fabricated by a combination of an electrospinning method and a hydrothermal method, and their morphological, structural, and chemical properties are measured by field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. For comparison, CNFs and spindle-shaped $Fe_2O_3$ NPs are prepared by either an electrospinning method or a hydrothermal method, respectively. Dye-sensitized solar cells (DSSCs) fabricated with the composites exhibit enhanced open circuit voltage (0.70 V), short-circuit current density ($12.82mA/cm^2$), fill factor (61.30%), and power conversion efficiency (5.52%) compared to those of the CNFs (0.66 V, $11.61mA/cm^2$, 51.96%, and 3.97%) and spindle-shaped $Fe_2O_3$ NPs (0.67 V, $11.45mA/cm^2$, 50.17%, and 3.86%). This performance improvement can be attributed to a synergistic effect of a superb catalytic reaction of spindle-shaped $Fe_2O_3$ NPs and efficient charge transfer relative to the one-dimensional nanostructure of the CNFs. Therefore, spindle-shaped $Fe_2O_3$-NP-coated CNF composites may be proposed as a potential alternative material for low-cost counter electrodes in DSSCs.

• Journal of Powder Materials
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• v.23 no.2
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• pp.91-94
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• 2016

High-quality colloidal CdSe/ZnS (core/shell) is synthesized using a continuous microreactor. The particle size of the synthesized quantum dots (QDs) is a function of the precursor flow rate; as the precursor flow rate increases, the size of the QDs decreases and the band gap energy increases. The photoluminescence properties are found to depend strongly on the flow rate of the CdSe precursor owing to the change in the core size. In addition, a gradual shift in the maximum luminescent wave (${\lambda}_{max}$) to shorter wavelengths (blue shift) is found owing to the decrease in the QD size in accordance with the quantum confinement effect. The ZnS shell decreases the surface defect concentration of CdSe. It also lowers the thermal energy dissipation by increasing the concentration of recombination. Thus, a relatively high emission and quantum yield occur because of an increase in the optical energy emitted at equal concentration. In addition, the maximum quantum yield is derived for process conditions of 0.35 ml/min and is related to the optimum thickness of the shell material.

• Journal of Powder Materials
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• v.23 no.4
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• pp.287-296
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• 2016

$Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using $NH_4OH$ as a chelating agent. The co-precipitation temperature is varied in the range of $30-80^{\circ}C$. Calcination of the prepared precursors with $Li_2CO_3$ for 8 h at $1000^{\circ}C$ in air results in Li $Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ powders. Two kinds of obtained powders have been characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analyzer, and tap density measurements. The co-precipitation temperature does not differentiate the XRD patterns of precursors as well as their final powders. Precursor powders are spherical and dense, consisting of numerous acicular or flaky primary particles. The precursors obtained at 70 and $80^{\circ}C$ possess bigger primary particles having more irregular shapes than those at lower temperatures. This is related to the lower tap density measured for the former. The final powders show a similar tendency in terms of primary particle shape and tap density. Electrochemical characterization shows that the initial charge/discharge capacities and cycle life of final powders from the precursors obtained at 70 and $80^{\circ}C$ are inferior to those at $50^{\circ}C$. It is concluded that the optimum co-precipitation temperature is around $50^{\circ}C$.