• Journal of Powder Materials
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• v.24 no.1
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• pp.41-45
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• 2017

The effects of the heat treatment temperature and of the atmosphere on the dehydrogenation and hydrogen reduction of ball-milled $TiH_2-WO_3$ powder mixtures are investigated for the synthesis of Ti-W powders with controlled microstructure. Homogeneously mixed powders with refined $TiH_2$ particles are successfully prepared by ball milling for 24h. X-ray diffraction (XRD) analyses show that the powder mixture heat-treated in Ar atmosphere is composed of Ti, $Ti_2O$, and W phases, regardless of the heat treatment temperature. However, XRD results for the powder mixture, heat-treated at $600^{\circ}C$ in a hydrogen atmosphere, show $TiH_2$ and TiH peaks as well as reaction phase peaks of Ti oxides and W, while the powder mixture heat-treated at $900^{\circ}C$ exhibits only XRD peaks attributed to Ti oxides and W. The formation behavior of the reaction phases that are dependent on the heat treatment temperature and on the atmosphere is explained by thermodynamic considerations for the dehydrogenation reaction of $TiH_2$, the hydrogen reduction of $WO_3$ and the partial oxidation of dehydrogenated Ti.

• Journal of Powder Materials
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• v.20 no.2
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• pp.100-106
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• 2013

Ultra-fine zirconium carbide (ZrC) powder with nano-sized primary particles was synthesized by the carbothermal reduction method by using nano-sized $ZrO_2$ and nano-sized graphite powders mixture. The synthesized ZrC powder was well dispersed after simple milling process. After heat-treatment at $1500^{\circ}C$ for 2 h under vacuum, ultra-fine ZrC powder agglomerates (average size, $4.2{\mu}m$) were facilely obtained with rounded particle shape and particle size of ~200 nm. Ultra-fine ZrC powder with an average particle size of 316 nm was obtained after ball milling process in a planetary mill for 30 minutes from the agglomerated ZrC powder.

• Journal of Powder Materials
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• v.23 no.3
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• pp.202-206
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• 2016

A Ni-Ti-B alloy powder prepared by mechanical alloying (MA) of individual Ni, Ti, and B components is examined with the aim of elucidating the phase transitions and crystallization during heat treatment. Ti and B atoms penetrating into the Ni lattice result in a Ni (Ti, B) solid solution and an amorphous phase. Differential thermal analysis (DTA) reveals peaks related to the decomposition of the metastable Ni (Ti, B) solid solution and the separation of equilibrium $Ni_3Ti$, $TiB_2$, and ${\tau}-Ni_20Ti_3B_6$ phases. The exothermal effects in the DTA curves move to lower temperatures with increasing milling time. The formation of a $TiB_2$ phase by annealing indicates that the mechanochemical reaction of the Ni-Ti-B alloy does not comply with the alloy composition in the ternary phase diagram, and Ti-B bonds are found to be more preferable than Ni-B bonds.

• Journal of Korean Society for Atmospheric Environment
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• v.33 no.4
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• pp.297-305
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• 2017

In this study, the activity and structural properties of catalysts prepared by mechanochemical method under dry condition were studied. A dry milling was used as a mechanochemical method. The precursors of vanadium were $NH_4VO_3$ and $V_2O_5$. The activity and characterization of the catalysts prepared by dry milling were compared with those prepared by impregnation. In addition, the correlation between the catalytic activity and the structural characteristics was observed through XRD, Raman, and $H_2$-TPR analysis. As a result, the monomeric vanadate species exhibited excellent redox characteristics, which were confirmed to be related to the catalytic activity.

• Korean Journal of Materials Research
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• v.27 no.9
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• pp.507-511
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• 2017

An optimum route to fabricate oxide dispersion strengthened ferritic superalloy with desired microstructure was investigated. Two methods of high energy ball milling or polymeric additive solution route for developing a uniform dispersion of $Y_2O_3$ particles in Fe-Cr-Al-Ti alloy powders were compared on the basis of the resulting microstructures. Microstructural observation revealed that the crystalline size of Fe decreased with increases in milling time, to values of about 15-20 nm, and that an FeCr alloy phase was formed. SEM and TEM analyses of the alloy powders fabricated by solution route using yttrium nitrate and polyvinyl alcohol showed that the nano-sized Y-oxide particles were well distributed in the Fe based alloy powders. The prepared powders were sintered at 1000 and $1100^{\circ}C$ for 30 min in vacuum. The sintered specimen with heat treatment before spark plasma sintering at $1100^{\circ}C$ showed a more homogeneous microstructure. In the case of sintering at $1100^{\circ}C$, the alloys exhibited densified microstructure and the formation of large reaction phases due to oxidation of Al.

• Journal of Powder Materials
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• v.30 no.4
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• pp.332-338
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• 2023

Thermite welding is an exceptional process that does not require additional energy supplies, resulting in welded joints that exhibit mechanical properties and conductivity equivalent to those of the parent materials. The global adoption of thermite welding is growing across various industries. However, in Korea, limited research is being conducted on the core technology of thermite welding. Currently, domestic production of thermite powder in Korea involves recycling copper oxide (CuO). Unfortunately, controlling the particle size of waste CuO poses challenges, leading to the unwanted formation of pores and cracks during thermite welding. In this study, we investigate the influence of powder particle size on thermite welding in the production of Cu-thermite powder using waste CuO. We conduct the ball milling process for 0.5-24 h using recycled CuO. The evolution of the powder shape and size is analyzed using particle size analysis and scanning electron microscopy (SEM). Furthermore, we examine the thermal reaction characteristics through differential scanning calorimetry. Additionally, the microstructures of the welded samples are observed using optical microscopy and SEM to evaluate the impact of powder particle size on weldability. Lastly, hardness measurements are performed to assess the strengths of the welded materials.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.54 no.4
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• pp.139-143
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• 2005

For application of carbon nano-tube (CNT) as a counter electrode materials of dye-sensitized solar cell (DSSC), the electrochemical behavior of CNT electrode was studied, employing cyclic-voltammetry (C-V) and impedance spectroscopy. Fabrication of CNT-paste and formation of CNT-counter electrode for characteristic measurement have been carried out using ball-milling and doctor blade process, respectively. Unit cell for measurements was assembled using Pt electrode, CNT electrode, and iodine-embedded electrolyte. Field emission-scanning electron microscopy (FE-SEM) was used for structural investigation of CNT powder and electrode. Sheet resistance of electrode was measured with 4-point probe method. Electrochemical properties of electrode, C-V and impedance spectrum, were studied, employing potentiogalvanostat (EG&G 273A) and lock in amplifier (EG&G 5210). As a results, the sheet resistance of CNT electrode is almost similar to that of F-doped SnO2 (FTO) coated glass substrate as approximately 10 ohm/sq. From C-V and impedance spectroscopy measurements, it was found that CNT electrode has high reaction rate and low interface reaction resistance between CNT surface and electrolyte. These results provides that CNT electrode were superior to that of conventional Pt electrode. Particularly, the reaction rate in the CNT electrode is about thrice high than Pt electrode. Therefore. CNT electrode is to be good candidate material for counter electrode in DSSC.

• Korean Journal of Materials Research
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• v.24 no.8
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• pp.413-416
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• 2014

The effects of an addition of CNT on the sensing properties of nano ZnO:CNT-based gas sensors were studied for $H_2S$ gas. The nano ZnO sensing materials were grown by a hydrothermal reaction method. The nano ZnO:CNT was prepared by ball-milling method. The weight range of the CNT addition on the ZnO surface was from 0 to 10%. The nano ZnO:CNT gas sensors were fabricated by a screen-printing method on alumina substrates. The structural and morphological properties of the ZnO:CNT sensing materials were investigated by XRD, EDS, and SEM. The XRD patterns revealed that nano ZnO:CNT powders with a wurtzite structure were grown with (1 0 0), (0 0 2), and (1 0 1) dominant peaks. The size of the ZnO was about 210 nm, as confirmed by SEM images. The sensitivity of the nano ZnO:CNT-based sensors was measured for 5 ppm of $H_2S$ gas at room temperature by comparing the resistance in air with that in target gases.

• Journal of Powder Materials
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• v.8 no.1
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• pp.49-54
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• 2001

The synthesis and characteristics of W-Ni-Fe nanocomposite powder by hydrogen reduction of ball milled W-Ni-Fe oxide mixture were investigated. The ball milled oxide mixture was prepared by high energy attrition milling of W blue powder, NiO and $Fe_2O_3$ for 1 h. The structure of the oxide mixture was characteristic of nano porous agglomerate composite powder consisting of nanoscale particles and pores which act as effective removal path of water vapor during hydrogen reduction process. The reduction experiment showed that the reduction reaction starts from NiO, followed by $Fe_2O_3$ and finally W oxide. It was also found that during the reduction process rapid alloying of Ni-Fe yielded the formation of $\gamma$-Ni-Fe. After reduction at 80$0^{\circ}C$ for 1 h, the nano-composite powder of W-4.57Ni-2.34Fe comprising W and $\gamma$-Ni-Fe phases was produced, of which grain size was35nm for W and 87 nm for $\gamma$-Ni-Fe, respectively. Sinterability of the W heavy alloy nanopowder showing full density and sound microstructure under the condition of 147$0^{\circ}C$/20 min is thought to be suitable for raw material for powder injection molding of tungsten heavy alloy.

• Journal of Powder Materials
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• v.14 no.4
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• pp.230-237
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• 2007

The fabrication of Fe alloy-40 wt.%TiC composite materials using spark plasma sintering process after ball-milling was studied. Raw powders to fabricate Fe alloy-TiC composite were Fe alloy, $TiH_{2}$ and activated carbon. Fe alloy powder was Distaloy AE (4%Ni-1%Cu-0.5%Mo-0.01%C-bal.%Fe) made by Hoeganes company with better toughness and lower melting point. These powders were ball-milled in horizontal attrition ball mill at a ball-to-powder weight ratio of 30 : 1. After that, these mixture powders were sintered by using spark plasma sintering apparatus for 5 min at $1200-1275^{\circ}C$ in vacuum atmosphere under $10^{-3}$ torr. DistaloyAE-40 wt.%TiC composite was directly synthesized by dehydrogenation and carburization reaction during sintering process. The phase transformation of as-milled powders and sintered materials was confirmed using X-ray diffraction (XRD) and transmission electron microscope (TEM). The density and harness materials was measured in order to confirm the densification behavior. In case of DistaloyAE-40 wt.%TiC composite retained for 5 min at $1275^{\circ}C$, it has the relative density of about 96% through the influence of rapid densification and fine TiC particle reinforced Fe-based composites materials.