• Journal of Korean Society of Occupational and Environmental Hygiene
• /
• v.25 no.3
• /
• pp.294-300
• /
• 2015

Objectives: The aim of this study is to identify physicochemical properties such as chemical composition, size, shape and crystal structure of powder byproducts generated from a metallization process and its 1st scrubber in the semiconductor industry. Methods: Powder samples were collected from inner chambers during maintenance of the W-plug process equipment (using tungsten hexafluoride as a precursor material) and its 1st scrubber. The chemical composition, size and shape of the powder particles were determined by field emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) equipped with an energy dispersive spectroscope (EDS). The crystal structure of the powders was analyzed by X-ray diffraction (XRD). Results: From the SEM-EDS and TEM-EDS analyses, O and W were mainly detected, which indicates the powder byproducts are tungsten trioxide ($WO_3$), whereas Al, F and Ti were detected as low peaks. The powder particles were spherical and nearly spherical, and the particle size collected from the process equipment and its 1st scrubber showed 10-20 nm (agglomerates: 55-90 nm) and 16-20 nm (agglomerates: 80-120 nm) as primary particles, respectively. The XRD patterns of the yellow powder byproducts exhibit five peaks at $23.8^{\circ}$ $33.9^{\circ}$ $41.74^{\circ}$ $48.86^{\circ}$ and $54.78^{\circ}$ which correspond to the (200), (220), (222), (400), and (420) planes of cubic $WO_3$. Conclusions: We elucidated the physicochemical characteristics of the powder byproducts collected from W-plug process equipment and its 1st scrubber. This study should provide useful information for the development of alternative strategies to improve the working environment and workers' health.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 2005.04a
• /
• pp.33-34
• /
• 2005

• Korean Chemical Engineering Research
• /
• v.51 no.3
• /
• pp.313-318
• /
• 2013

In order to investigate the effect of $V_2O_5$ loading of $V_2O_5-WO_3/TiO_2$ catalyst on the NO reduction and the formation of $N_2O$, the experimental study was carried out in a differential reactor using the powder catalyst. The NO reduction and the ammonia oxidation were, respectively, investigated over the catalysts compose of $V_2O_5$ content (1~8 wt%) based on the fixed composition of $WO_3$ (9 wt%) on $TiO_2$ powder. $V_2O_5-WO_3/TiO_2$ catalysts had the NO reduction activity even under the temperature of $200^{\circ}C$. However, the lowest temperature for NO reduction activity more than 99.9% to treat NO concentration of 700 ppm appeared at 340 with very limited temperature window in the case of 1 wt% $V_2O_5$ catalyst. And the temperature shifted to lower one as well as the temperature window was widen as the $V_2O_5$ content of the catalyst increased, and finally reached at the activation temperature ranged $220{\sim}340^{\circ}C$ in the case of 6 wt% $V_2O_5$ catalyst. The catalyst of 8 wt% $V_2O_5$ content presented lower activity than that of 8 wt% $V_2O_5$ content over the full temperature range. NO reduction activity decreased as the $V_2O_5$ content of the catalyst increased above $340^{\circ}C$. The active site for NO reduction over $V_2O_5-WO_3/TiO_2$ catalysts was mainly related with $V_2O_5$ particles sustained as the bare surface with relevant size which should be not so large to stimulate $N_2O$ formation at high temperature over $320^{\circ}C$ according to the ammonia oxidation. Currently, $V_2O_5-WO_3/TiO_2$ catalysts were operated in the temperature ranged $350{\sim}450^{\circ}C$ to treat NOx in the effluent gas of industrial plants. However, in order to save the energy and to reduce the secondary pollutant $N_2O$ in the high temperature process, the using of $V_2O_5-WO_3/TiO_2$ catalyst of content $V_2O_5$ was recommended as the low temperature catalyst which was suitable for low temperature operation ranged $250{\sim}320^{\circ}C$.

• Korean Journal of Materials Research
• /
• v.24 no.5
• /
• pp.249-254
• /
• 2014

Due to their unique properties, tungsten borides are good candidates for the industrial applications where certain features such as high hardness, chemical inertness, resistance to high temperatures, thermal shock and corrosion. In this study, conditions were investigated for producing tungsten boride powder from tungsten oxide($WO_3$) by self-propagating high-temperature synthesis (SHS) followed by HCl leaching techniques. In the first stage of the study, the exothermicity of the $WO_3$-Mg reaction was investigated by computer simulation. Based on the simulation experimental study was conducted and the SHS products consisting of borides and other compounds were obtained starting with different initial molar ratios of $WO_3$, Mg and $B_2O_3$. It was found that $WO_3$, Mg and $B_2O_3$ reaction system produced high combustion temperature and radical reaction so that diffusion between W and B was not properly occurred. Addition of NaCl and replacement of $B_2O_3$ with B successfully solved the diffusion problem. From the optimum condition tungsten boride($W_2B$ and WB) powders which has 0.1~0.9 um particle size were synthesized.

• Journal of Powder Materials
• /
• v.9 no.3
• /
• pp.167-173
• /
• 2002

A new approach to produce nanostructured WC/Co composite powders by a mechanochemical process was made to improve the mechanical properties of advanced hardmetals. Homogeneous spherical W-Co salt powders were made by spray drying of aqueous solution from ammonium metatungstate($(NH_4)_6(H_2W_{12}O_{40})\cdo4H_2O$,AMT) and cobalt nitrate hexahydrate (Co(NO$_3$)$_2$.6$H_2O$). spray dried W-Co salt powders were calcined for 1 hr at $700^{\circ}C$ in atmosphere of air. The oxide powder was mixed with carbon black by ball milling and this mixture was heated with various temperatures and times in $H_2$. The $WO_3/CoWO_4$ composite oxide powders were obtained by calcinations at $700^{\circ}C$. The primary particle size of W/Co composite oxide powders by SEM was 100 nm. The reduction/carburization time decreased with increasing temperatures and carbon additions. The average size of WC particle carburized at $800^{\circ}C$ by TEM was smaller than 50 nm.

• Bulletin of the Korean Chemical Society
• /
• v.19 no.8
• /
• pp.856-862
• /
• 1998

Vanadium oxide catalyst supported on ZrO2-WO3 was prepared by adding the Zr(OH)4 powder into a mixed aqueous solution of ammonium metavanadate and ammonium metatungstate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using solid-state 51V NMR and FTIR. In the case of calcination temperature at 773 K, for the samples containing low loading V2O5 below 18 wt % vanadium oxide was in a highly dispersed state, while for samples containing high loading V2O5 equal to or above 18 wt % vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of ZrO2-WO3. The ZrV2O7 compound was formed through the reaction Of V2O5 and ZrO2 at 873 K and the compound decomposed into V2O5 and ZrO2 at 1073 K, which were confirmed by FTIR and 51V NMR.

• Journal of the Korean Ceramic Society
• /
• v.39 no.3
• /
• pp.321-326
• /
• 2002

ZnWO$_4$ nano-powders were successfully prepared by polymerized complex method using zinc nitrate and tungstic acid as starting materials. In order to investigate the thermal decomposition and crystallization process, the polymeric precursors were heat-treated at temperatures from 300 to 600$^{\circ}$C for 3 h, and the heat-treated powders were characterized by XRD and FTIR. The surface morphology of the heat-treated powders were observed using SEM and TEM. The crystallite size was measured by X-ray analysis. Crystallization of the ZnWO$_4$ powders were detected at 400$^{\circ}$C and entirely completed at a temperature of 600$^{\circ}$C. The particles heat-treated 400 and 500$^{\circ}$C showed primarily co-mixed morphology with spherical and silkworm-like forms, while the particles heat-treated at 600$^{\circ}$C showed more homogeneous morphology. The average crystalline size were 19.9∼24.nm showing an ordinary tendency to increase with the temperatures from 400 to 600$^{\circ}$C.

• Journal of Powder Materials
• /
• v.23 no.5
• /
• pp.372-378
• /
• 2016

This study focuses on the development of an alkaline leaching hydrometallurgy process for the recovery of tungsten from WC/Co hardmetal sludge, and an examination of the effect of the process parameters on tungsten recovery. The alkaline leaching hydrometallurgy process has four stages, i.e., oxidation of the sludge, leaching of tungsten by NaOH, refinement of the leaching solution, and precipitation of tungsten. The WC/Co hardmetal sludge oxide consists of $WO_3$ and $CoWO_4$. The leaching of tungsten is most affected by the leaching temperature, followed by the NaOH concentration and the leaching time. About 99% of tungsten in the WC/Co hardmetal sludge is leached at temperatures above $90^{\circ}C$ and a NaOH concentration above 15%. For refinement of the leaching solution, pH control of the solution using HCl is more effective than the addition of $Na_2S{\cdot}9H_2O$. The tungsten is precipitated as high-purity $H_2WO_4{\cdot}H_2O$ by pH control using HCl. With decreasing pH of the solution, the tungsten recovery rate increases and then decrease. About 93% of tungsten in the WC/Co hardmetal sludge is recovered by the alkaline leaching hydrometallurgy process.

• Korean Journal of Materials Research
• /
• v.12 no.12
• /
• pp.930-934
• /
• 2002

Nanosized $WO_3$ powders were synthesized by the sol-precipitation process using $WCl_{6}$ as the starting material, ethanol as a solvent and $NH_4$OH solution as a precipitant, followed by a washing-drying treatment and calcination. The effects on the powder crystallinity and microstructure of calcination temperature were investigated with XRD and FE-SEM. The $WO_3$ powders calcined at $500^{\circ}C$ and $700^{\circ}C$ showed good crystallinity and their mean particle size was 30nm and 70nm, respectively. These powders were used for the preparation of pastes which were printed as thick films on alumina substrates with comb-type Pt electrodes. The particle size strongly influenced the $NO_2$ gas sensing property of the thick films. A significant reduction in the $NO_2$ sensitivity was observed for the film prepared from larger particle size, having thus a larger grain size. For the film having a smaller grain size, on the other hand, the higher $NO_2$ sensitivity was observed and the sensitivity increased with $NO_2$ concentration.

• Journal of Powder Materials
• /
• v.11 no.2
• /
• pp.111-117
• /
• 2004

The oxidation behavior of 91 WC-9Co hardmetal in weight percentage has been studied in the present work as a part of the development of recycling process. The morphological and compositional changes of the WC-Co hardmetal with oxidation time at 90$0^{\circ}C$ were analyzed by using surface observation and X-ray diffraction. respective]y. As the oxidation time increased, the WC-Co hardmetal was continuously expanded to form porous oxide mixtures of $CoWO_4$ and $WO_3$. The morphology of porous oxide mixture was basically dependent on initial shape of the WC-Co hardmetal. From thermo-gravimetric (TG) analysis, it was found that the oxidation rate was increased with increasing oxidation temperature and oxygen content in the flowing atmospheric gas. The fraction of oxidation versus time curves showed S-curve relationship at a given of oxidation temperature. These oxidation behaviors of the WC-Co hardmetal were discussed in terms of previously proposed kinetic models.