• 한국분말재료학회지
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• 제5권3호
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• pp.210-219
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• 1998

The W-Cu composite powders were synthesized from W and Cu elemental powders by ball-milling process, and their microstructural changes and sintering behaviors were evaluated. The ball milling process was carried out in a 3-dimensional mixer (Turbula mixer) using zirconic ($ZrO_2$) ball and alumina ($Al_2O_3$) vial up to 300 hrs. The ball-milled W-Cu powders revealed nearly spherical shape. Microstructure of the composite powders showed onion-like structure which consists of W and Cu shells due to the moving characteristic of Turbula mixer. The W and Cu elements in the composite powders milled for 300 hrs were homogeneously distributed, and W grain size in the ball-milled powder was smaller than 0.5 $\mu\textrm{m}$. Fe impurity introduced during ball milling process was very low as of 0.001 wt%. The relative sintered density of ball-milled W-Cu specimens reached about 94% after sintering at $1100^{\circ}C$.

• 한국분말재료학회지
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• 제5권2호
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• pp.89-97
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• 1998

Sintering behavior of nanostructured(NS) W-Cu powders prepared by mechanical alloying (MA) was investigated as a function of sintering temperature. MA NS W-2owt%Cu and W-3owt%Cu composite powders with the crystal size of 20-30 nm were annealed at 90$0^{\circ}C$, and thermal characteristics of those powders were investigated by DSC. Sintering behavior of MA NS W-Cu composite powders was investigated during the solid-state sintering and the Cu-liquid phase sintering. The new nanosintering phenonenon of MA W-Cu powders at solid-state sintering temperature was suggested to explain the W-grain growth in the inside of MA powders. The sintering densification of MA NS W-Cu powders was enhanced at Cu melting temperature by arrangement of MA powders, i.e., the first rearrangement of MA powders was occurred, and then the rearrangement of W-grains in the sintered parts was also took place during liquid-phase sintering, i.e., the second rearrangement was happened. Due to the double rearrangement process of MA NS W-Cu powders, the high sintered density with more than 96%o was obtained and the fine and high homogeneous state of W and Cu phases was achieved by sintering at 1200 $^{\circ}C$.

• 한국재료학회지
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• 제11권11호
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• pp.953-959
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• 2001

Homogeneous spherical W-Co salt powders were made by spray drying of aqueous solution of ammonium $metatungstate(NH_4)_6(H_2W_{12}O_{40}){\cdot}4H_2O,\; AMT)$ and cobalt nitrate $hexahydrate(Co(NO_3)_2{\cdot}6H_2O)$. The thermal decomposition process of spray dried W-Co salt powders was studied by TG, XRD, SEM, TEM and FT-IR. Spray dried W-Co salt powders were calcined for 1 hour in the temperature from$ 350^{\circ}C$ to $800^{\circ}C$ in atmosphere of air. At the temperatures over $600^{\circ}C$, spherical $CoWO_4/WO_3$ composite oxide powders were obtained. The primary particle size of W/Co composite oxide powders increased with increasing thermal decomposition temperature due to the particle growth. The observed crystallite size by TEM was in the range of 60nm and that of $CoWO_4$ calculated by Scherrer's formula at $800^{\circ}C$ was smaller than 55nm. The crystallite site was identified by XRD and TEM.

• 한국세라믹학회지
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• 제35권6호
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• pp.543-550
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• 1998

에멀젼 증발법에 의해 구형의 산화텅스텐 분말을 제조하는 연구를 하였다. 분말의 특성은 TGA, X-ray 회절, SEM, image analysis 등을 이용하여 조사하였다. 텅스텐 이온이 함유된 수상과 등유, 계면활성제, 파라핀유로 이루어진 유기상을 고속으로 교반하여 에멀젼을 제조하였다. 에멀젼을 $160^{\circ}C$의 등유욕내에서 증발시틴 후 얻어진 침전물을 $160^{\circ}C$에서 하소하여 텅스텐 산화 분말을 제조하였다. 산화텅스텐 분말의 평균 입경은 $0.5\;\mu\textrm{m}$ 였으며 모양은 구형이었다. Watre-in-oil형 에멀젼으로 제조된 $W_{3}$는 oil-in-water 형의 것보다 응집도가 적었다. 계면활성제의 HLB값이 증가할수록, 에멀젼 중의 텅스텐 이온의 농도가 감소할수록 평균입도가 작아졌으며, $W_{3}$ 입자들의 응집도는 증가하였다. 계면활정제로 사용한 Span 80의 농도는 8 vol%가 적당했고, 에멀젼 제조시 교반속도는 5000rpm이 적당했다.

• 한국분말재료학회지
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• 제9권3호
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• pp.167-173
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• 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.

• 한국재료학회지
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• 제13권3호
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• pp.169-173
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• 2003

W-Cu composite powders can be prepared by mechanochemical process, where the $WO_3$-CuO composite powders were mechanically synthesized from the elemental oxide powders and subsequently reduced to W-Cu composite powders. In the present work, reduction behavior of$ WO_3$-CuO composite powders that were synthesized at different milling time was examined in terms of hygrometric analysis. In case of $WO_3$-CuO ball-milled for 20 h, the reaction temperature of CuO\longrightarrowCu became lower than in case of 1 h. Also, the reaction of $WO_3$\longrightarrow$WO_{2.9-2.72}$ and $WO_{2.9-2.72}$ \longrightarrow$WO_2$were shifted to lower temperatures and the peaks were changed to much sharper shape. While the reaction of $WO_2$\longrightarrowW in case of ball-milling for 20 h started at lower temperature, the peak temperature was the same as in 1 h ball-milling. The reduced W particle size was somewhat finer fer 20 h ball-milling. It was considered that the refinement of oxide particles caused by ball-milling process leads to such a change in the reduction behavior.

• 한국재료학회지
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• 제27권10호
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• pp.513-517
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• 2017

An optimum route to fabricate a hybrid-structured W powder composed of nano and micro size powders was investigated. The mixture of nano and micro W powders was prepared by a ball milling and hydrogen reduction process for $WO_3$ and W powders. Microstructural observation for the ball-milled powder mixtures revealed that the nano-sized $WO_3$ particles were homogeneously distributed on the surface of large W powders. The reduction behavior of $WO_3$ powder was analyzed by a temperature programmed reduction method with different heating rates in Ar-10% $H_2$ atmosphere. The activation energies for the reduction of $WO_3$, estimated by the slope of the Kissinger plot from the amount of reaction peak shift with heating rates, were measured as 117.4 kJ/mol and 94.6 kJ/mol depending on reduction steps from $WO_3$ to $WO_2$ and from $WO_2$ to W, respectively. SEM and XRD analysis for the hydrogen-reduced powder mixture showed that the nano-sized W particles were well distributed on the surface of the micro-sized W powders.

• 한국세라믹학회지
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• 제27권8호
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• pp.955-964
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• 1990

A new process of emulsiion-spray pyrolysis for synthesizing ceramic powders was developed and the characteristics of Al2O3-20w/o ZrO2 composite powders prepared by this method were investigated. The composite powders synthesized in this study were spherical dense particles with 0.1~0.4${\mu}{\textrm}{m}$ of diameter. As found in powders derived by the emulsion-hot kerosene drying method, all zirconia in Al2O3-20w/o ZrO2 powders heat-treated at 120$0^{\circ}C$ was in the tetragonal form at room temperature. The relative density and the fracture toughness of composites sintered at 1$650^{\circ}C$ for 4hrs were 95% and 5.2MPa.m1/2, respectively.

• 한국분말재료학회지
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• 제10권6호
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• pp.422-429
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• 2003

The reduction mechanism of the composite powders mixed with $WO_3$ and CuO has been studied by using thermogravimetry (TG), X-ray diffraction, and microstructure analyses. The composite powders were made by simple Turbula mixing, spray drying, and ball-milling in a stainless steel jar with the ball to powder ratio of 32 to 1 at 80 rpm for 1 h without process controlling agents. It is observed that all the oxide composite powders are converted to W-coated Cu composite powder after reducing treatment under hydrogen atmosphere. For the formation mechanism of W-coated Cu composite powder, the sequential reduction steps are proposed as follows: CuO contained in the ball-milled composite powder is initially reduced to Cu at the temperature range from 20$0^{\circ}C$ to 30$0^{\circ}C$. Then, $WO_3$ powder is reduced to W $O_2$ via W $O_{2.9}$ and W $O_{2.72}$ at higher temperature region. Finally, the gaseous phase of $WO_3(OH)_2$ formed by reaction of $WO_2$ with water vapour migrates to previously reduced Cu and deposits on it as W reduced by hydrogen. The proposed mechanism has been proved through the model experiment which was performed by using Cu plate and $WO_3$ powder.

• 한국분말재료학회지
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• 제9권3호
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• pp.174-181
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• 2002

Nanosized tungsten carbide powders were synthesized by the chemical vapor condensation(CVC) process using the pyrolysis of tungsten hexacarbonyl($W(CO)_6$). The effect of CVC parameters on the formation and the microstructural change of as-prepared powders were studied by XRD, BET and TEM. The loosely agglomerated nanosized tungsten-carbide($WC_{1-x}$) particles having the smooth rounded tetragonal shape could be obtained below $1000^{\circ}C$ in argon and air atmosphere respectively. The grain size of powders was decreased from 53 nm to 28 nm with increasing reaction temperature. The increase of particle size with reaction temperature represented that the condensation of precursor vapor dominated the powder formation in CVC reactor. The powder prepared at $1000^{\circ}C$ was consisted of the pure W and cubic tungsten-carbide ($WC_{1-x}$), and their surfaces had irregular shape because the pure W was formed on the $WC_{1-x}$ powders. The $WC_{1-x}$ and W powders having the average particles size of about 5 nm were produced in vacuum.