• Journal of Powder Materials
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• v.17 no.1
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• pp.36-43
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• 2010

In present work, amorphous TiCuNi powders were fabricated by mechanical alloying process. Amorphization and crystallization behaviors of the TiCuNi powders during high-energy ball milling and subsequent microstructure changes were studied by X-ray diffraction and transmission electron microscope. TEM samples were prepared by the focused ion beam technique. The morphology of powders prepared with different milling times was observed by field-emission scanning electron microscope and optical microscope. The powders developed a fine, layered, homogeneous structure with milling times. The crystallization behavior showed that glass transition, $T_g$, onset crystallization, $T_x$, and super cooled liquid range ${\Delta}T=T_x-T_g$ were 628, 755 and 127K, respectively. The as-prepared amorphous TiCuNi powders were consolidated by spark plasma sintering process. Full densified TiCuNi samples were successfully produced by the spark plasma sintering process. Crystallization of the MA powders happened during sintering at 733K.

• Journal of Powder Materials
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• v.30 no.1
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• pp.41-46
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• 2023

In this study, an Al₈₂Ni₇Co₃Y₈ (at%) bulk metallic glass is fabricated using gas-atomized Al₈₂Ni₇Co₃Y₈ metallic glass powder and subsequent spark plasma sintering (SPS). The effect of powder size on the consolidation of bulk metallic glass is considered by dividing it into 5 ㎛ or less and 20-45 ㎛. The sintered Al₈₂Ni₇Co₃Y₈ bulk metallic glasses exhibit crystallization behavior and crystallization enthalpy similar to those of the Al₈₂Ni₇Co₃Y₈ powder with 5 ㎛ or less and it is confirmed that no crystallization occurred during the sintering process. From these results, we conclude that the Z-position-controlled spark plasma sintering process, using superplastic deformation by viscous flow in the supercooled liquid-phase region of amorphous powder, is an effective process for manufacturing bulk metallic glass.

• Journal of Powder Materials
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• v.13 no.4 s.57
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• pp.269-277
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• 2006

[ ${\beta}-W(W_3O)$ ] oxide layer on the surface of each W(tungsten) nanopowder produced by the electric explosion of wire(EEW) process were formed during the 1vol.% air passivation process. The oxide layer hindered sintering densification of compacts during SPS process. The oxide phase was reduced to the pure W phase during SPS. The W nanopowder's compacts treated by the hydrogen reduction showed high sintered density of 94.5%. after SPS process at $1900^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.40 no.8
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• pp.751-757
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• 2003

Rapid densification of a SiC-30 wt% TiC powder with additive 10 wt% A1$_2$O$_3$-Y$_2$O$_3$-CaO was conducted by Spark Plasma Sintering(SPS). The fully-densified materials can be obtain through the SPS process with very fast heating rate and short holding time. In the present work, the heating rate and applied pressure were kept to be $100^{\circ}C$/min and 40 MPa, while sintering temperature varied from $1600^{\circ}C$ to $1800^{\circ}C$ for 10 min. The full densification of SiC-30 wt% TiC composites with the addition of $Al_2$O$_3$, $Y_2$O$_3$ and CaO was achieved at the temperature above $1700^{\circ}C$ by spark plasma sintering. The XRD found that 3C-SiC and TiC were maintained the entire SPS process temperature, without phase transformation of SiC and formation of YAG phase to $1800^{\circ}C$. The microstructures of the rapidly densified SiC-30 wt% TiC composites consisted of smaller equiaxed SiC grains and larger TiC grains. The biaxial strength of 635.2 MPa and fracture toughness of 6.12 MPaㆍ$m^{1/2}$ were found for the specimen prepared at $1750^{\circ}C$.

• Journal of Powder Materials
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• v.12 no.6 s.53
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• pp.422-427
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• 2005

The $Al_2O_3$ with various phases were prepared by simple ex-situ hydrolysis and spark plasma sintering (SPS) process of Al powder. The nano bayerite $(\beta-Al(OH)_3)$ phase was derived by hydrolysis of commercial powder of Al with micrometer size, whereas the bohemite (AlO(OH)) phase was obtained by hydrolysis of nano Al powder synthesized by pulsed wire evaporation (PWE) method. Compaction as well as dehydration of both nano bayerite and bohemite was carried out simultaneously by SPS method, which is used to fabricate dense powder compacts with a rapid heating rate of $100^{\circ}C$ per min. under the pressure of 50MPa. After compaction treatment in the temperature ranges from $100^{\circ}C\;to\; 1100^{\circ}C$, the bayerite and bohemite phases change into various alumina phases depending on the compaction temperatures. The bayerite shows phase transition of $Al(OH)_3{\to}{\eta}-Al_2O_3{\to}{\theta}-Al_2O_3{\to}\alpha-Al_2O_3$ sequences. On the other hand, the bohemite experiences the phase transition from AlO(OH) to ${\gamma}-Al_2O_3\;at\;350^{\circ}C.$ It shows AlO(OH) ${\gamma}-Al_2O_3{\to}{\delta}-Al_2O_3{\to}{\alpha}-Al_2O_3$ sequences. The ${\gamma}-Al_2O_3$ compacted at $550^{\circ}C$ shows a high surface area $(138m^2/g)$.

• Journal of Powder Materials
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• v.26 no.4
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• pp.299-304
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• 2019

Nb-Si-B alloys with Nb-rich compositions are fabricated by spark plasma sintering for high-temperature structural applications. Three compositions are selected: 75 at% Nb (Nb0.7), 82 at% Nb (Nb1.5), and 88 at% Nb (Nb3), the atomic ratio of Si to B being 2. The microstructures of the prepared alloys are composed of Nb and $T_2$ phases. The $T_2$ phase is an intermetallic compound with a stoichiometry of $Nb_5Si_{3-x}B_x$ ($0{\leq}x{\leq}2$). In some previous studies, Nb-Si-B alloys have been prepared by spark plasma sintering (SPS) using Nb and $T_2$ powders (SPS 1). In the present work, the same alloys are prepared by the SPS process (SPS 2) using Nb powders and hypereutectic alloy powders with composition 67at%Nb-22at%Si-11at%B (Nb67). The Nb67 alloy powders comprise $T_2$ and eutectic ($T_2+Nb$) phases. The microstructures and hardness of the samples prepared in the present work have been compared with those previously reported; the samples prepared in this study exhibit finer and more uniform microstructures and higher hardness.

• Nuclear Engineering and Technology
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• v.53 no.8
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• pp.2582-2590
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• 2021

The high-energy milling is one of the most extended techniques to produce Oxide dispersion strengthened (ODS) powder steels for nuclear applications. The consequences of the high energy mill process on the final powders can be measured by means of deformation level, size, morphology and alloying degree. In this work, an ODS ferritic steel, Fe-14Cr-5Al-3W-0.4Ti-0.25Y₂O₃-0.6Zr, was fabricated using two different mechanical alloying (MA) conditions (M_std and M_act) and subsequently consolidated by Spark Plasma Sintering (SPS). Milling conditions were set to evidence the effectivity of milling by changing the revolutions per minute (rpm) and dwell milling time. Differences on the particle size distribution as well as on the stored plastic deformation were observed, determining the consolidation ability of the material and the achieved microstructure. Since recrystallization depends on the plastic deformation degree, the composition of each particle and the promoted oxide dispersion, a dual grain size distribution was attained after SPS consolidation. M_act showed the highest areas of ultrafine regions when the material is consolidated at 1100 ℃. Microhardness and small punch tests were used to evaluate the material under room temperature and up to 500 ℃. The produced materials have attained remarkable mechanical properties under high temperature conditions.

• Korean Journal of Materials Research
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• v.17 no.2
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• pp.107-114
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• 2007

Porous Ti compacts were fabricated by spark plasma sintering (SPS) method and their in vitro and in vivo biocompatibilities were investigated. Alkaline phosphatase (ALP) activity representing the activity of osteoblast was increased when osteoblast-like MG-63 cells were cultured on the Ti powder surface. Some genes related to cell growth were over-expressed through microarray analysis. The porous Ti compact with 32.2% of porosity was implanted in the subcutaneous tissue of rats to confirm in vivo cytotoxicity. 12 weeks post-operation, outer surface and inside the porous body was fully filled with fibrous tissue and the formation of new blood vessels were observed. No inflammatory response was confirmed. To investigate the osteoinduction, porous Ti compact was implanted in the femur of NZW rabbits for 4 months. Active in-growth of new bone from the surrounded compact bone was observed around the porous body. From the results, The porous Ti compacts fabricated by spark plasma sintering might be available for the application of the stem part of artificial hip joint.

• Journal of Powder Materials
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• v.22 no.6
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• pp.426-431
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• 2015

Microstructural examination of the Nb-Si-B alloys at Nb-rich compositions is performed. The Nb-rich corner of the Nb-Si-B system is favorable in that the constituent phases are Nb (ductile and tough phase with high melting temperature) and $T_2$ phase (very hard intermetallic compound with favorable oxidation resistance) which are good combination for high temperature structural materials. The samples containing compositions near Nb-rich corner of the Nb-Si-B ternary system are prepared by spark plasma sintering (SPS) process using $T_2$ and Nb powders. $T_2$ bulk phase is made in arc furnace by melting the Nb slug and the Si-B powder compact. The $T_2$ bulk phase was subsequently ball-milled to powders. SPS is performed at $1300^{\circ}C$ and $1400^{\circ}C$, depending on the composition, under 30 MPa for 600s, to produce disc-shaped specimen with 15 mm in diameter and 3 mm high. Hardness tests (Rockwell A-scale and micro Vickers) are carried out to estimate the mechanical property.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.60 no.11
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• pp.2083-2087
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• 2011

The SiC-$ZrB_2$ composites were produced by subjecting a 40:60 vol.% mixture of zirconium diboride($ZrB_2$) powder and ${\beta}$-silicon carbide (SiC) matrix to spark plasma sintering(SPS). Sintering was carried out for 60sec at $1400^{\circ}C$ (designation as TP145 and TP146), $1500^{\circ}C$(designation as TP155 and TP156) and uniaxial pressure 50MPa, 60MP under argon atmosphere. The physical, electrical, and mechanical properties of the SiC-$ZrB_2$ composites were examined. The relative density of TP145, TP146, TP155 and TP156 were 94.75%, 94.13%, 97.88% and 95.80%, respectively. Reactions between ${\beeta}$-SiC and $ZrB_2$ were not observed via x-ray diffraction (hereafter, XRD) analysis. The flexural strength, 306.23MPa of TP156 was higher than that, 279.42MPa of TP146 at room temperature, but lower than that, 392.30MPa of TP155. The properties of a SiC-$ZrB_2$ composites through SPS under argon atmosphere were positive temperature coefficient resistance (hereafter, PTCR) in the range from $25^{\circ}C$ to $500^{\circ}C$. The electrical resistivities of TP145, TP146, TP155 and TP156 were $6.75{\times}10^{-4}$, $7.22{\times}10^{-4}$, $6.17{\times}10^{-4}$ and $6.71{\times}10^{-4}{\Omega}{\cdot}cm$ at $25^{\circ}C$, respectively. The densification of a SiC-$ZrB_2$ composite through hot pressing depend on the sintering temperature and pressure. However, it is convinced that the densification of a SiC-$ZrB_2$ composite do not depend on sintering pressure under SPS.