• Journal of Powder Materials
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• v.5 no.2
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• pp.98-110
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• 1998

$Ti_{52}Al_{48}$ and $(Ti_{52}Al_{48})_{100-x}B_x(x=0.5, 2, 5)$ alloys have been Produced by mechanical milling in an attritor mill using prealloyed powders. Microstructure of binary $Ti_{52}Al_{48}$ powders consists of grains of hexagonal phase whose structure is very close to $Ti_2Al$. $(Ti_{52}Al_{48})_{95}B_5$ powders contains TiB2 in addition to matrix grains of hexagonal phase. The grain sizes in the as-milled powders of both alloys are nanocrystalline. The mechanically alloyed powders were consolidated by vacuum hot pressing (VHP) at 100$0^{\circ}C$ for 2 hours, resulting in a material which is fully dense. Microstructure of consolidated binary alloy consists of $\gamma$-TiAl phase with dispersions of $Ti_2AlN$ and $A1_2O_3$ phases located along the grain boundaries. Binary alloy shows a significant coarsening in grain and dispersoid sizes. On the other hand, microstructure of B containing alloy consists of $\gamma$-TiAl grains with fine dispersions of $TiB_2$ within the grains and shows the minimal coarsening during annealing. The vacuum hot pressed billets were subjected to various heat treatments, and the mechanical properties were measured by compression testing at room temperature. Mechanically alloyed materials show much better combinations of strength and fracture strain compared with the ingot-cast TiAl, indicating the effectiveness of mechanical alloying in improving the mechanical properties.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 1996.11a
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• pp.6-6
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• 1996

Ceramic based nanocomposite, in which nano-sized ceramics and metals were dispersed within matrix grains and/or at grain boundaries, were successfully fabricated in the ceramic/cerarnic and ceramic/metal composite systems such as $Al_2O_3$/SiC, $Al_2O_3$/$Si_3N_4$, MgO/SiC, mullite/SiC, $Si_3N_4/SiC, $Si_3N_4$/B, $Al_2O_3$/W, $Al_2O_3$/Mo, $Al_2O_3$/Ni and $ZrO_2$/Mo systems. In these systems, the ceramiclceramic composites were fabricated from homogeneously mixed powders, powders with thin coatings of the second phases and amorphous precursor composite powders by usual powder metallurgical methods. The ceramiclmetal nanocomposites were prepared by combination of H2 reduction of metal oxides in the early stage of sinterings and usual powder metallurgical processes. The transmission electron microscopic observation for the $Al_2O_3$/SiC nanocomposite indicated that the second phases less than 70nm were mainly located within matrix grains and the larger particles were dispersed at the grain boundaries. The similar observation was also identified for other cerarnic/ceramic and ceramiclmetal nanocornposites. The striking findings in these nanocomposites were that mechanical properties were significantly improved by the nano-sized dispersion from 5 to 10 vol% even at high temperatures. For example, the improvement in hcture strength by 2 to 5 times and in creep resistance by 2 to 4 orders was observed not only for the ceramidceramic nanocomposites but also for the ceramiclmetal nanocomposites with only 5~01%se cond phase. The newly developed silicon nitride/boron nitride nanocomposites, in which nano-sized hexagonal BN particulates with low Young's modulus and fracture strength were dispersed mainly within matrix grains, gave also the strong improvement in fracture strength and thermal shock fracture resistance. In presentation, the process-rnicro/nanostructure-properties relationship will be presented in detail. The special emphasis will be placed on the understanding of the roles of nano-sized dispersions on mechanical properties.

• Journal of the Korean Ceramic Society
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• v.28 no.12
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• pp.961-968
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• 1991

The nature and composition of the surfaces of silicon nitride and β-Sialon powders were investigated using high voltage and high resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). β-Sialon powder was produced from Hadong kaolin by the carbothermic reduction and simultaneous nitridation. XPS showed that Al was contained in the surface of β-Sialon powder besides Si, N and O components, which is different from that of silicon nitride. It was supposed that Al in the surface of β-Sialon was bonded with oxygen from the oxygen-nitrogen ratio and the measurement of Al 2p binding energies. After both silicon nitride and β-Sialon powders were oxidized at 800℃ for 24h in air, nitrogen didn't exist in the surfaces and the depth of the oxide layer increased. The measurement of Si 2p binding energies showed that the chemical shifts occurred from Si3N2O and/or Si2N2O to SiO2 phase.

• Journal of the Korean Chemical Society
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• v.32 no.3
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• pp.267-275
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• 1988

Fine powders of amorphous $Al_2O_3,\;SiO_2,\;Al_2O_3-SiO_2$ system were prepared by hydrolysis of solutions containing alkoxides, aluminium tri-isopropoxide and silicon tetra-ethoxide. High purity ultrafine ${\beta}-sialon$ powders were prepared by the carbothermal reduction-nitridation of amorphous $Al_2O_3-SiO_2$ powders mixed with carbon black as a reducing agent. In the hydrolysis step the effect of the factors such as pH, reaction temperature and amount of water on the conversion rate of alkoxides to oxides was investigated. In the carbothermal reduction-nitridation the reaction path was assumed by the analysis of intermediates formed in the process of ${\beta}-sialon$ synthesis and the reaction kinetics of ${\beta}-sialon$ formation was considered.

• Journal of the Korean Ceramic Society
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• v.47 no.6
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• pp.566-571
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• 2010

Dispersion behavior of the slurries consisted of bimodal-type AlN powders was examined in non-aqueous solvent system. Azotropic solvent system and copolymer acidic dispersant were applied to the slurries. Measurements of the sedimentation height and the viscosity of the each slurry, and the test of particle size distribution of the each powder sample were conducted as examinations for the dispersion behavior at the various dispersant contents. The bimodal-type particle size distribution was continued after addition of the dispersant and small particle portions were increased as the dispersant content increases. The density of the green sheet was also increased as the dispersant content increases and a green density of $2.114\;g/cm^3$ was obtained at the sample prepared from 2.4 wt% dispersant content. The increase of large particle portions resulted in the surface defects of the green sheets.

• Journal of Powder Materials
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• v.6 no.1
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• pp.111-118
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• 1999

Ni(Fe)Al powders containing a homogeneous distribution of the in-situ formed AIN and $Al_2O_3$ dispersoids have been produced by mechanical alloying process in a controlled atmosphere using high energy attrition mill. The powders have been successfully consolidated by hot extrusion process. The phase information investigated by TEM and XRD analysis reveals that Fe can be soluble up to 20% to the NiAl phase ($\beta$) at room temperature after MA process. Subsequent thermomechanical treatment under specific condition has been tried to induce secondary recrystallization (SRx) to improve high temperature properties, however, the clear evidence of SRx was not obtained in this material. Mechanical properties in term of strength at room temperature as well as at high temperatures have been improved by the addition pf AIN, and the room temperature ductility has been shown to be improved after heat treatment, presumably due to the precipitation of second phase of $\alpha$ in this material.

• Journal of the Korean Ceramic Society
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• v.26 no.1
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• pp.100-108
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• 1989

Aluminum hydroxides were prepared by the alkoxide hydrolysis method using Al-isopropoxide as a starting material and NH4OH as a catalytic agent. When Al-isopropoxide was hydrolyzed in a H2O-NH3 system, only Al(OH)3 was obtained over all pH values. However, AlOOH was formed besides Al(OH)3 when Al-isopropoxide was hydrolyzed in a H2O-NH3-isopropyl alcohol system. The AlOOH/Al(OH)3 ratio was increased as the isopropyl alcohol content was increased. The hydroxides, Al(OH)3 and AlOOH, obtained in this study and the commerical products, $\alpha$-Al2O3 and AlOOH were subjected to the carbothermal reduction and nitridation reaction to product AlN powder, using carbon black as a reducing agent under N2 atmosphere at various temperatures. AlN was synthesized from the obtained Al(OH)3 and the commercial AlOOH at 145$0^{\circ}C$, however, synthesized from the obtained AlOOH and the commercial alpha-alumina at 135$0^{\circ}C$. The temperature difference is assumed to be attributed to the reactivity of those powders. AlN powder prepared from the Al-isopropoxide was observed to have the narrower particle size distribution than that prepared from the commercial $\alpha$-Al2O3 or AlOOH.

• Journal of the Korean Ceramic Society
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• v.31 no.1
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• pp.1-10
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• 1994

Monodispersed alumina and Mg-doped alumina fine particles were prepared by controlled hydrolysis of alkoxides. Aluminium alkoxide and magnesium alkoxide were dissolved into complex solvent which was composed of hydrophobic n-octanol and hydrophilic acetonitrile. Hydroxypropyl cellulose(HPC) was used as a dispersant for the alumina particles. The size of these prepared powders was approximately 0.3 ${\mu}{\textrm}{m}$. In the case of sintering above 100$0^{\circ}C$, most of these prepared powders were transformed to $\alpha$-alumina. The relative density of the sintered body of these prepared powders at 1$600^{\circ}C$ was 98%. The sintered body of the Mg-doped alumina powder had more uniform grain size than that of the undoped alumina podwer.

• Korean Journal of Materials Research
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• v.14 no.4
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• pp.293-299
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• 2004

Transition metal ions doped $TiO_2$ nanostructured powders were prepared with simply heating aqueous $TiOCl_2$ solutions, contained various metal ions (Ni, Al, Fe, Zr, and Nb) of 1.47 mol% added as metal-chlorides, at $100^{\circ}C$ for 4 hrs by homogeneous precipitation process under suppressing conditions of water vaporization. The characterizations for prepared $TiO_2$ powders were carried out to observe doping of metal ions, their concentrations and microstructures using XRD, UV-VIS (DRS), XPS, SEM, TEM and ICP. Also, photo-oxidative abilities were evaluated by decomposition of 4-chlorophenol (4CP) under ultraviolet light irradiations. No secondary oxide phases were formed in all the $VTiO_2$ powders, showing doping with various transition metal ions. When adding ions ($Ni^{2+}$ or$ Al^{3+ }$ and $Zr^{4+}$ ) having valance states or ionic radii greatly different from those of $Ti^{4+}$ , the $TiO_2$ powders of mixed anatase and rutile phases were formed, whereas in the case of additions of $^Fe{3+ }$ and $Nb^{ 5+}$ as well as no addition of metal ion the powders with pure rutile phase alone were formed. Among the prepared $TiO_2$ powders, Ni$^{2+}$ doped $TiO_2$ powders, containing a small amount of anatase phase, showed excellent photo-oxidative ability in 4CP decomposition because of relative decreases in electron-hole recombination and poisoning of $TiO_2$ surface during the photoreaction.n.

• Korean Chemical Engineering Research
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• v.53 no.5
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• pp.620-626
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• 2015

$Ho^{3+}$ doped $SrAl_2O_4$ upconversion phosphor powders were synthesized by spray pyrolysis, and the crystallographic properties and luminescence characteristics were examined by varying activator concentrations and heattreatment temperatures. The effect of organic additives on the crystal structure and luminescent properties was also investigated. $SrAl_2O_4:Ho^{3+}$ powders showed intensive green emission due to the $^5F_4/^5S_2{\rightarrow}^5I_8$ transition of $Ho^{3+}$. The optimal $Ho^{3+}$ concentration in order to achieve the highest luminescence was 0.1%. Over this concentration, emission intensities were largely diminished via a concentration quenching due to dipole-dipole interaction between activator ions. According to the dependence of emission intensity on the pumping power of a laser diode, it was clear that the upconversion of $SrAl_2O_4:Ho^{3+}$ occurred via the ground state absorption-excited state absorption processes involving two near-IR photons. Synthesized powders were monoclinic as a major phase, having some hexagonal phase. The increase of heat-treatment temperatures from $1000^{\circ}C$ to $1350^{\circ}C$ led to crystallinity enhancement of monoclinic phase, reducing hexagonal phase. The hexagonal phase, however, did not disappear even at $1350^{\circ}C$. When both citric acid (CA) and ethylene glycol (EG) were added to the spray solution, the resulting powders had pure monoclinic phase without forming hexagonal phase, and led to largely enhancement of crystallinity. Also, N,N-Dimethylformamide (DMF) addition to the spray solution containing both CA and EG made it possible to effectively reduce the surface area of $SrAl_2O_4:Ho^{3+}$ powders. Consequently, the $SrAl_2O_4:Ho^{3+}$ powders prepared by using the spray solution containing CA/EG/DMF mixture as the organic additives showed about 168% improved luminescence compared to the phosphor prepared without organic additives. It was concluded that both the increased crystallinity of high-purity monoclinic phase and the decrease of surface area were attributed to the large enhancement of upconversion luminescence.