• Bulletin of the Korean Chemical Society
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• v.22 no.12
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• pp.1309-1315
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• 2001

Zirconium sulfate supported on zirconia catalysts were prepared by impregnation of powdered $Zr(OH)_4$ with zirconium sulfate aqueous solution followed by calcining in air at high temperature. The characterization of prepared catalysts was performed using Fourier transform infrared (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and by the measurement of surface area. The addition of zirconium sulfate to zirconia increased the phase transition temperature of $ZrO_2$ from amorphous to tetragonal due to the interaction between zirconium sulfate and zirconia, and the specific surface area and acidity of catalysts increased in proportion to the zirconium sulfate content up to 10 wt% of $Zr(SO_4)_2$. Infrared spectra of ammonia adsorbed on $Zr(SO_4)2}ZrO_2$ showed the presence of Bronsted and Lewis acid sites on the surface. $10-Zr(SO_4)_2}ZrO_2$ calcined at $600^{\circ}C$ exhibited maximum catalytic activities for 2-propanol dehydration and cumene dealkylation. The catalytic activities for both reactions were correlated with the acidity of catalysts measured by ammonia chemisorption method.

• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.879-885
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• 1994

Coprecipitation technique was used to synthesize ZrO2+12 mol% CeO2 powders with ZrOCl2.8H2O and Ce(NO3)3.6H2O as starting materials. The powders were dried on different conditions such as distilled water, ethanol, and azeotropic distillation. The powders prepared by azeotropic distillation showed weak aggregation of particles and the average particle size of powders calcined at 85$0^{\circ}C$ for 1 hour was 0.19 ${\mu}{\textrm}{m}$. The optimum sintering temperature and holding time are 130$0^{\circ}C$ and 2.5~10 hours, respectively. Beyond the optimum conditions, a phase transition from tetragonal to monoclinic causes to produce cracks in the sintered bodies and to decrease the density.

• Electrical & Electronic Materials
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• v.16 no.9
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• pp.64.2-65
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• 2003

A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{＋}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{＋}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.

• Korean Journal of Materials Research
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• v.26 no.2
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• pp.95-99
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• 2016

In this study, 5 um sized $ZrSiO_4$ was ground to 1.9 um, 0.3 um, and 0.1 um sized powders by wet high energy milling process, and the sintering characteristics were observed. Pure $ZrSiO_4$ itself can-not be sintered to these levels of theoretical density, but it was possible to sinter $ZrSiO_4$ powder of nano-scale size of, -0.1 um to the theoretical density and to lower the sintering temperature for full density. Also, the decomposition of $ZrSiO_4$ with a size in the micron range resulted in the formation of monoclinic $ZrO_2$; however, in the nano sized range, the decomposition resulted in the tetragonal phase of $ZrO_2$. So, it was possible to improve the sintering characteristics of nano-sized $ZrSiO_4$ powders.

• Journal of the Korean Ceramic Society
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• v.39 no.11
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• pp.1055-1062
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• 2002

The phase stability and the Low Temperature Degradation(LTD) mechanism of Tetragonal Zirconia Polycrystals(TZP), sintered specimens of $Y_2O_3$-Stabilized Zirconia(2Y-TZP), doped with trivalent cations, were evaluated by investigating meachnical properties, Raman spectra, lattice parameter variation and the oxygen vacancy behavior under applied electric field. XRD observation was put forward on 2Y-TZP doped with trivalent cation whose ionic radii were larger than $Zr^{4+}(Sc^{3+},\;Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+},\;La^{3+})$ up to 2 mol% and sintered at 1500 h for 1h. For $La^{3+}$ doping, the stability of tetragonal phase was degraded due to the formation of the pyrochlore phase $(La_2Zr_2O_7)$ as the dopant content increased above exceeded 0.5 mol%. As the dosage increased, tetragonal phase maintained for the case of $Sc^{3+}$, whose radius was similar to $Zr^{4+}$, on the other hand, the cubic phase was formed for the cases of $Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+}$. As the radii of dopant cation increased, c/a ratio increased and it was experimentally observed that the amount of monoclinic phase decreased when the specimens were annealed at $220{\circ}C$ for 500 h.

• Journal of the Korean Ceramic Society
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• v.37 no.4
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• pp.359-367
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• 2000

Particulate composites of Al2O3/SiC, Al2O3/ZrO2 and Al2O3/ZrO2/SiC have been fabricated to investigate their R-curve behaviors and toughening mechanisms. Al2O3 containing 30 vol% SiC particles of 3${\mu}{\textrm}{m}$ showed rising R-curve behavior owing to the strong crack bridging by SiC particles. The fracture toughness reached 9.1 MPa {{{{ SQRT {m} }} at the crack length of 1000${\mu}{\textrm}{m}$. On the other hand, ZrO2-toughened Al2O3 had a high flat R-curve since it rose steeply in the short crack region due to the well known transformation toughening. For Al2O3/ZrO2/SiC composites, the R-curve behavior was similar to that of Al2O3/SiC but with slightly higher toughness. The SiC particles in this composite decreased the amount of transformable tetragonal phase to reduce the effect of transformation toughening by 50%. It was also found that the fracture toughness of this composite with two different toughening mechanisms was markedly lower than that estimated by the simple addition of two contributions.

• Journal of the Korean Ceramic Society
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• v.31 no.1
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• pp.104-114
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• 1994

ZrO2 fibers were fabricated by means of the Sol-Gel process using Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 solution as a starting material. The optimum experimental parameters such as molar ratio of starting materials, concentration, temperature, viscosity, the amounts of stabilizer and the pH of solution were determined. The experimentally determined optimum variables which produce good ZrO2 fibers were used to manufacture the Y2O3-and CaO-ZrO2 fibers. The amounts of Y2O3 and CaO were varied within the range from 1.5~5 mol% and 3~15 mol% respectively. The phase transformation and microstructural evolution of the fabricated ZrO2 gel fibers were investigated after heat treatments up to 120$0^{\circ}C$ by X-ray diffraction, Raman microprobe spectroscopy, SEM, and specific surface area and pore volume measurements. From the analysis of X-ray diffraction and Raman spectra, the phase of heat treated Y2O3-and CaO partially stabilized ZrO2 gel fibers(Y2O3:2.5~3 mol%, CaO:6~9 mol%) were identified as a tetragonal phase up to 100$0^{\circ}C$. The maximum tensile strength of 2.5Y2O3-97.5ZrO2 and 6CaO-94ZrO2 (in mol%) fibers heat treated at 100$0^{\circ}C$ for 1 hr was found be 1.3~2 GPa with diameters of 10~20 ${\mu}{\textrm}{m}$.

• Korean Journal of Materials Research
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• v.14 no.6
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• pp.394-398
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• 2004

A Ti47Al1.7W-3.7Zr alloy was oxidized between $900^{\circ}C$ and $1050^{\circ}C$, and the oxide scales formed were studied. The oxide scales consisted primarily of an outer$TiO_2$ layer, an intermediate $Al_2$$O_3$-rich layer, and an inner mixed ($TiO _2$ + $Al_2$$O_3$) layer. Besides $TiO_2$ and $Al_2$$O_3$, oxidation led to the formation of some $Ti_2$AlN and TiN. Both W and Zr were preferentially segregated below the intermediate $Al_2$$O_3$-rich layer. Tungsten in the oxide scale was present as $WO_3$ and ${Ti}_{x}$$W_{1-x}$, whereas zirconium as monoclic-$ZrO_2$ and tetragonal-$ZrO_2$.

• Korean Journal of Materials Research
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• v.24 no.5
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• pp.259-265
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• 2014

$ZrO_2$ films were coated on aluminum etching foil by the sol-gel method to apply $ZrO_2$ as a dielectric material in an aluminum(Al) electrolytic capacitor. $ZrO_2$ films annealed above $450^{\circ}C$ appeared to have a tetragonal structure. The withdrawal speed during dip-coating, and the annealing temperature, influenced crack-growth in the films. The $ZrO_2$ films annealed at $500^{\circ}C$ exhibited a dielectric constant of 33 at 1 kHz. Also, uniform $ZrO_2$ tunnels formed in Al etch-pits $1{\mu}m$ in diameter. However, $ZrO_2$ film of 100-200 nm thickness showed the withstanding voltage of 15 V, which was unsuitable for a high-voltage capacitor. In order to improve the withstanding voltage, $ZrO_2$-coated Al etching foils were anodized at 300 V. After being anodized, the $Al_2O_3$ film grew in the directions of both the Al-metal matrix and the $ZrO_2$ film, and the $ZrO_2$-coated Al foil showed a withstanding voltage of 300 V. However, the capacitance of the $ZrO_2$-coated Al foil exhibited only a small increase because the thickness of the $Al_2O_3$ film was 4-5 times thicker than that of $ZrO_2$ film.

• Korean Journal of Materials Research
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• v.18 no.4
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• pp.211-217
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• 2008

A $ZrO_2$ coating solution containing $ZrO_2$ photo-catalysis, which is transparent in visible light, was prepared by the hydrolysis of alkoxide, and thin films on the $SiO_2$ glass substrate were formed in a dipcoating method. These thin films were heat-treated at temperatures ranging from $250^{\circ}C-800^{\circ}C$ and their characteristics were subjected to thermal analysis, XRD, spectrometry, SEM, EDS, contact angle measurement, and AFM. Tetragonal $ZrO_2$ phase was found in the thin film heat treated at $450^{\circ}C$, and anatase $TiO_2$ phase was detected in the thin film heat-treated at $600^{\circ}C$ and above. The thickness of the films was approximately 300 nm, and the roughness was 0.66 nm. Thus, the film properties are excellent. The films are super hydrophilic with a contact angle of $4.0^{\circ}$; moreover, they have self-cleaning effect due to the photo catalytic property of anatase $TiO_2$.