• 한국세라믹학회지
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• 제37권1호
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• pp.50-56
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• 2000

Precursor gels with the composition of xZrO2·(100-x)SiO2 systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence of tetragonal to monoclinic transformation of ZrO2 was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal ZrO2 occurred through 3-dimensional diffusiion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about 310∼325±10kJ/mol. The growth of t-ZrO2, in proportion to the cube of radius, increased with increasing heating temperature and hteat-treatment time. It was suggested that the diffusion of Zr4+ ions by Ostwald ripening was rate-limiting process for thegrowth of t-ZrO2 crystallite size. The fracture toughness of xZrO2·(100-x)SiO2 systems glass ceramics increased with increasing crystallite size of t-ZrO2. The fracture toughness of 30ZrO2·70SiO2 system glass ceramics heated at 1,100℃ for 5h was 4.84 MPam1/2 at a critical crystaliite size of 40 nm.

• E2M - 전기 전자와 첨단 소재
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• 제16권9호
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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.

• The Korean Journal of Ceramics
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• 제5권4호
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• pp.400-403
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• 1999

The mechanical and electrical properties of hot-pressed and annelaed $\beta$-SiC+39vol.% $ZrB_2$ electroconductive ceramic composites were investigated as a function of the liquid forming additives of $Al_2O_3+Y_2O_3$(6:4 wt%). In this microstructures, no reactions and elongated $\alpha$-SiC grains with equiaxed $ZrB_2$ grains were observed between $\beta$-SiC and $ZrB_2$. The properties of the $\beta$-SiC+39vol.%$ZrB_2$ composites with 4wt% $Al_2O_3+Y_2O_3$ at R.T. are as follows: fracture toughness is 6.37 MPa.m1/2, electical resistivity is $1.51\times10^{-4}\Omega \cdot\textrm{cm}$ and the relative density is 98.6% of the theoretical density. The fracture toughness of the $\beta$-SiC+39 vol.% $ZrB_2$ composites were weakly decreased with increasing amount of $Al_2O_3+Y_2O_3$ additives. Internal stresses due to the difference of $\beta$-SiC and $ZrB_2$ thermal expansion coefficient and elastic modulus mismatch appeared to contribute to fracture toughening in $\beta$-SiC+39vol.%$ZrB_2$ electroconductive ceramic composites.

• 한국안전학회지
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• 제14권3호
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• pp.110-119
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• 1999

This study was conducted to invent brake of non-steel material without using asbestos and disc pad added $ZrSiO_4$ was made. The physical properties and friction characteristics were investigated by varying methods. The physical properties were inspected of shear strength, hardness, heat expansion, specific gravity, % of gashole, thickness variation, weight variation and pH variation. The friction stability was measured by friction coefficient on variations of speed, temperature and deceleration condition. It was found that the physical properties were in general excellent. According to the friction characteristics tests, $ZrSiO_4$ had an abrasive property. As a results, the friction materials containing $ZrSiO_4$ 3~5vol% showed better resistance to fading and improved friction stability than the materials without ZrSiO$_4$.

• 한국세라믹학회지
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• 제34권7호
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• pp.774-780
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• 1997

Porous low reflective coating films of SiO2.ZrO2 system were prepared from the mixed alkoxide solutions of Zr(O-nC3H7)4 and partially prehydrolyzed TEOS by the sol-gel method using the dip-coating technique. In the case of 90SiO2.10ZrO2 porous coating films with HCl and H2O content was 0.3 mole and 4 mole, 378 m2/g of the specific surface area, 0.254 cm3/g of total pore volume, 30-50$\AA$ of average pore diameter. The transmittance of 90SiO2.10ZrO2 porous coated films was 95.38% at the wavelength of 550 nm, compared with the parent glass, the transmittance was increased with 4.38%.

• 한국재료학회지
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• 제18권11호
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• pp.604-609
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• 2008

The sintering behavior of zircon with silica was investigated. Zircon with 5 vol% of sedimentation $SiO_2$ resulted in the apparent density of $4.45\;g/cm^3$, the diametral tensile strength of $12.125\;kgf/cm^2$, and the micro Vickers hardness of 1283 HV. The dissociation temperature and mechanical characteristics of the $ZrSiO_4$ were changed with different kinds of $SiO_2$. $SiO_2$ addition prevented dissociation of $ZrSiO_4$. Zircon with 5 vol% of sedimentation $SiO_2$ and with 5 vol% of fused $SiO_2$ resulted in increased diametral tensile strength and increased micro Vickers hardness by suppression of $ZrSiO_4$ dissociation and low temperature liquid $SiO_2$ formation. Zircon with fumed $SiO_2$ and quartz $SiO_2$ resulted in decreased diametral tensile strength and decreased micro Vickers hardness because of cristobalite and quartz phase formation and high temperature liquid $SiO_2$ formation. Zircon with 10 vol% of $SiO_2$ resulted in decreased diametral tensile strength and decreased micro Vickers hardness because of weak particle coupling due to excess formation of liquid $SiO_2$.

• 한국세라믹학회지
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• 제32권12호
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• pp.1357-1368
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• 1995

Nasigels of composition Na0.75Zr2PSi2O12 and Na3Zr2PSi2O12 have been synthesized by the sol-gel technique using metal alkoxide precursors. The monolithic dry gels of Na0.75Zr2PSi2O12 with no crack have been prepared by the control of the shrinkage rte, but gels of Na3Zr2PSi2O12 were impossible to prepare without cracking. The gels treated up to 80$0^{\circ}C$ led to the formtion of glass but the glasses were converted to the crystalline phases at above this temperature. Crystaline phases precipitated from the Na0.75Zr2PSi2O12 glass were NASICON-like phase, Na2Si2O5, and free Zirconia. Phase that precipitated from the Na3Zr2PSi2O12 was only rhombohedral NASICON. For Na0.75Zr2PSi2O12 gels, framework of PO4 tetrahedra and SiO4(PO4) tetrahedra formed at low temperature but changed to that of SiO4 and SiO4(PO4) tetrahedras as it were crystallized. In the case of Na3Zr2PSi2O12 gel, framework of isolated PO4 and SiO4 tetrahedras formed at low temperature but changed to SiO4(PO4) tetrahedra framework which usually formed in the NASICON crystal after crystallization at high temperature. The gels treated up to 80$0^{\circ}C$ contained the residual water. The ionic conduction was attributed to the motion of proton and Na+ ion at low (up to 150~20$0^{\circ}C$) and high temperatures, respectively. As the temperature of heat treatment increased, ionic conductivity gradaully increased with the extent of precipitation of crystalline phase.

• 산업기술연구
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• 제20권A호
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• pp.247-256
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• 2000

Precursor gels with the composition of $xZrO_2{\cdot}(100-x)SiO_2$ systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence on tetragonal to monoclinic transformation of $ZrO_2$ was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal $ZrO_2$ occurred through 3-dimensional diffusion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about $310{\sim}325{\pm}10kJ/mol$. The growth of $t-ZrO_2$, in proportion to the cube of radius, increased with increasing heating temperature and heat-treatment time. It was suggested that the diffusion of Zr4+ions by Ostwald ripening was rate-limiting process for the growth of $t-ZrO_2$ crystallite size. The fracture toughness of $xZrO_2{\cdot}(100-x)SiO_2$ systems glass ceramics increased with increasing crystallite size of $t-ZrO_2$. The fracture toughness of $30ZrO_2{\cdot}70SiO_2$ system glass ceramics heated at $1,100^{\circ}C$ for 5 h was $4.84Mpam^{1/2}$ at a critical crystaliite size of 40 nm.

• 한국재료학회지
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• 제21권4호
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• pp.220-224
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• 2011

Zircon has excellent thermal, chemical, and mechanical properties, but it is hard to make a dense sintered product because of dissociation during the sintering process. This study analyzes how the addition of $SiO_2$ and $Al_2O_3$ affects the mechanical properties of sintered zircon, particularly in regards to reducing the thermal dissociation and improving the mechanical properties of $ZrSiO_4$. Zircon specimens containing different amounts of $SiO_2$ and $Al_2O_3$ were prepared and sintered to observe how the mechanical properties of $ZrSiO_4$ changed according to the differing amount of $SiO_2$ and $Al_2O_3$. The $ZrSiO_4$ that was used for the starting material was ground by ball mill to an average particle size of 3 ${\mu}m$. The $SiO_2$ and $Al_2O_3$ that was used for additives were ground to an average particle size of 3 ${\mu}m$ and 0.5 ${\mu}m$, respectively. Adding $SiO_2$ resulted in transformation in the liquid phase at high temperatures, which had little effect on suppressing the thermal dissociation but enhanced the mechanical properties of $ZrSiO_4$. When $Al_2O_3$ was added, the mechanical properties of $ZrSiO_4$ decreased due to the formation of pores and abnormal grains in the microstructure of the sintered zircon.

• 한국세라믹학회지
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• 제37권4호
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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.