• Journal of the Korean Ceramic Society
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• v.32 no.5
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• pp.617-625
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• 1995

In order to reduce reflectance of soda-lime glass having average reflectance of 7.35% and refractive index of 1.53, single (SiO2), double (SiO2/20SiO2-80ZrO2), and triple (SiO2/ZrO2/75SiO2-25ZrO2) layers were designed and fabricated on the glass substrate by Sol-Gel method. Stble sols of SiO2-ZrO2 binary system for antireflective (AR) coatings were synthesized with tetraethyl orthosilicate (TEOS) and zirconium n-butoxide as precursors and ethylacetoacetate (EAcAc) as a chelating agent in an atmosphere environment. Films were deposited on soda-lime glass at the withdrawal rates of 3~11 cm/min using the prepared polymeric sols by dip-coating and they were heat-treated at 45$0^{\circ}C$ for 10 min to obtain homogeneous, amorphous and crack-free films. In case of SiO2-ZrO2 binary system, refractive index of film increased with an increase of ZrO2 mol%. Designed optical constant of films could be obtained through varying the withdrawal rate. In the visible region (380~780nm), reflectance was measured with UV/VIS/NIR Spectrophotometer. Average reflectances of the prepared single-layer [SiO2 (n=1.46, t=103nm)], double-layer [SiO2 (n=1.46, t=1-4nm)/20SiO2-80ZrO2 (n=1.81, t=82nm)], and triple-layer [SiO2 (n=1.46, t=104nm)/ZrO2 (n=1.90, t=80nm)/75SiO2-25ZrO2 (n=1.61, t=94 nm)] were 4.74%, 0.75% and 0.38%, respectively.

• Journal of the Korean Ceramic Society
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• v.32 no.7
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• pp.853-857
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• 1995

ZrSiO4 powders were prepared from partially hydrolyzed solution of Si(OC2H5)4 and ZrOCl2.8H2O solution by the sol-gel method and formation rate of ZrSiO4 on the reaction parameter was investigated. In order to prepare homogeneous ZrSiO4 precursor gels, the H2O/Si(OC2H5)4 molar ratio of about 2, the pH of the ZrOCl2.8H2O solution fo about 4 and stirring time of the mixed solutions of about 2 hrs were appropriate. Formation of temperature of ZrSiO4 reduced about 15$0^{\circ}C$ by milling and formation of ZrSiO4 at 1300~135$0^{\circ}C$ showed an accelerative increase through the hedvall effect by silica.

• 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.

• Journal of the Korean Ceramic Society
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• v.37 no.12
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• pp.1178-1186
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• 2000

타일의 내마모성과 내산성을 향상시키기 위해 결정화유리가 최근에 새로운 유약 재료로서 소개되고 있다. 신 유약의 연구에 사용된 조성은 $Ca_2$ZrSi$_4$O$_{12}$ 상에 근접하는 CaO-ZrO$_2$-SiO$_2$계의 유리조성의 분말로, 마이크로파 가열 (2.45 GHz)에 의해서 900-120$0^{\circ}C$의 0-20분간 소성되어 평가되었다. 그 결과, 100$0^{\circ}C$ 이상에서 소성한 시편은 내부 결정화를 나타내었으며, 결정상은 미세(5$mu extrm{m}$)한 크기를 갖는 $Ca_2$ZrSi$_4$O$_{12}$가 주 결정상이며, $Ca_2$ZrSi$_4$O$_{12}$, CaSiO$_3$, SiO$_2$의 세 상이 나타났다. 소결체의 미세구조는 사용한 유리분말의 입도의 영향을 받았다. 미세분말 (<38$\mu\textrm{m}$)을 이용한 소결체의 조직이 조세분말 (45-150$\mu\textrm{m}$)의 경우보다 수축율면에서 높았으며 낮은 기공도를 갖는 미세구조를 가졌다. 마이크로파에 의한 유리분말의 소성은 1000-120$0^{\circ}C$ 구간에서 10분 이내 결정화가 완료되는 급속 가열 공정이었으며 CaO-ZrO$_2$-SiO$_2$계 결정화 유리 제조에 균일한 체적가열을 할 수 있었다.

• Journal of the Korean Ceramic Society
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• v.30 no.9
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• pp.731-739
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• 1993

R-curve measurements were performed on Al2O3(matrix)-ZrO2-SiC whisker composite and Al2O3-ZrO2, Al2O3-SiC whisker composites in the favor of comparing the effect of ZrO2 and SiC whisker, as a second phase, to Al2O3 matrix. Al2O3-SiC whisker and Al2O3-ZrO2-SiC whisker were fabricated by hot pressing at 1$700^{\circ}C$, 15MPa and Al2O3-ZrO2 by pressureless sintering at 1$600^{\circ}C$. A controlled flaw/strength technique was utilized to determine fracture resistance as a function of crack extension and R-curve behaviour was determined from the relationship which is KR=K0(Δa)m. R-curveresults were KR=6.173$\times$Δa0.031 for Al2O3-ZrO2, KR=18.796$\times$Δa0.172 for Al2O3-SiC whisker and KR=11.96$\times$Δa0.110 for Al2O3-ZrO2-SiC whisker composite. From the analysis of R-curve and expeirmental data above three composites, it is found that R-curve behaviour of Al2O3-ZrO2-SiC whisker composite was dominated initially by the strengthening effect of ZrO2 and after, some extended crack were influenced by the effect of SiC whisker. Analysis of SEM and X-ray data revealed that whisker bridging in the crack wake and whisker pull-out mechanisms were the main mechanism for the R-curve behaviour.

• Journal of the Korean Vacuum Society
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• v.9 no.4
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• pp.315-320
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• 2000

We have investigated the crystal structure and electrical properties of Pt/SBT/$ZrO_2$/Si (MFIS) and Pt/SBT/Si (MFS) structures for the gate oxide of ferroelectric memory. XRD spectra and SEM showed that the SBT film of SBT/$ZrO_2$/Si structure had larger grain than that of SBT/Si structure. $ZrO_2$ film between SBT film and Si substrate is confirmed as a good candidate for a diffusion barrier by the analysis of AES. The remanent polarization decreased and coercive voltage increased in Pt/SBT/$ZrO_2$/Pt/$SiO_2$/Si structure. This effect may increase memory window of MFIS structure directly related to the coercive voltage. From the capacitance-volt-age characteristics, the memory windows of Pt/SBT (210 nm)/$ZrO_2$ (28 nm)/Si structure were in the range of 1~l.5 V at the applied voltage of 4~6 V. The current densities of Pt/SBT/ZrO$_2$/Si with as -deposited Pt electrode and annealed at $800^{\circ}C$ in $O_2$ambient were $8\times10^{-8} A/\textrm{cm}^2$ and $4\times10^{-8}A/\textrm{cm}^2$ , respectively.

• Journal of the Korean Ceramic Society
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• v.37 no.1
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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.

• Journal of the Korean Ceramic Society
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• v.52 no.1
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• pp.19-22
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• 2015

The joining behavior of YSZ ceramics to the glasses used in the $9Al_2O_3-24ZrO_2-51SiO_2-16R_2O$ and $9Al_2O_3-24ZrO_2-51SiO_2-7La_2O_3-9R_2O$ (wt%) glass systems was investigated. The glass transition and softening temperatures were determined to be $430^{\circ}C$ and $760^{\circ}C$, respectively. The behavior of the contact angle was inversely proportional to an increase in the temperature. The Zr element in YSZ acted as a nucleation agent and contributed to the bonding behavior at the interface.

• Transactions of the Korean Society of Mechanical Engineers A
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• v.39 no.9
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• pp.901-907
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• 2015

The Vickers hardness test is a common method used to characterize the hardness of ceramic materials. However, the hardness is not a deterministic value, but is a random variable. The objective of this paper is to investigate the statistical properties of the bending strength and a set of Vickers hardness values in single $ZrO_2$ and composite $ZrO_2/SiC$ with a SiC additive. In this work, we compare the characteristic value and variation with the results based on Weibull statistical analysis. The probability distributions of the bending strength and Vickers hardness agreed relatively well with the Weibull distribution. We evaluate the scale parameter and shape parameter in asreceived $ZrO_2$ and $ZrO_2/SiC$ composite ceramics, as well as in their heat treated ceramics.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.138-138
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• 2017

차세대 CMOS 소자의 지속적인 고직접화를 위해서는 높은 gate capacitance와 낮은 gate leakage current를 확보를 위한, 적절한 metal gate electrode와 high-k dielectric 물질의 개발이 필수적으로 요구된다. 특히, gate dielectric으로 적용하기 위한 다양한 high-k dielectric 물질 후보군 중에서, 높은 dielectric constant와, 낮은 leakage current, 그리고 Si과의 우수한 열적 안정성을 가지는 Zr silicates 또는 Hf silicates(ZrSiO4와 HfSiO4) 물질이 높은 관심을 받고 있으며, 이를 원자층 증착법을 통해 구현하기 위한 노력들이 있어왔다. 그러나, 현재까지 보고된 원자층 증착법을 이용한 Zr silicates 및 Hf silicates 공정의 경우, 개별적인 Zr(또는 Hf)과 Si precursor를 이용하여 ZrO2(또는 HfO2)과 SiO2를 반복적으로 증착하는 방식으로 Zr silicates 또는 Hf silicates를 형성하고 있어, 전체 공정이 매우 복잡해지는 문제점 뿐 아니라, gate dielectric 내에서 Zr과 Si의 국부적인 조성 불균일성을 야기하여, 제작된 소자의 신뢰성을 떨어뜨리는 문제점을 나타내왔다. 따라서, 본 연구에서는 이러한 문제점을 개선하기 위하여, 하나의 precursor에 Zr (또는 Hf)과 Si 원소를 동시에 가지고 있는 DNS-Zr과 DNS-Hf bimetallic precursor를 이용하여 새로운 ZrSiO4와 HfSiO4 ALD 공정을 개발하고, 그 특성을 살펴보고자 하였다. H2O와 O3을 reactant로 사용한 원자층 증착법 공정을 통하여, Zr:Si 또는 Hf:Si의 화학양론적 비율이 항상 일정한 ZrSiO4와 HfSiO4 박막을 형성할 수 있었으며, 이들의 전기적 특성 평가를 진행하였으며, dielectric constant 및 leakage current 측면에서 우수한 특성을 나타냄을 확인할 수 있었다. 이러한 결과를 바탕으로, bimetallic 전구체를 이용한 ALD 공정은 차세대 고성능 논리회로의 게이트 유전물질에 응용이 가능할 것으로 판단된다.