• 한국결정성장학회지
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• 제12권3호
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• pp.126-132
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• 2002

$ZrOCl_2{\cdot}8H_2O$ 수용액과 KOH 수용액의 반응으로부터 얻은 침전물을 $100^{\circ}C$에서 24 시간 동안 숙성시켜 정방정상 지르코니아를 제조한 후 수열합성 조건을 변화시킴으로써 비등방성 형상의 나노 결정형 지르코니아 분말을 합성하였다. 수열합성 시 반응온도와 반응시간이 증가할수록 정방정상인 구형 입자는 감소하고 상대적으로 단사정상 spindle-like 입자와 막대상 입자가 증가하였다. NaOH 용액의 농도가 증가함에 따라 입성장과 함께 정방정상에서 단사정상으로의 상전이가 촉진되었으며, 저온에서 반응시간이 짧은 경우 합성한 분말들은 반응초기에 응집된 입자들이 NaOH 용액에 부분적으로 용해되면서 응집입자 및 결정입자 크기가 감소되어 비표면적이 증가하였다가 반응시간이 길어지고 반응온도가 높아짐에 따라 입성장에 의하여 점차 비표면적이 감소하였다.

• 한국세라믹학회지
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• 제42권2호
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• pp.123-126
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• 2005

용매열법으로 출발물질의 농도를 변수로 차여 $BaTiO_3$ 분말을 합성하였다. 평균입자크기는 출발물질의 농도에 따라 비례하였는데 TiO_2를 기준으로 1/16M 농도에tj 59nm이었고 1/2M 농도에서는 89nm까지 증가하였다. 평균입자 크기가 89nm인 BT 분말에 대하여 리트벨트법에 의하여 분석한 결과 상분율은 정방정상 $75.5\%$이었고, 격자상수는 정방정상은 a=0.3999(nm), c=0.40319(nm)이고, 입방정상은 a=0.4015(nm)이었다. 이 분말을 $500^{\circ}C$ 1시간 열처리 후 TEM분석을 한 결과, 분말 내부에 수산 이온들이 거의 존재하지 않음을 확인하였다.

• 한국세라믹학회지
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• 제34권6호
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• pp.645-651
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• 1997

입성장 제어없이 정방정 니르코니아의 파괴인성과 상 안정성을 증진시키기 위해 $Y_{2}O_{3}$와 $Nb_{2}O_{5}$가 첨가된 정방정 지르코니아를 상압소결방법으로 제조하였다. 지르코니아 복합체는 상 안정성이 뛰어난 조성에 상변화가 우수한 조성을 중량비로 혼합 합성하였다. 상변화가 우수한 조성을 15 wt% 첨가한 복합체와 동일한 단일조성의 경우 공기중에 $1500^{\circ}C$ 10시간 소결후 9$MPam^{1/2}$의 파괴인성값과 $220^{\circ}C$에서 $1000^{\circ}C$/까지 100시간이상 agmg을 한 뒤에도 우수한 저온 및 고온 상 안정성이 관찰되었다. 복합체와 상응하는 단일조성은 90.24 mol% $ZrO_2$-5.31 mol% $Y_{2}O_{3}$ mol% $Nb_{2}O_{5}$이었다. 조직관찰 결과 결정립은 소결시간에 따라 증가하였으며 미세균열이나 twinning은 발견되지 않았다.

• 한국세라믹학회지
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• 제54권6호
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• pp.530-534
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• 2017

The figures of merit in the on-resonance and off-resonance conditions ($FOM_{on}$ and $FOM_{off}$) for the piezoelectric energy harvester (PEH) were measured and compared in $[(K_{0.485}Na_{0.515})_{1-X}Li_X](Nb_{0.99}Ta_{0.01})O_3$ (x = 0.04 ~ 0.09) (KNLNT) ceramics with various Li contents. The crystal structure of CuO-doped KNLNT ceramics changes from orthorhombic to tetragonal around the Li fraction of 0.065. The stable temperature range for the tetragonal phase widens to both higher and lower temperatures as Li is substituted. The piezoelectric charge constant ($d_{33}$), electromechanical coupling factor ($k_p$) and mechanical quality factor ($Q_m$) have maximum values at the Li fraction between 0.055 and 0.065 where the phase boundary lies between the orthorhombic and tetragonal phases. Both $FOM_{on}$ and $FOM_{off}$ have peak values around the phase boundary but the peak compositions are not exactly coincided. The optimal Li fraction in the KNLNT ceramic for a PEH application was found to be between 0.055 and 0.065.

• 한국전기전자재료학회논문지
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• 제36권5호
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• pp.513-519
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• 2023

It was reported that a tetragonal phase can be stabilized with maintaining good piezoelectric properties when Na_0.5K_0.5NbO₃ (KNN) is modified with 0.06 mol SrTiO₃. However, such a high amount of SrTiO₃ leads not only to poor sinterability but low Curie temperature (T_C). To maintain high TC with good piezoelectric properties in KNN-based lead-free piezoelectric ceramics, this study investigates the effect of Li-doping on the dielectric and piezoelectric properties of 0.96Na_0.5K_0.5NbO₃-0.04SrTiO₃ (KNN-4ST) ceramics. As a result, the orthorhombic-tetragonal phase transition was observed at 2 mol% Li₂CO₃ modified KNN-4ST ceramics, whose T_C, d₃₃ and k_p values are 328℃, 165pC/N and 0.33, respectively.

• The Journal of Advanced Prosthodontics
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• 제1권3호
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• pp.113-117
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• 2009

STATEMENT OF PROBLEM. Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported. PURPOSE. The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM). MATERIAL AND METHODS. Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad $S\ddot{a}ckingen$, Germany) were prepared in 40 mm (length) $\times$ 4 mm (width) $\times$ 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and $225^{\circ}C$ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences ($\alpha$= .05). RESULTS. The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below $125^{\circ}C$ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above $150^{\circ}C$, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa. CONCLUSION. The monoclinic phase started to appear after aging treatment above $100^{\circ}C$. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above $175^{\circ}C$. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

• 한국재료학회지
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• 제22권7호
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• pp.342-345
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• 2012

The dielectric properties and phase transformation of poled <001>-oriented $Pb(Mg_{1/3}Nb_{2/3})O_3-x%PbTiO_3$(PMN-x%PT) single crystals with compositions of x = 20, 30, and 35 mole% are investigated for orientations both parallel and perpendicular to the [001] poling direction. An electric-field-induced monoclinic phase was observed for the initial poled PMN-30PT and PMN-35PT samples by means of high-resolution synchrotron x-ray diffraction. The monoclinic phase appears from $-25^{\circ}C$ to $100^{\circ}C$ and from $-25^{\circ}C$ to $80^{\circ}C$ for the PMN-30PT and PMN-35PT samples, respectively. The dielectric constant (${\varepsilon}$)-temperature (T) characteristics above the Curie temperature were found to be described by the equation$(1/{\varepsilon}-1/{\varepsilon}_m)^{1/n}=(T-T_m)/C$, where ${\varepsilon}_m$ is the maximum dielectric constant and $T_m$ is the temperature giving ${\varepsilon}_m$, and n and C are constants that change with the composition. The value of n was found to be 1.82 and 1.38 for 20PT and 35PT, respectively. The results of mesh scans and the temperature-dependence of the dielectric constant demonstrate that the initial monoclinic phase changes to a single domain tetragonal phase and a to paraelectric cubic phase. In the ferroelectric tetragonal phase with a single domain state, the dielectric constant measured perpendicular to the poling direction was dramatically higher than that measured in the parallel direction. A large dielectric constant implies easier polarization rotation away from the polar axis. This enhancement is believed to be related to dielectric softening close to the morphotropic phase boundary.

• 한국세라믹학회지
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• 제33권6호
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• pp.637-644
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• 1996

$Zr(i-OC_3H_7)_4$로부터 가수분해법으로 Y-TZP 분말을 제조한 다음, 하소온도를 달리하여 정방정상의 상온 안정화와 25$0^{\circ}C$에서의 등온상전이 거동을 고찰하였다. 그 결과, 정방정상 지르코니아 입자의 상온 안정화 효과는 하소온도가 낮을 수록, 고용된 $Y_2O_3$의 양이 클 수록 증가하였다. 또한 25$0^{\circ}C$에서 aging 하면서 Y-TZP 분말의 등온상전이를 관찰한 결과, 입자크기 효과 및 고용효과에 의해 상온 안정화된 정방정상 지르코니아 입자에서는 aging 시 등온상전이가 일어나지 않고, 반면에 구속효과에 의하여 상온 안정화된 정방정상 입자에서는 등온상전이가 활발히 진행되었다. 등온상전이로 생성된 단사정상 입자의 내부에는 많은 쌍정과 미세균열들이 존재하였는데 이는 상전이시 변형에너지를 감소시키기 위한 것으로 사료되었다.

• 한국전기전자재료학회논문지
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• 제28권3호
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• pp.165-169
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• 2015

In this paper, in order to develop the composition ceramics with the excellent dielectric properties, $Pb(Mg_{1/2}W_{1/2})_{0.03}(Ni_{1/3}Nb_{2/3})_{0.09}(Zr_{0.5}Ti_{0.5})_{0.88}O_3$ ceramics were fabricated by the conventional solid-state method. The effects of ZnO addition on their microstructure and piezoelectric properties were systematically investigated. The rhombohedral-tetragonal phase coexistence has been found in the ceramics without ZnO content and then with further increasing ZnO content, specimens exhibited tetragonal phase. The optimized ZnO content formed liquid phase and aided the grain growth of specimens. When 0.4 wt% ZnO was added, the optimal physical properties ($d_{33}=422pC/N$, $d_{31}=161pC/N$, ${\varepsilon}_r=1,905$, $k_p=0.55$, $Q_m=160$) were obtained.

• Transactions on Electrical and Electronic Materials
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• 제18권6호
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• pp.334-337
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• 2017

In this paper, to develop the ceramics with high $d_{33}$ and high $Q_m$ for ultrasonic transducer applications, $0.10Pb(Ni_{1/3}Nb_{2/3})O_3-0.07Pb(Mn_{1/3}Nb_{2/3})O_3-0.83Pb(Zr_{0.5}Ti_{0.5})_{0.83}O_3$ (PNN-PMN-PZT) ceramics were sintered at $940^{\circ}C$ using $CuO-Li_2CO_3-Bi_2O_3$ (CLBO) as a sintering aid by a traditional solid-state technique. The influence of zinc oxide additive on the physical properties of the prepared ceramics were systematically investigated. The R-T (rhombohedral-tetragonal) phase coexistence was found in the ceramics without zinc oxide additive and with increasing amounts of ZnO additive, the specimens showed a tetragonal phase. The formation of a liquid phase between ZnO and $Bi_2O_3$ contributed significantly to the grain growth of specimens. For the 0.1 wt% ZnO ceramics, the optimal physical properties of $d_{33}=370pC/N$, ${\varepsilon}_r=1,344$, $k_p=0.621$, and $Q_m=1,523$ were obtained.