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조소라,김대수,조유리,손신중,강형원,남산,한승호,Jo, Sora,Kim, Daesu,Cho, Yuri,Son, Sin Joong,Kang, Hyung-Won,Nahm, Sahn,Han, Seung Ho 한국전기전자재료학회 2018 전기전자재료학회논문지 Vol.31 No.4
The piezoelectric properties of $0.65Pb(Zr_{1-x}Ti_x)O_3-0.35Pb(Zn_{1/6}Ni_{1/6}Nb_{2/3})O_3$ ($PZT_x-PZNN$) ceramics with $0.530{\leq}x{\leq}0.555$ were investigated for application to piezoelectric energy harvesters. Although a morphotropic phase boundary (MPB) was found at approximately x = 0.545, the ceramic with the highest figure of merit (FOM) ($d_{33}{\times}g_{33}$) was observed at a composition of x = 0.540. Values of this figure of merit, $d_{33}{\times}g_{33}$, of $19.6pm^2/N$ and $20.2pm^2/N$ were obtained from $PZT_{0.540}-PZNN$ ceramics sintered at $920^{\circ}C$ and $950^{\circ}C$, respectively. A high output power of $937{\mu}W$ and a high power density of $3.3mW/cm^3$ were obtained from unimorph-type piezoelectric energy harvesters fabricated using $PZT_{0.540}-PZNN$ ceramic sintered at $920^{\circ}C$ for 4h.
0.65Pb(Zr1-xTix)O3-0.35Pb(Zn1/6Ni1/6Nb2/3)O3 세라믹의 압전 특성 및 압전 에너지 하베스터 적용
조소라,김대수,조유리,손신중,강형원,남산,한승호 한국전기전자재료학회 2018 전기전자재료학회논문지 Vol.31 No.4
The piezoelectric properties of 0.65Pb(Zr1-xTix)O3-0.35Pb(Zn1/6Ni1/6Nb2/3)O3 (PZTx-PZNN) ceramics with 0.530≤x≤0.555 were investigated for application to piezoelectric energy harvesters. Although a morphotropic phase boundary(MPB) was found at approximately x=0.545, the ceramic with the highest figure of merit (FOM) (d33×g33) was observedat a composition of x=0.540. Values of this figure of merit, d33×g33, of 19.6 pm2/N and 20.2 pm2/N were obtained fromPZT0.540-PZNN ceramics sintered at 920℃ and 950℃, respectively. A high output power of 937 μW and a high powerdensity of 3.3 mW/cm3 were obtained from unimorph-type piezoelectric energy harvesters fabricated using PZT0.540-PZNNceramic sintered at 920℃ for 4h.
HRTEM에 의한 pseudo-brookite 형 화합물$(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$에서의 변조구조 관찰
이확주,박현민,조양구,류현,남산,Lee, Hwack-Joo,Park, Hyun-Min,Cho, Yang-Koo,Ryu, Hyun,Nahm, Sahn,Bando, Y. 한국현미경학회 1999 Applied microscopy Vol.29 No.1
Pseudo-brookite 구조의 $MgTi_2O_5$와 이와 유사한 구조를 갖는 $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$에 관한 미세구조를 200kV에서 작동되는 고분해능 투과전자현미경을 사용하여 관찰하였다. 변조구조는 $MgTi_2O_5$에서는 발견되지 않았으나, $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$에서는 복잡한 구조가 발견되었다. $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ 구조의 전자회절패턴은 $MgTi_2O_5$와 fundamental 회절점들은 유사하나 4가지 형태의 초격자 회절점이 더 존재하였다. 변조구조의 주기는 [220] 방향으로 3.63nm, 0.79nm, 그러고 0.64 nm를 이루고 [420] 방향으로는 0.81nm를 이룬다. 미세구조 관찰중 전자빔에 의하여 상전이가 야기되어 변조된 구조에서 좀 더 단순화된 변조없는 구조로 가역적으로 전환한다. 가해지는 전자빔에 의한 손상기구는 ledge 구조의 kink에서 void가 형성되어 작은 결정들로 갈라지고 손상이 커지면, 최종적으로 결정성을 잃게 된다. Microstructural observations on the pseudo-brookite $MgTi_2O_5$ and the similar type of $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ were carried out using a top-entry HRTEM working at 200 kV. The modulated structures were found in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$, however, not in $MgTi_2O_5$. The electron diffraction patterns of sublattice in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ are quite similar to those of pseudo-brookite $MgTi_2O_5$. but the complicated superlattice reflections are present in the diffraction patterns. Four types of modulations have been found. The periodicities for the modulated structure are found to be 3.63 nm, 0.79 nm and 0.64 nm along [220] direction, and 0.81 nm along [420] direction. The phase transition from the modulated structure to the unmodulated one was also observed in situ due to the electron beam irradiation reversibly. Further damage by the electron beam made the crystal to be fragmented into many small crystals with the formation of the voids at the kinks in ledged structure of the surface. The anisotropic arrangements of In and O atoms in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ might cause the compound to be unstable under the electron beam.
Pyrochlore형 화합물 $In_2(Ti_{1.7}Zn_{0.3})O_{0.67}$과 $In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$에서의 변조구조 관찰
이확주,박현민,조양구,류현,남산,Lee, Hwack-Joo,Park, Hyun-Min,Cho, Yang-Koo,Ryu, Hyun,Nahm, Sahn,Bando, Y. 한국현미경학회 1999 Applied microscopy Vol.29 No.4
Pyrochlore 구조를 갖는 $Lu_2Ti_2O_7$와 그와 유사한 구조를 갖는 화합물, $In_2(Ti_{1.7}Zn_{0.3})O_{6.7}$와 $In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$에 대한 미세구조 관찰을 200kV에서 작동되는 HRTEM을 이용하여 관찰하였다. 두 화합물에서는 변조구조가 관찰되었으나 pyrochlore구조인 $Lu_2Ti_2O_7$에서는 관찰되지 않았다. 전자회절패턴 분석에서는 변조구조는 incommensurate이고 [220] 방향으로 sublattice의 2.69배로 그 주기가 0.953 nm인 초격자가 관찰되었다. 고분해능 격자상에서는 sublattice의 2배 또는 3배의 초격자들로 조합되며 평균적으로 2.7배로 그 주기가 0.967 nm가 되는 초격자상이 관찰되었다. 두 화합물의 결정구조는 입방정 pyrochlore 구조와 아주 유사하나 입방정 축은 $90^{\circ}$에서 약간 벗어난 구조를 갖는다. 변조구조는 전자빔에 의하여 점차적으로 변조구조가 없는 구조로 비가역적으로 변환된다. Microstructural observations on the pyrochlore-type $Lu_2Ti_2O_7$ and the similar type of compounds, $In_2(Ti_{1.7}Zn_{0.3})O_{6.7}$ and $In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$ which were made by the isothermal heat-treatment at 1623K for 18 days in Pt tube, were carried out using a top-entry HRTEM working at 200 kV. The modulated structures were found in both compounds, however, not in $Lu_2Ti_2O_7$. From the electron diffraction pattern analysis, the modulated superlattices are incommensurate and are 2.69 times of sublattices along (220) direction. The high resolution TEM images have shown that the superlattices consist of alternate superlattices which are composed of two or three sublattices, resulting in the average of 2.7 times of sublattices in accordance with the analysis of electron diffraction patterns. The crystal structures of both compounds are found to quite similar to those of pyrochlore, however the evidence that the cubic axes are slightly deviated from right angle. The modulated structure has gradually changed to the unmodulated structure induced by electron irradiation.
$(Li_{1/2}Pr_{1/2})TiO_3$ 세라믹의 미세구조 평가
이확주,류현,박현민,조양구,남산,Lee, Hwack-Joo,Ryu, Hyun,Park, Hyun-Min,Cho, Yang-Koo,Nahm, Sahn 한국현미경학회 2002 Applied microscopy Vol.32 No.3
복합 페로브스카이트$(Li_{1/2}Pr_{1/2})TiO_3$ (LPT)의 미세구조를 X-ray diffractometry와 투과전자현미경으로 관찰하였다. LPT는 A-site 양이온 결핍에 의한 vacancy ordering을 갖고 있으며 산소 팔면체의 antiphase tilting과 inphase tilting 그리고 A-site 양이온의 anti-parallel shift 가 관찰되었다. 스피노달 분해에 의한 상변태도 관찰되었다. 측정된 NPT 재료의 유전체 특성은 ${\varepsilon}_r=84.6,\;Q\;{\Large f}_o=776\;GHz,\;{\tau}_{f}=-233.66ppm/^{\circ}C$이었다. Microstructural investigations of $(Li_{1/2}Pr_{1/2})TiO_3$ (LPT) complex perovskite compounds were carried out using X-ray diffractometry and transmission electron microscopy. LPT has not only the ordering of A-site cation deficiencies but also has the antiphase and inphase tilting of oxygen octahedron and the antiparallel shift of cations. Both the antiphase boundaries and the ferroelastic domains are present in the microstructure. Spinodal decomposition is found in the microstructure. The measured dielectric properties were ${\varepsilon}_r=84.6,\;Q\;{\Large f}_o=776\;GHz,\;{\tau}_{f}=-233.66ppm/^{\circ}C$.
Complex Perovskite $(Na_{1/2}Pr_{1/2})TiO_3$의 미세구조 관찰
이확주,류현,박현민,조양구,남산,Lee, Hwack-Joo,Ryu, Hyun,Park, Hyun-Min,Cho, Yang-Koo,Nahm, Sahn 한국현미경학회 2002 Applied microscopy Vol.32 No.2
복합 페로브스카이트$(Na_{1/2}Pr_{1/2})TiO_3$ (NPT)의 미세구조를 X-ray diffractometry와 투과전자 현미경으로 관찰하였다. NPT는 A-site 양이온에 의한 1 : 1 chemical ordering을 갖고 있지 않으며 산소 팔면체의 antiphase tilting과 inphase tilting 그리고 A-site 양이온의 antiparallel shift가 관찰 되었다. 2차상도 관찰되었으나, 이를 확인하지 못하였다. 측정된 NPT 재료의 유전체 특성은 ${\varepsilon}_r=99.6,\;Q\;{\Large f}_o=1124\;GHz,\;{\tau}_{f}=-233.64ppm/^{\circ}C$이었다. Microstructural investigations of $(Na_{1/2}Pr_{1/2})TiO_3$ (NPT) complex perovskite compounds were carried out using X-ray diffractometry and transmission electron microscopy. NPT had not 1:1 chemical ordering of Asite cations but had the antiphase and inphase tilting of oxygen octahedron and the antiparallel shift of cations. Both the antiphase boundaries and the ferroelastic domains were not present in the microstructure. Unidentified second phase was found in the microstructure. The measured dielectric properties were ${\varepsilon}_r=99.6,\;Q\;{\Large f}_o=1124\;GHz,\;{\tau}_{f}=-233.64ppm/^{\circ}C$.