Journal of the Korean Crystal Growth and Crystal Technology (한국결정성장학회지)

The Korea Association of Crystal Growth (한국결정성장학회)
권호 표지

Synthesis and characterization of perovskite nano-sized (Pb, La)$TiO_3$ powder using mechano chemical process

기계화학공정을 이용한 Perovskite 구조의 (Pb, La)$TiO_3$ 나노 분말 합성 및 특성

  • Lim, Bo-Ra-Mi (Functional Nano-Materials Research Lab., Hanyang University) ;
  • Yang, Jae-Kyo (Functional Nano-Materials Research Lab., Hanyang University) ;
  • Lee, Dong-Suk (R&D Center, Innochips Technology) ;
  • Noh, Tae-Hyung (R&D Center, Innochips Technology) ;
  • Seo, Jung-Hye (Dept. of Information Communication Eng, Hanbat National University) ;
  • Lee, Youn-Seoung (Dept. of Information Communication Eng, Hanbat National University) ;
  • Kim, Hee-Taik (Functional Nano-Materials Research Lab., Hanyang University) ;
  • Choa, Yong-Ho (Functional Nano-Materials Research Lab., Hanyang University)
  • 임보라미 (한양대학교 기능성 나노재료 연구실) ;
  • 양재교 (한양대학교 기능성 나노재료 연구실) ;
  • 이동석 ((주) 이노칩 테크놀로지 부설연구소) ;
  • 노태형 ((주) 이노칩 테크놀로지 부설연구소) ;
  • 서정혜 (한밭대학교 정보통신학) ;
  • 이연승 (한밭대학교 정보통신학) ;
  • 김희택 (한양대학교 기능성 나노재료 연구실) ;
  • 좌용호 (한양대학교 기능성 나노재료 연구실)
  • Published : 2008.10.31
Download PDF
⟨ Previous Next ⟩

Abstract

Mechano Chemical Process (MCP) skips the calcinations steps at an intermediate temperature that is always required in the conventional solid-state reaction because forming phase from raw powder is activated by mechanical energy. In this study, we prepared (Pb, La)$TiO_3$ nanopowder with perovskite structure by only high energy MCP. Especially, the PLT nanopowder was synthesized without any thermal treatment using oxides, not salts as raw powder. This process is also very simple due to dry milling method, unnecessary to dry of powder. The oxide powder was milled up to 12 hr at intervals of an hour using MCP and the pure PLT phase of perovskite structure was formed after milling time of 3 hr. And the average particle size was 20 nm with narrow distribution after milling time of 3 hr from raw powder of several $\mu m$ with inhomogeneous distribution.

기계화학공정(MCP; Mechano Chemical Process)은 원료 분말이 기계적인 에너지로 인해 상 형성이 활성화되기 때문에 기존의 볼밀링을 이용한 고상반응에서 필수적인 높은 온도에서의 하소 공정이 필요하지 않다. 본 연구에서는 고 에너지 MCP 방법을 이용하여 perovskite 구조를 가지는 PLT 나노 분말을 제조하였다. 특히, 일반적으로 출발물질로 염을 이용하는 것과 달리 산화물을 원료 분말로 사용하여 어떠한 열처리 공정 없이 PLT 나노 분말을 합성하였다. 또한 건식으로 밀링을 하여 분말 건조 공정이 필요 없어서 공정이 간단하다. MCP 밀링은 시간 별로 12시간까지 진행하였으며, 제조된 분말의 상 분석과 결정면 분석 결과 3시간 이후에는 perovskite 구조의 순수한 PLT 상을 형성하였다. 또한 마이크로 크기의 원료 분말이 밀링 3시간이 지나자 약 20 nm 크기의 균일한 나노 입자가 생성되었다.

Keywords

References

  1. T.-Y. Kim and H.M. Jang, "B-site vacancy as the origin of spontaneous normal-to-relaxor ferroelectric transitions in La-modified $PbTiO_3$", Applied Physics Letters 77 (2000) 3824 https://doi.org/10.1063/1.1330218
  2. R. Tickoo, R.P. Tandon, N.C. Mehra and P.N. Kotru, "Dielectric and ferroelectric properties of lanthanum modified lead titanate ceramics", Materials Science and Engineering B94 (2002) 2
  3. J. Chen, X. Xing, R. Yu, J. Deng and G. Liu, "Microstructural characterization of sol-gel derived $Pb_{1−x}La_xTiO_3$ ferroelectrics", Journal of Alloys and Compounds 388 (2005) 309
  4. L. Seveyrat, M. Lemercier, B. Guiffard, L. Lebrun and D. Guyomar, "Temperature dependence of macroscopic and microscopic PZT properties studied by thermomechanical analysis, dielectric measurements and X-ray diffraction", Ceramics International In press
  5. X. Junmin, J. Wang and T. Weiseng, "Synthesis of lead zirconate titanate from an amorphous precursor by mechanical activation", Journal of Alloys and Compounds 308 (2000) 139 https://doi.org/10.1016/S0925-8388(00)00917-8
  6. L.B. Kong, J. Ma, T.S. Zhang, W. Zhu and O.K. Tan, "$Pb(Zr_xTi_{1−x})O_3$ceramics via reactive sintering of partially reacted mixture produced by a high-energy ball milling process", Journal of Materials Research 16 (2001) 1636 https://doi.org/10.1557/JMR.2001.0227
  7. S. Singh, O.P. Thakur, C. Prakash and K.K. Raina, "Improved piezoelectric properties via mechano-chemical activation in modified PCT ceramics", Materials Chemistry and Physics 94 (2005) 8
  8. S.H. Ng, J.M. Xue and J. Wang, "High temperature piezoelectric strontium bismuth titanate from mechanical activation of mixed oxides", Materials Chemistry and Physics 75 (2002) 131 https://doi.org/10.1016/S0254-0584(02)00066-4
  9. L.B. Kong, T.S. Zhang, J. Ma and F. Boey, "Progress in synthesis of ferroelectric ceramic materials via highenergy mechanochemical technique", Progress in Materials Science 53 (2008) 217
  10. B.D. Cullity, "Elements of X-ray diffraction", 2nd edition (Addison-Wesley, Cananda 1978)