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

The Korea Association of Crystal Growth (한국결정성장학회)
권호 표지

Low temperature synthesis of ZnO nanopowders by the polymerized complex method

착체중합법을 이용한 ZnO 나노분말의 저온합성

  • 권용재 (한양대학교 나노공학과 CPRC) ;
  • 김경훈 (한양대학교 세라믹공학과 CPRC) ;
  • 임창성 (한서대학교 재료공학과 CPRC) ;
  • 심광보 (한양대학교 나노공학과 CPRC)
  • Published : 2002.10.01
Download PDF
⟨ Previous Next ⟩

Abstract

Nano-sized ZnO particles were successfully synthesized at low temperatures by a polymerized complex method via an organochemical route. The polymeric precursors could be prepared using Zn nitrate hexahydrate and a mixed solution of citric acid and ethylene glycol as a chelating agent and a reaction medium. The polymeric precursors were calcined at temperatures from 300 to $700^{\circ}C$ for 3 h, and evaluated for degree of crystallization process, thermal decomposition, surface morphology and crystallite size. The thermal decomposition and crystallization process were analyzed by TG-DTA, FI-IR and XRD. The morphology and crystallite size of the calcined particles were evaluated by scanning electron microscopy (SEM), transmittance electron microscopy (TEM) and Scherrer's equation. Crystallization of the ZnO particles was detected at $300^{\circ}C$ and entirely completed above $400^{\circ}C$. Particles calcined between 400 and $700^{\circ}C$ showed a uniform size distribution with a round shape. The average particle sizes calcined at $400^{\circ}C$ for 3 hour were 30~40nm showing an ordinary tendency to increase with the temperatures.

유기화학적 방법인 착체중합법을 이용하여 나노사이즈의 ZnO 분말을 저온에서 합성하였다. 고분자 전구체는 Zn nitrate hexahydrate를 사용하였고, chelating agent로서 citric acid를 reaction medium으로서 ethylene glycol을 혼합하여 제조하였다. 고분자 전구체를 300~$700^{\circ}C$의 온도범위에서 3시간 동안 하소하였으며, 열분해와 결정화 과정을 TG-DTA, FI-IR과 XRD 등을 이용하여 분석하였다. 결정화 온도에 따른 입자의 형상이나 크기를 SEM, TEM의 분석 및 Scherrer's equation을 이용한 계산을 통하여 관찰 및 비교를 하였다. ZnO의 결정화는 $300^{\circ}C$부터 시작되었고, $400^{\circ}C$에서 완전히 합성되었음을 알 수 있었다. 400~$700^{\circ}C$에서 하소된 ZnO 입자들은 대부분 둥근 형태로 균일하게 분포되었으며, $400^{\circ}C$에서 하소된 분말의 평균입도는 약 30~40nm를 보였다. 일반적으로 온도의 상승에 따라 입경이 증가되는 일반적인 경향이 관찰되었다.

Keywords

References

  1. A. van Dijken, E.A. Meulenkamp, D. Vanmaekelbergh and A. Meijerink, 'Identification of the Transition Responsible for the Visible Emission in ZnO using Quantum Size Effects', J. Luminescence90 (2000) 123
  2. A. Salvador, M.C. Pascual-Marti, J.R. Adell, A. Requeni and J.G. March, 'Analytical Methodologies for Atomic Spectrometric Determination of Metallic Oxides in UV Sunscreen Creams', J. Pharmaceutical and Biomedical Analysis 22 (2002) 301
  3. Ruixing Li, Shinryo Yabe, Mica Yamashita, Shigeyosi Mornose, Sakae Yoshida, Shu Yin and Tsugio Sato, 'Uv-shielding Properties of Zinc Oxide-doped Ceria Fine Powders Derived Via Soft Solution Chemical Routes', Mat. Chem. Phys. 75 (2002) 39.
  4. B.-C. Kim, J.-B. Paik, Y.-S. Han, N.-Y. Lee and B.-K. Lee, 'Synthesis of ZnO : Zn Phosphors with Reducing Atmosphere and Their Luminescence Properties', J. Kor. Ceram. Soc. 37(1) (2000) 1
  5. Takuya Tsuzuki and Paul G. McCormick, 'ZnO Nano-particles Synthesized by Mechanochemical Processing', Scripta Mater. 44 (2001) 1731
  6. Z. Wang and H.J. Li, 'Highly Ordered Zinc Oxide Nanotubules Synthesized Within the Anodic Aluminum Oxide Template', Appl. Phys. A 74 (2002) 201
  7. M. Shiojiri and C. Kaito, 'Structure and Growth of ZnO Smoke Particles Prepared by Gas Evaporation Technic', J. Crystal Growth 52 (1985) 173
  8. Maggio P. Pechini, 'Method of Preparing Lead and Alkaline Earth Titanates and Coating Method Using the Same to form a Capacitor', United States Patent Office, 3,33,697, Patented July 11 (1967)
  9. Bonamali Pal and Maheshwar Sharon, 'Enhanced Photocatalytic Activity of Highly Porous ZnO Thin Films Prepared by Sol-gel Process', Mat. Chem, Phys. 76 (2002) 82
  10. S.W Yun, Y. Shin and S.G. Cho, 'Sintering Behavior and Electrical Characteristics of ZnO Varistors Prepared by Pechini Process', J. Kor. Ceram. Soc. 35(5) (1998) 498
  11. S.-J. Jun, S. Kim and J.-H. Han, 'Synthesis of Stoichio-metric Hydroxyapatite Powder by $CO_{3}^{2-}$ Substitution During Precipitation', J. Kor. Ceram. Soc. 35(3) (1998) 209
  12. A. Cuneyt Tas, Peter J. Majewski and Fritz Aldinger, 'Chemical Preparation of Pure and Strontium- and/ or Magnesium-doped Lanthanum Gallate Powders', J. Am. Ceram. Soc. 83(12) (2000) 2954
  13. J.H. Ryu, C.S. Lim and K.H. Auh, 'Synthesis of $ZnWO_{4}$ Nauopowders by Polymerized Complex Method', J. Kor. Ceram. Soc. 39(3) (2002) 321
  14. D. Mondelaers, G. Vanhoyland, H. Van den Rul, J. D'Hean, M.K. Van Bael, J. Mullens and L.C. Van Poucke, 'Synthesis of ZnO Nanopowder Via an Aqueous Acetate-citrate Gelation Method', Materials Research Bulletin 1974 (2002) 1
  15. H.-C. Kao and W.-C. Wei, 'Kinetics and Microstructual Evolution of Heterogeneous Transformation of ${\theta}$-Alumina to ${\alpha}$-Alumina', J. Am. Ceram. Soc. 83(2) (2000) 362