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

The Korea Association of Crystal Growth (한국결정성장학회)
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Preparation and characterization of CoAl2O4 blue ceramic nano pigments by attrition milling

어트리션밀을 이용한 CoAl2O4 나노 무기 안료의 제조 및 특성 평가

  • Lee, Ki-Chan (Icheon Branch, Korea Institute of Ceramic Engineering and Technology) ;
  • Yoon, Jong-Won (Department of Advanced Materials Science and Engineering, Dankook University) ;
  • Kim, Jin-Ho (Icheon Branch, Korea Institute of Ceramic Engineering and Technology) ;
  • Hwang, Kwang-Taek (Icheon Branch, Korea Institute of Ceramic Engineering and Technology) ;
  • Han, Kyu-Sung (Icheon Branch, Korea Institute of Ceramic Engineering and Technology)
  • 이기찬 (한국세라믹기술원 이천분원) ;
  • 윤종원 (단국대학교 신소재공학과) ;
  • 김진호 (한국세라믹기술원 이천분원) ;
  • 황광택 (한국세라믹기술원 이천분원) ;
  • 한규성 (한국세라믹기술원 이천분원)
  • Received : 2013.08.26
  • Accepted : 2013.09.23
  • Published : 2013.10.31
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Abstract

Cobalt aluminate ($CoAl_2O_4$) is a highly stable pigment with excellent resistance to light, weather, etc., which has resulted in widespread use as a ceramic pigment. Due to the unique optical characteristics, $CoAl_2O_4$ is generally used as a coloring agent to decorate porcelain products, glass, paints and plastics. Here, $CoAl_2O_4$ pigments were synthesized by polymerized complex method and solid state reaction. Then $CoAl_2O_4$ pigment were grinded using the attrition milling with 1 mm size zirconia ball for 3 hours. The attrition milling process was performed at the constant speed of 800 rpm and ball to powder weight ratio (BPR) was 100 : 1. The characteristics of synthesized pigment were analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), particle size analyser (PSA) and CIE $L^*a^*b^*$. The XRD patterns of $CoAl_2O_4$ show single phase spinel structure. The particle size of $CoAl_2O_4$ measured by FE-SEM, TEM and PSA analysis was in the range of 100~200 nm. The blue color of obtained $CoAl_2O_4$ pigments could be confirmed through CIE $L^*a^*b^*$ measurement.

$CoAl_2O_4$는 열적 및 화학적으로 매우 안정한 물질이며 독특한 광학적 특성으로 인해 도자기 제품, 유리, 페인트, 플라스틱을 장식하는 세라믹 착색제로 사용되어져 왔다. 본 연구에서는 착체중합법(Polymerized complex method)과 고상합성법(Solid state reaction)을 이용하여 단상의 $CoAl_2O_4$ 청색 무기 안료를 합성하였고, 잉크젯 프린팅용 잉크로의 응용 시 노즐 막힘 및 분산안정성과 같은 문제점을 방지하기 위해 고에너지 밀링 공정 중 하나인 어트리션밀을 이용하여 입자를 미세화하였다. 밀링 공정은 직경 1 mm의 지르코니아 볼을 이용하여 BPR(Ball to powder weight ratio) 100 : 1, 800 rpm의 조건에서 3시간 동안 진행되었다. 합성된 안료는 XRD, FE-SEM, TEM, PSA, 그리고 CIE $L^*a^*b^*$ 측정을 통하여 어트리션밀링 전후의 특성을 분석하였다. XRD 측정 결과 단상의 $CoAl_2O_4$ 청색 무기 안료가 합성되었고, 고에너지 밀링 공정을 통하여 100~200 nm의 입자 크기를 가지는 청색 나노 무기 안료를 얻었다.

Keywords

References

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