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

The Korea Association of Crystal Growth (한국결정성장학회)
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Synthesis parameters of hydroxyapatite preparation by a precipitation process

합성조건이 침전법에 의한 Hydroxyapatite 제조에 미치는 영향

  • Moon, Sung Wook (Department of Ocean Advanced Materials Convergence Engineering, Korea Maritime and Ocean University) ;
  • Lee, Byeong Woo (Department of Ocean Advanced Materials Convergence Engineering, Korea Maritime and Ocean University)
  • 문성욱 (한국해양대학교 해양신소재융합공학과) ;
  • 이병우 (한국해양대학교 해양신소재융합공학과)
  • Received : 2022.05.31
  • Accepted : 2022.06.13
  • Published : 2022.06.30
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Abstract

Hydroxyapatite (HAp) was synthesized from calcium hydroxide (Ca(OH)2) reacting with phosphoric acid (H3PO4) in aqueous solution. HAp powders were synthesized from extremely high concentration of precursor solutions over 3 M of Ca(OH)2 aqueous suspension using modified process parameters such as phosphoric acid (H3PO4) pouring rate, aging time and post ball milling process. Regardless of phosphoric acid pouring rate, the DCPD (dicalcium phosphate dihydrate) was formed at room temperature and when heated above 700℃, β-TCP (tricalcium phosphate) was synthesized and the amount reached its maximum at 900℃. When the synthesized powder was sintered at 1150℃, β-TCP, a high temperature impurity phase, remained. The single HAp phase without DCPD was obtained from post ball-milled precipitates followed by 3 day aging. For the ball-milled precipitates even without the aging process, the desired single HAp phase without β-TCP could be obtained by heat treatment above 500℃. The post ball milling process provided a convenient route for HAp synthesis.

수산화칼슘(Ca(OH)2)과 인산(H3PO4) 수용액을 반응시켜 수산화아파타이트(hydroxyapatite, HAp)를 합성하였다. 3 M 이상의 고농도 수산화칼슘원료를 전구체로 사용하고 인산 첨가속도, 반응용액 유지시간, 반응생성물에 대한 볼밀링, 합성 후 열처리 같은 합성조건을 변화시켜 HAp를 합성하였다. 인산 첨가속도에 관계없이 상온에서 합성할 경우 주된 불순물상(phase)인 DCPD(dicalcium phosphate dihydrate)가 형성되었고, 700℃ 이상 가열 시 β-TCP(tricalcium phosphate)가 합성되기 시작해 900℃에서 그 양이 최대가 되었다. 합성된 분말을 1150℃에서 소결 할 경우에도 고온안정 불순물 상인 β-TCP 상은 없어지지 않고 남아있었다. 합성 수용액에 대한 볼밀링 후 3일 간 그 용액을 유지할 경우 DCPD 상이 없는 단일 HAp 상을 얻을 수 있었으며, 유지시간 없이 합성물에 대한 볼밀링 과정만을 거친 경우에도 500℃ 이상 열처리를 통해 β-TCP 상이 없는 단일상의 HAp를 얻을 수 있었다. 이러한 추가적인 볼밀링 과정을 적용함으로써 HAp를 손쉽게 합성할 수 있었다.

Keywords

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