Malaysian Journal of Analytical Sciences Vol 21 No 1 (2017): 136 - 148

DOI: http://dx.doi.org/10.17576/mjas-2017-2101-16

 

 

 

SYNTHESIS AND CHARACTERIZATION OF HYDROXYAPATITE NANOPARTICLE

 

(Sintesis dan Pencirian Nanozarah Hidrosiapatit)

 

Sahlil Miraz Mohamed Rafie* and Darman Nordin

 

Department of Chemical and Process Engineering,

Faculty of Engineering and Built Environment,

Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

 

*Corresponding author: sahlilmiraz.rafie@gmail.com

 

 

Received: 21 October 2015; Accepted: 14 June 2016

 

 

Abstract

In this research, hydroxyapatite (HA) nano-size powder was synthesized using wet chemical precipitation technique under atmospheric pressure where calcium hydroxide (Ca(OH)₂) and ortho-phosphoric acid (H₃PO₄) were used as precursors. Distilled water was used as a diluting media for the reaction and sodium hydroxide (NaOH) was used to control the initial pH. The initial pH values, reaction temperature and calcined temperature play an important role in the morphology on HA as well as the phase formation and degree of crystallinity. Nano HA powder has been studied at different initial pH value which is between 9.00 to 11.00, reaction temperature from 80 °C to 100 °C and calcined temperature at 700 °C to 800 °C. The optimum initial pH value was found at pH 10.00, reaction temperature at 100 °C and calcined temperature was at 800 °C. The crystallographic properties were evaluated by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) and Field Emission Scanning Microscope (FESEM). The Design Expert version 9.0.2 with statistical and graphical analysis of the result, by using analysis of variance (ANOVA) was applied to optimize variable in the process of synthesis of HA. Based on analysis of variance (ANOVA) that has been perform, calcined temperature was to be influential variables on mass of HA with value of probability less than 0.05.

 

Keywords:  hydroxyapatite, chemical precipitation, crystallinity, morphology, optimization

 

Abstrak

Dalam kajian ini, nanozarah hidroksiapatit (HA) dihasilkan melalui kaedah pemendakan di bawah tekanan atmosfera di mana kalsium hidroksida (Ca(OH)₂) dan asid orto fosforik (H₃PO₄) merupakan larutan asas bagi penyediaan HA. Air suling digunakan sebagai agen pelarut dalam menyediakan larutan asas bagi proses pemendakan ini. Larutan natrium hidroksida di gunakan bagi mengawal nilai pH. Nilai pH, suhu tindak balas dan suhu relau merupakan faktor penting dalam pencirian dan penghabluran nanozarah HA. Nanozarah HA disediakan pada nilai pH antara 9.00 hingga 11.00, suhu tindak balas 80 °C hingga 100 °C dan suhu relau pada 700 °C hingga 800 °C. Pencirian nanozarah HA di uji menggunakan X-ray Difractometer (XRD), Inframerah Transformasi Fourier (FTIR), dan Mikroskop Pengimbas Pancaran Medan (FESEM). Perisian Design-Expert 9.0.2 digunakan untuk menganalisis data dan pengoptimuman penghasilan mendakan HA.  Berdasarkan analisis varian (ANOVA) yang dilakukan, suhu relau merupakan pemboleh ubah yang mempengaruhi berat HA dengan nilai kemungkinan kurang dari 0.05.

 

Kata kunci:  hikdroksiapatit, mendakan bahan kimia, penghabluran, pencirian, pengoptimuman

 

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