J Dent Hyg Sci.  2022 Sep;22(3):191-198. 10.17135/jdhs.2022.22.3.191.

X-Ray Diffraction Analysis of Various Calcium Silicate-Based Materials

Affiliations
  • 1Department of Pediatric Dentristry & Wonkwang Bone Regeneration Research Institute, College of Dentistry, Wonkwang University, Daejeon 35233, Korea
  • 2Department of Dental Hygiene, Baekseok University, Cheonan 31065, Korea
  • 3Department of Dental Hygiene, Sunmoon University, Asan 31460, Korea

Abstract

Background
The purpose of this study was to evaluate the composition of the crystal phases of various calcium silicate-based materials (CSMs): ProRoot white MTA (mineral trioxide aggregate) (WMTA), Ortho MTA (OM), Endocem MTA (EM), Retro MTA (RM), Endocem Zr (EN-Z), BiodentineTM (BD), EZ-sealTM (EZ), and OrthoMTA III (OM3).
Methods
In a sample holder, 5 g of the powder sample was placed and the top surface of the material was packed flat using a sterilized glass slide. The prepared slides were mounted on an X-ray diffraction (XRD) instrument (D8 Advance; Bruker AXS GmbH, Germany). The X-ray beam 2θ angle range was set at 10∼90° and scanned at 1.2° per minute. The Cu X-ray source set to operate at 40 kV and 40 mA in the continuous mode. The peaks in the diffraction pattern of each sample were analyzed using the software Diffrac (version 2.1). Then, the peaks were compared and matched with those of standard materials in the corresponding Powder Diffraction File (PDF-2, JCPDS International Center for Diffraction Data). A powder samples of the materials were analyzed using XRD and the peaks in diffraction pattern were compared to the Powder Diffraction File data.
Results
Eight CSMs showed a similar diffraction pattern because their main component was calcium silicate. Eight CSMs showed similar diffraction peaks because calcium silicate was their main component. Two components were observed to have been added as radiopacifiers: bismuth oxide was detected in WMTA, OM, and EM while zirconium oxide was detected in RM, EN-Z, BD, EZ, and OM3. Unusual patterns were detected for the new material, OM3, which had strong peaks at low angles.
Conclusion
It was caused by the presence of Brushite, which is believed to have resulted in crystal growth in a particular direction for a specific purpose.

Keyword

Calcium silicate; Mineral trioxide aggregate; Root canal filling materials; X-ray diffraction analysis
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