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Room-Temperature Mechanochemical Synthesis and Consolidation of Nanocrystalline HfB2-HfO2 Composite Powders
N. Akçamlı1,2, D. Ağaoğulları1, Ö. Balcı3, M. L. Öveçoğlu1, İ. Duman1
1 Istanbul Technical University, Faculty of Chemical and Metallurgical Engineering, Department of Metallurgical and Materials Engineering, Particulate Materials Laboratories (PML), 34469 Maslak, Istanbul, Turkey
2 Bursa Technical University, Faculty of Natural Sciences, Architecture and Engineering, Department of Metallurgical and Materials Engineering, Yıldırım 16330, Bursa, Turkey
3 Koç University, Department of Chemistry, Rumelifeneri Yolu, 34450 Sarıyer, Istanbul, Turkey
received November 4, 2017, received in revised form January 7, 2018, accepted February 12, 2018
Vol. 9, No. 2, Pages 101-118 DOI: 10.4416/JCST2017-00084
Abstract
This study reports on the in-situ preparation of HfB2-HfO2 composite powders at room temperature by means of mechanochemical synthesis (MCS) from HfCl4-B2O3-Mg powder blends. The effects of milling duration and excess amounts of B2O3 and Mg reactants (20 and 30 wt%) on the HfB2 formation mechanism were investigated. After MCS and purification, HfB2, HfO2 and Mg2Hf5O12 phases were obtained. The Mg2Hf5O12 phase decomposed during the annealing treatment conducted at 1000 °C under Ar flow. The as-synthesized, purified, annealed and subsequently leached powders were characterized with an X-ray diffractometer (XRD), stereomicroscope (SM), scanning electron microscope (SEM), transmission electron microscope (TEM) and particle size analyzer (PSA). The HfB2-HfO2 composite powders with an average particle size of 140 nm and predominantly rounded morphology were consolidated with cold pressing/pressureless sintering (PS) and spark plasma sintering (SPS) techniques. The relative density values of the HfB2-HfO2 composites obtained by means of PS (with 2 wt% Co) and SPS techniques were 91.82 % and 93.79 %, respectively. A relatively high densification rate for the HfB2-HfO2 ceramic was achieved by means of Co addition, which was considered a promising sintering aid for HfB2-based ceramics. The HfB2-HfO2 composite sample consolidated with SPS exhibited hardness, wear volume loss amount and friction coefficient values of 18.45 GPa, 4.30 mm3 and 0.60, respectively.
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Keywords
HfB2-HfO2 composites, powders, solid state reaction, sintering, microstructure-final, mechanical properties
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