Synthesis of CaB6 powders via mechanochemical reaction of Ca/B2O3 blends

• Published in: Powder technology 2012-07, Vol.225, p.136-142
• Main Authors: BALCI, Ozge, AGAOGULLARI, Duygu, DUMAN, Ismail, ÖVECOGLU, M. Lutfi
• Format: Article
• Language: English
• Subjects: Applied sciences; Atomic absorption analysis; atomic absorption spectrometry; Blends; Boron oxide; Calcium; Calcium hexaboride; Centrifugation, cyclones; Chemical engineering; Crystallization, leaching, miscellaneous separations; Decantation; Diffraction; drying; energy; Exact sciences and technology; Grinding; HCl leaching; High energy ball milling; hydrochloric acid; Liquid-liquid and fluid-solid mechanical separations; Mechanochemical processing; milling; Miscellaneous; mixing; Polymer blends; powders; raw materials; Scanning electron microscopy; Solid-solid systems; Spectroscopy; steel; Synthesis; temperature; washing; X-radiation; X-ray diffraction
• ISSN: 0032-5910; 1873-328X
• DOI: 10.1016/j.powtec.2012.03.051

The synthesis of CaB6 powders by mechanochemical processing was investigated in the present study. The synthesis was carried out using stoichiometric amounts of Ca/B2O3 powder blends as low cost raw materials. Milling was performed at room temperature in a high energy ball-mill using hardened steel vial and balls with a constant ball-to-powder weight ratio (10:1). The effect of milling duration on the production efficiency of CaB6 powders was investigated. Milled powders were leached by different HCl concentrations under the effect of ultrasonic stirring. The final product was obtained after repeated centrifuging, decanting, washing and drying treatments. Phase and microstructural characterization investigations of the milled and leached powders were carried out by X-ray Diffractometry (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) whereas supernatant liquid was characterized by Atomic Absorption Spectrometry (AAS). The best results for the preparation of CaB6 powders were obtained from the 6h milled and repeated leached (2 and 0.5M HCl solution) powders. The synthesis of submicron CaB6 powders by mechanochemical processing was investigated in the present study. The best results for the preparation of CaB6 powders were obtained from the Ca/B2O3 powder blend milled for 6h and repeated leached in 2 and 0.5M HCl solution. [Display omitted] ► A novel-room temperature process was utilized for the production of submicron CaB6. ► CaB6 powders were obtained by mechanochemical processing and subsequent leaching. ► The parameters of milling duration and HCl concentration were investigated. ► The production efficiency of CaB6 powders were evaluated. ► Extension of milling duration and repeating leaching resulted in high efficiency.