Combined effect of high-energy ball milling and silica fume addition in BaCO3-Al2O3. Part I: Formation of cementing phases

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2. Materials and methods
2.1 Raw materials and preparation of barium aluminate cements
The starting raw materials Aluminum oxide and barium carbonate used in this study were A.R. Grade, supplied by Loba Chemie Pvt. Ltd (Mumbai, India). Fume silica was procured from Shiva minerals Pvt. Ltd. (Rajgangpur, India). For reference purposes, a commercially available calcium aluminate cement CA-25 C (Almatis, India) was used.
Aluminum oxide and barium carbonate were weighed in a proportion to give Al2O3: BaO weight ratio of 8:2. Mixes of Aluminum oxide and barium carbonate with and without the incorporation of silica fume were prepared in the same manner. Silica fume was additionally introduced in two proportions viz. 5 and 10 weight %. Complete coding of samples prepared is given in Table 1. The mixture containing aluminum oxide and barium carbonate were pulverized in a high-energy planetary ball mill. This planetary ball mill was manufactured by V.B. Ceramics, Chennai, India. It consists of a 250 ml stainless steel cylindrical jar, internally lined with tungsten carbide. The grinding balls made of tungsten carbides having diameter 10 mm were used as a hard grinding medium. Grinding media and the material weight ratio were kept 3:1 and milling speed was set at constant 300 rpm throughout the study. The milling operation was carried out continuously at room temperature for 1, 3, 5 and 10 h. Introduction of silica fume was done only in mixes after they were pulverized for 10 h. They were then thoroughly mixed in an agate mortar pestle for 30 minutes. The ground mixes were analyzed by differential scanning calorimetry (DSC) for determination of their possible reaction temperatures. Model NETZSCH DSC 404F3 was used for this thermal analy...

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