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3.4. Cycle experiments in combustion furnaceThe experiments were carried out in the cycling combustion furnace device (Fig. 2) to investigate the properties and mineralogical of the fresh Fe2O3/Al2O3 OC particles and the used Fe2O3/Al2O3 OC particles.The results of XRD analysis of the oxygen carrier after one, five and ten cycles are shown in Fig. 8. There are no significant changes in sample composition after one and five cycles combustion. After ten cycles, some other impurities such as Ca3Al2O6, small amount of Ca–Mg–Al compounds and SiO2 were detected in the XRD patterns. This phenomenon can be explained from that the coal ash reacted with Al2O3 to produce new compounds in teen cycle combustion processed at a high temperature.Diagram fase residu dalam CLC dievaluasi oleh Factsage perangkat lunak, yang berjalan di bawah Microsoft Windows dengan berbagai modul yang dapat melakukan berbagai perhitungan thermochemical dan menghasilkan tabel, grafik dan angka-angka dalam metalurgi kimia dan fisik, kimia dan lingkungan, dll. Berdasarkan komponen residu, data yang dimasukkan ke dalam perangkat lunak Factsage untuk membentuk diagram fase. Gambar 9 menunjukkan fase mungkin terbentuk ketika abu dan berbagai logam oksida dipanaskan hingga 950 C, proporsi yang berbeda CaO – MgO-SiO2-Al2O3 dihasilkan padat mencair pada suhu berbeda. Diagram fase biner CaO-Al2O3 gambar 8 hadiah yang berbeda misalnya rasio molar antara Al2O3 / (CaO + Al2O3) akan menghasilkan Ca3Al2O6 antara suhu dari 300 1500 C, konsisten dengan hasil dari 10# residu pada gambar 7. Selain itu, Ca2Fe2O5 dan Ca3MgSi2O8 telah terdeteksi setelah remaja combustions siklus, yang konsisten dengan diagram fase mineral (gambar 9), dan komponenratio of CaO, Al2O3, SiO2 and MgO changed in combustion processes. With the increasing of cycle numbers, a certain amount of solid solution appeared at different combustion temperature. For example, iron silicon compounds in quaternary phase diagram (Fig. 9), however, there are more active sites such as SiO2, Al2O3, MgO etc in solid melts.These active sites can react with trace heavy metal elements and compounds, which produced crystal and glass depositing on the particle surface of Fe2O3/Al2O3 OC at a high temperatures.Thses actions could cause serious sinter, thus leading to the reactivity deterioration of o Fe2O3/Al2O3 OC [40].Fig. 10 shows the element varieties on the surface of Fe2O3/Al2O3OC by EDX analysis. After one combustion cycle, particle size is relatively uniform and the surface is rough, whose effective reaction area is larger. According to the EDX spectrum analysis, Fe, Al, and Si were the main elements detected in all samples. The main component of fresh particles is Fe2O3 and few Al2O3 without producing obvious agglomeration or melting reaction. After 10 cycles, some large granular polymer appeared in the particle surface, and the particle surface became dense and smooth. Whatever, the EDX results demonstrated the deposition of accumulation on the particle surface of Fe2O3/Al2O3 OC in the CLC processes.Except for the main component Fe and Al, Si, Ca and other components detected obviously, trace elements Ti mainly coming from coal ash is also accumulation increased on the surface of Fe2O3/Al2O3 OC after ten cycles combustions. These produce
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