Microwave and Microwave Assisted Solvothermal Synthesis of Vanadium (V)-Benzene-1,3,5-Trycarboxylate Coordination Compound: Effect Microwave on Structural and Microstructural Evolution

Nur Aini, M.Si, Khoirur Reza, Muhammad Hasib Nurulloh, Rachmawati Ningsih

Abstract


V-BTC compounds were successfully synthesis using conventional solvothermal, direct microwave synthesis and microwave assisted solvothermal synthesis. The effect of microwave power on structure, morphology and crystallinity was investigated. The P-XRD revealed the direct microwave synthesis at 300W and 450W power resulting dominantly amorf structure, while the conventional solvothermal at 160oC/48h and microwave assisted solvothermal produced the crystalline peak of XRD pattern. Proven by le-bail refinement methods, the crystal structures show agreement with polyoxovanate coordination structure of [(C2H8N)12[(V5O9Cl)6(C9H3O6)8] which crystallized in Fm3 ̅m cubic crystal. SEM analysis revealed the differences in crystallinity and morphological evolution with increasing the microwave power. V-BTC solvothermal shows granular morphology with irregular shape, rough surface, porous and agglomerate particles, while microwave integration approach resulting more compact particles, higher crystallinity, and the growth of elongated plat-like morphology at 450W. Microwave-assisted synthesis produced smaller particles and narrowed the particle-size distribution compared with conventional solvothermal synthesis, demonstrating that microwave irradiation can influence the nucleation and crystal growth process of V-BTC compounds

Keywords


V-BTC, V-MOF, Microwave-Solvothermal Synthesis

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References


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DOI: https://doi.org/10.18860/al.v14i2.45653

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