Journal ID : TRKU-11-11-2021-11501
[This article belongs to Volume - 63, Issue - 10]
Total View : 438

Title : Effect of N,N, Dimethyl Formamide (DMF) Volume Fraction and Activation Process on HKUST-1 Synthesis and its Properties

Abstract :

DMF is a common solvent using for HKUST-1 synthesis in solvothermal process. As solvent it is commonly believed that DMF to a certain degree will play role on the quality of final product. This research explores the possibility to enhance HKUST-1 quality by optimizing the usage of DMF during synthesis process. The experiment was performed by preparing solvent that consist of aquadest, ethanol, and DMF. Three samples (A,B, and C) were prepared using DMF that has volume fraction of 0.222; 0.333; and 0.444, respectively. Synthesis was done by heating the autoclave reactor at 100°C for 24 hours. The final products are prussian blue solid material. Sample analysis was performed to examine the properties of the final product. First, SEM analyis was performed and the microstructure of bipyramide crystal was observed. This structure is resembles the HKUST-1. XRD test also confirms that all the samples have peaks at around 6.70°, 9.48°, and 11.62° that is unique for HKUST-1. Additional process, i.e. heating process is done on one of the samples as the representative of the others (sample B) to examine if there is remaining solvent that is trapped. Not all samples are checked for activation process because all samples show similarities during SEM and XRD test. Sample B is then heated at 29°C (B1), 75°C (B2), 115°C (B3), 155° (B4), and 170°C (B5), respectively. The result from SEM and XRD test showed that sample B1, B2, B3, B4, and B5 could endure additional heating process and the remaining solvent that is trapped on the pore is succesfuly removed. Another test is BET adsorption measurement. The measurement concludes that samples A, B, and C are fall within microporous material category because they have pore diameter less than 2 nm and the pore diameter is getting smaller as the DMF volume fraction increases. Specific pore volume and specific surface area calculation also reveal that samples tend to have higher specific pore volume and specific surface area when DMF volume fraction increases. From the result of this experiment it can be concluded that DMF volume fraction has significant impact in controlling the properties of HKUST-1 that is produced during solvothermal synthesis process.

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