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000878641 1001_ $$00000-0001-9504-8514$$aKrause, Simon$$b0$$eCorresponding author
000878641 245__ $$aThe impact of crystal size and temperature on the adsorption-induced flexibility of the Zr-based metal-organic framework DUT-98
000878641 260__ $$aFrankfurt, M.$$bBeilstein-Institut zur Förderung der Chemischen Wissenschaften$$c2019
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000878641 520__ $$aIn this contribution we analyse the influence of adsorption cycling, crystal size, and temperature on the switching behaviour of the flexible Zr-based metal-organic framework DUT-98. We observe a shift in the gate opening pressure upon cycling of adsorption experiments of micro meter-sized crystals and assign this to a fragmentation of the crystals. In a series of modulated syntheses we downsize the average crystal size of DUT-98 crystals from 120 µm to 50 nm and characterize the obtained solids by X-ray diffraction, infrared spectroscopy, as well as scanning and transmission electron microscopy. We analyse the adsorption behaviour by nitrogen and water adsorption at 77 K and 298 K, respectively and show that adsorption-induced flexibility is only observed for micro meter-sized crystals. Nanometer-sized crystals were found to exhibit reversible type I adsorption behaviour upon adsorption of nitrogen and exhibit a crystal-size dependent steep water uptake of up to 20 mmol g -1 at 0.5  p / p 0 with potential for water harvesting and heat pump applications. We furthermore investigate the temperature-induced structural transition by in situ PXRD. At temperatures beyond 110 °C the open pore state of nano meter-sized DUT-98 crystals are found to irreversibly transform in a closed pore state. The connection of crystal fragmentation upon adsorption cycling and the crystal size-dependence of the adsorption-induced flexibility is an important finding for evaluation of these materials in future adsorption-based applications. This work thus extends the limited amount of studies on crystal size effects in flexible MOFs and hopefully motivates further investigations into this field.
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000878641 7001_ $$00000-0002-9851-5031$$aBon, Volodymyr$$b1
000878641 7001_ $$0P:(DE-Juel1)145710$$aDu, Hongchu$$b2
000878641 7001_ $$0P:(DE-Juel1)144121$$aDunin-Borkowski, Rafal E$$b3
000878641 7001_ $$0P:(DE-HGF)0$$aStoeck, Ulrich$$b4
000878641 7001_ $$00000-0001-7052-1029$$aSenkovska, Irena$$b5
000878641 7001_ $$0P:(DE-HGF)0$$aKaskel, Stefan$$b6$$eCorresponding author
000878641 773__ $$0PERI:(DE-600)2583584-1$$a10.3762/bxiv.2019.52.v1$$p1737-1744$$tBeilstein journal of nanotechnology$$v10$$x2190-4286$$y2019
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