DOI: 10.17863/cam.116966
title: Research data supporting the publication "Understanding metal-organic framework densification: solvent effects and the growth of colloidal primary nanoparticles in monolithic ZIF-8"

description: Research data supporting a full paper entitled " Understanding metal-organic framework densification: solvent effects and the growth of colloidal primary nanoparticles in monolithic ZIF-8" by A. Pathak, et al. Monolithic metal-organic frameworks (monoMOFs) are prepared. The aim is to create monoZIF-8 under aqueous conditions and samples are prepared using a variety of solvents, with characterization focusing on monoZIF-8 made in 15% v/v EtOH-water. Products are analysed for composition, morphology, mechanical properties and primary nanocrystallite size. The porosity of the samples is also tested. The following supporting data are presented: Powder XRD data: A Panalytical Empyrean diffractometer is used, fitted with an X’celerator detector and with a Cu-Kα1 (λ = 1.540598 Å) source working at 40 kV and 40 mA with a 0.02° step size. Data supplied in Origin files. Elemental Analysis: C, H, N uses an Exeter Analytical Inc. CE-440 Elemental Analyzer, with a combustion temperature of 975 °C. Inductively-coupled plasma-optical emission spectroscopy (ICP-OES) for Zn quantification uses a Thermo Fisher Scientific iCAP7400 Duo ICP-OES spectrometer running Qtegra software. For sample preparation, see paper. Data supplied as pdf and Excel files. FTIR Spectroscopy: Uses a Thermo Scientific Nicolet iS50 spectrometer working in attenuated total reflection mode. Data in Origin. Electron Microscopy: Low magnification scanning electron microscope (SEM) images are obtained using a TESCAN MIRA3 FEG-SEM. Images are processed using AzTec Suite. Samples are mounted on an Al-stub and sputter-coated with chromium. High magnification SEM images and elemntal analysis use a JEOL IT500HR/LA high-resolution SEM operating at 2 kV. TEM images use a Talos F200X G2 and data and are analyzed using FEI TEM Imaging and Analysis. EDS data are processed using Velox. Lower magnification images use a JEOL JEM-2010 TEM at 200 kV with a space resolution of 0.24 nm. Primary nanocrystallite size distributions are calculated in ImageJ. For TEM, carbon-coated Cu grids are used. SEM data as tif and hdr files. EDS supplied as Word and txt files and in tif format. TEM data in emi, ser and tif files with histograms supplied in Origin. Nanoindentation: The specimen surface is flattened by polishing with sandpapers and diamond suspensions. Tests use a KLA iMicro nanoindenter, with a 50 mN force actuator and a Berkovich tip. Continuous Stiffness Measurements (CSM) are performed, allowing measurement of the indentation modulus E* and Hardness H. 2 sets of 16 indents are performed in different areas, with 1000 nm maximum indentation depth. Tests use a constant indentation strain rate of 0.1 s-1. Max load is held for 1 s before unloading to quantify creep. Upon unloading, the load is held again at 10% of max load for 3 min. The CSM values of E* and H are averaged in the interval 500–1000 nm. Data in Origin and Excel formats. Gas adsorption: N2 adsorption isotherms at 77 K use an Anton Paar Nova-800. Activated samples are ex situ degassed at 110 °C, 20 ºC min-1, 6 h. Isotherms are evaluated using Kaomi software. Apparent surface areas are calculated using the BET equation. Micropore volumes and micropore size distributions are obtained using the Dubinin-Radushkevich (DR) and Dubinin-Astakhov (DA) equations, respectively. Mesopore size distributions are obtained using the Barrett-Joyner-Halenda (BJH) model applied to the desorption branch of the corresponding isotherm at down to P/P0=0.2. Total pore volumes are obtained at P/P0=0.95. Data supplied in Origin. Porosimetery: Helium pycnometry measurements (real density measurements) use MicroUltrapycnometer apparatus from Anton-Paar (Quantachrome). Hg porosimetry uses a POREMASTER-60 GT from Anton-Paar (Quantachrome). For Hg porosimetry, samples are located in a glass sample holder of known volume (by calibration-filling with mercury). The cell is evacuated and filled with Hg to give an electrical contact +0.1 psi. At this point, low-pressure intrusion measurement is started (pneumatic pressure of N2). At the end of low-pressure intrusion, the cell is recovered and weighed to calculate mass and volume of mercury. The cell is then submitted to high-pressure intrusion up to ca. 35500 psi. Sample volume at any desired pressure (and density) is calculated by subtracting the intruded volume at any given pressure from the measured volume at fill. Data in Origin format. Dynamic Light Scattering and Zeta potential: Measurements use a Malvern Panalytical Zetasizer Nano ZS with a 633 nm He-Ne Laser. Reaction aliquots are diluted to maintain mean count rates of 300–450 kcps. A DTS1070 folded capillary cell is used to measure zeta potential at 25 °C. Data in csv format. Thermogravimetric Analysis: Uses a Mettler Toledo TGA/DSC 2 STARe system. Samples are heated to 700 °C at 10 °C min–1. Measurements use a constant flow (80 mL min–1) of air (19–22 % O2 in N2, &lt;10 ppm H2O). Data in Origin format. UV-Vis Spectroscopy: Monolith doping with NADH is analyzed using UV-Vis spectroscopy on a Perkin Elmer Lambda 750. Data are analyzed in UV WinLab and Origin 2021b. Activated monolith is exposed to aqueous NADH over 6 h. Data in Origin format.