Dataset for article Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO₂/N₂, CO₂/CH₄ and O₂/N₂ separation

____________________Dataset for article Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO₂/N₂, CO₂/CH₄ and O₂/N₂ separation____________________

Last updated: 2026-01-12
DOI: 10.5281/zenodo.18196625 

______Contact______
* Karel Friess
* Karel.Friess@vscht.cz
* +420 220 44 4029
* ORCID: 0000-0002-1858-0555
* Dept. of Physical Chemistry. Faculty of Chemical Engineering, University of chemistry and Technology, Prague
* Technicka 5, 166 28, Prague 6, Czech Republic

______Licence______
*Dataset for article “Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO₂/N₂, CO₂/CH₄ and O₂/N₂ separation” 2025 by Jana Florekova, Tomas Pokorny, Saeed Ashtiani, Johannes Carolus Jansen, Alessio Fuoco, Mariagiulia Longo, Josef Schneider, Filip Průša, Karel Friess is licensed under CC BY NC 4.0
*licence information: https://creativecommons.org/licenses/by-nc/4.0/

------------------------------------------------------------------------------------------------

______About the dataset______
Addressing the global challenge of climate change necessitates the development of innovative technologies for efficient gas separation, particularly for CO2 capture. Mixed matrix membranes (MMMs) offer a promising solution by synergically integrating the CO2-selective Pebax®1657 with the intrinsic properties of metal–organic frameworks such as UiO-66. Herein, we focus on synthesizing, fabricating, and characterizing Pebax®1657-based MMMs with 0 (neat polymer), 5, 10, 15, and 20wt% of composite magnetic nanoparticles (MNPs) derived from amine-functionalized UiO-66 and Mn-Fe oxide nanoparticles. An external magnetic field applied during membrane casting enabled the controlled embedding of MNPs. Material properties were analyzed using Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDX), Thermogravimetric Analysis (TGA), Brunauer–Emmett–Teller method (BET), and surface roughness measurements.

______Methods of data collection______
*More detailed description can be found in article: 
Floreková, J.; Pokorný, T.; Ashtiani, S.; Jansen, J. C.; Fuoco, A.; Longo, M.; Schneider, J.; Průša, F.; Friess, K. Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO2/N2, CO2/CH4 and O2/N2 separation. Separation and Purification Technology 2026, 380, 135107. DOI: https://doi.org/10.1016/j.seppur.2025.135107.

*Sample preparation
Samples were prepared in advance before the measurement. The preparation is described for each method in detail in the article:
Floreková, J.; Pokorný, T.; Ashtiani, S.; Jansen, J. C.; Fuoco, A.; Longo, M.; Schneider, J.; Průša, F.; Friess, K. Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO2/N2, CO2/CH4 and O2/N2 separation. Separation and Purification Technology 2026, 380, 135107. DOI: https://doi.org/10.1016/j.seppur.2025.135107.

* Pyris diamond differential scanning calorimeter (DSC):
HW: a Pyris Diamond differential scanning calorimeter (DSC, Perkin Elmer, USA) and equipped with an Intracooler cooling system; samples weighing 10–15 mg were placed in a small aluminum foil pan (<5 mg) and subjected to a heating/cooling/heating cycle in the temperature range from −75 to 220 °C at a rate of 15 °C/min 

* FT-IR spectroscopy: 
HW: a Nicolet iS50 FT-IR spectrometer (Thermo Scientific, Waltham, Massachusetts, USA ); the sample of membrane was attached to the diamond surface and measured in ATR mode with DTGS  detector
acquisition: range 400–4000 cm−1  

* Gas adsorption porosimetry:
HW: an Autosorb iQ3 (Quantachrome Instrument) porosimeter; adsorption and desorption were measured at liquid nitrogen (−195.7 °C); before measurements, UiO-66-NH2 and MNPs samples were degassed at 60 °C for 24 h and magnetic Mn–Fe nanoparticles were degassed at 200 °C for 24 h; by BET analysis specific surface area from isotherms was measured in the relative pressure range 0.05–0.30; the DFT method, with a model N2 at 77 K on carbon, was used to calculate the average pore sizes

*Permeameter:
HW: an Integral constant volume permeameter custom-build and the instrument and experimental procedure description can be found in article: 
P. Otrisal, K. Friess, L. Feherova, Z. Melicharik, L. Svorc, C. Bungau, D.-E. Mosteanu: The heat stress effects on the gases permeability of the isolative type garment of the Czech armed forces chemical corps specialists body surface protection; Rev. Chim. (Bucharest), 70 (5) (2018), pp. 1597-1602.
The total amount of substance penetrated through the membrane from the beginning of the experiment is measured and the pressure change in the evacuated area (permeate area) is monitored.
Experiments were carried out at 25 °C with an inlet pressure of 1 bar using a self-developed fixed-volume pressure increase (time-lag) permeameter. The temperature was controlled by a thermostat (Julabo F250, Germany), and the pressure sensor range (Oerlikon Leybold, Germany) was adjusted according to the membrane permeability (10 Torr). To ensure a vacuum, the measuring cell was connected to a Trivac 4B oil rotary pump from Leybold Vacuum (Germany), equipped with filters to prevent the release of oil vapors from the pump into the apparatus and the environment. The membrane active area was (34 ± 0.05) mm, and the volume at the permeate side of the cell was (50 ± 0.1) cm³.

* Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX):
HW: a SEM (Oxford Instruments, Hitachi S-4800, Japan) with EDX and a 150 mm2 with SDD detector
Prior to morphology testing, the samples were immersed in liquid nitrogen and fragilely fractured to study the cross-section and surface structure. 
Before SEM analysis, the samples were coated with a 2 nm layer of gold nanoparticles to induce conductivity using the LUXOR benchtop sputter coater (Nanoscience, USA). The instrument operated at 15 kV during cross-sectional mapping. 

* Sorption:
Sorption tests were performed gravimetrically using a custom-made apparatus with a McBain quartz spiral balance (sensitivity: 15.253 mg mm−1) placed on an anti-vibration table (Thor Labs) to minimize disturbances. The temperature (25 °C) was controlled using a heating unit (Bravo B 4273) and cooling system (Julabo F250). Experiments were conducted at pressures ranging from 0.1 to 0.5 MPa and 1 MPa, with 30–55 mg samples sealed in glass tubes and evacuated (<10−3 mbar) using a rotary pump (Trivac D4B, Oerlikon Leybold). Spiral elongation was recorded by a CCD (Sony).

* Scanning transmission electron microscopy with energy-dispersive spectroscopy (STEM-EDS):
HW: STEM-EDS was employed for elemental mapping and was performed on a Talos F200 instrument equipped with a X-flash EDS detector (Bruker, Germany).
The device operated at an accelerated potential of 40–200 kV. The sample for STEM-EDS measurement was dispersed by sonification in cyclohexane, and the suspension was applied on Quantifoil R 2/2 300 mesh copper grids. Subsequently, the grid with the sample was cleaned using the H2/O2/Ar plasma generated by a Gatan Solarus II device to reduce organic contamination. 

* Thermogravimetric analysis (TGA):
HW: an STA PT 700 LT device (Linseis, Germany) in the temperature range from 30 to 700 °C
The samples were placed in alumina crucibles, and the measurement was carried out in a nitrogen atmosphere with a flow rate of 20 ml N2/min under the selected temperature regime. 

* X-ray photoelectron spectroscopy (XPS):
HW: a Kratos Supra device equipped with a monochromatic X-ray source with AlK α (E = 1486.6 eV) excitation; C 1 s (284.8 eV) was used for binding energy calibration

* X-ray diffraction (XRD):
HW: a Bruker D8 Discoverer θ-θ diffractometer (Karlsruhe, Germany) with Bragg-Brentano geometry and Cu Kα radiation (λ = 0.15418 nm, U = 40 kV, I = 40 mA)
acquisition: number of scans: 4445; increment: 0.0191241
* XRD analysis of powder: 
HW: a second-generation Bruker D2 Phaser X-ray diffractometer (Bruker, Billerica, MA, USA) equipped with Cu Kα radiation (λ = 0.15418 nm); angular range of 5–90° (2θ)

______Methods of data processing______
The dataset contains raw and processed data. The details regarding the processing are described in article: 
Floreková, J.; Pokorný, T.; Ashtiani, S.; Jansen, J. C.; Fuoco, A.; Longo, M.; Schneider, J.; Průša, F.; Friess, K. Controlled embedding of magnetically oriented Zr-MOF/Mn–Fe oxide nanohybrids in MMMs for enhancement of CO2/N2, CO2/CH4 and O2/N2 separation. Separation and Purification Technology 2026, 380, 135107. DOI: https://doi.org/10.1016/j.seppur.2025.135107.

------------------------------------------------------------------------------------------------

______File name structure_____
* PN_X_YYYYMMDD_S_V
PN – project number (GACR-24-11041S)
X – measurement method (DSC, FTIR, GasAdsorptionPorosimetry, Permeameter, SEM, Sorption, STEM, TGA, XPS, XRD)
YYYYMMDD – date of measurement (YYYY – year; MM – month; DD – date)
S – sample type (Membrane, type of membrane, nanoparticles, …)
V – version (raw/processed)

* Example: GAČR-24-11041S_FTIR_YYYYMMDD_sampleABCD_V-raw.ext

______File formats______
* Pyris diamond differential scanning calorimeter (DSC) - converted to XLSX
         The folder contains raw and processed data.
* FT-IR spectroscopy - original CSV
        The raw data were provided in .csv format and were subsequently processed using OriginPro 2019b (OriginLab Corporation).
* Gas adsorption porosimetry - converted from OPJU to XLSX/ XLSX + processed DOCX
        The folder contains raw and processed data.
*Permeameter - processed XLSX
       The folder contains permeability values calculated by the instrument software according to the equation given in the text. For each sample, the reported value corresponds to the average of three independent measurements (processed in Excel).
* Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) – original picture TIF (SEM) + original description of individual samples HDR (SEM) + original DOCX (EDX)
       The folder contains raw data.

* Sorption - converted from CSV to XLSX / original XLSX
        The folder contains processed data derived from the instrument output.
* Scanning transmission electron microscopy with energy-dispersive spectroscopy (STEM-EDS): original TIF and PNG
       The folder contains the raw data.
* Thermogravimetric analysis (TGA): original XLS and XLSX
       The folder contains the raw and proceseed data.
* X-ray photoelectron spectroscopy (XPS): original XLSX
        The folder contains raw data.
* X-ray diffraction (XRD): original TXT + original after software modification RAW 
        Before the software modifications, the raw data were available in .txt format, whereas after the software modifications they could be obtained only in .raw format.

______Date formats______
* YYYY-MM-DD
* HH-MM-SS 24hr format

______Units and abbreviations______
* All FTIR spectra are in Wavenumber (cm^-1) vs Absorbance (-)
* Data from gas adsorption porosimetry are in Relative presure (-) vs Volume (cm^3 g^-1)
* Data from permeameter are in Permeability (Barrer) vs Selectivity (-)
* Data from sorption are in Pressure (bar) vs Quantity adsorbed (g/g)
* Data from X-ray photoelectron spectroscopy (XPS) are in Binding energy (eV) vs CPS (counts per second)
* Data from X-ray diffraction (XRD) are in 2θ (°) vs Intensity (a.u.)