scholarly journals In Situ MOF-Templating of Rh Nanocatalysts under Reducing Conditions

2020 ◽  
Vol 73 (12) ◽  
pp. 1271
Author(s):  
Renata Lippi ◽  
Campbell J. Coghlan ◽  
Shaun C. Howard ◽  
Christopher D. Easton ◽  
Qinfen Gu ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Main Product ◽  
Metal Organic Frameworks ◽  
Co2 Hydrogenation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reducing Atmosphere ◽  
Reducing Conditions ◽  
Metal Organic

Manganese-based metal–organic frameworks (MOFs) metalated with Rh were used as pre-catalysts for CO2 hydrogenation. Activated insitu (80% H2, 20% CO2, 350°C), the resulting templated catalysts displayed CO2 conversion of up to 20%, with CH4 as the main product. Used catalysts were compared with samples templated in 5% H2/Ar at 350°C using powder X-ray diffraction, electron microscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. It was found that under reducing atmosphere Rh0 nanoparticles formed and organic MOF components decomposed, which allowed growth of MnO or MnCO3 and the formation of a mesh of catalytic Rh0 nanoparticles.

scholarly journals In situ X‐ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)‐based Metal‐Organic Frameworks with UiO‐66 and MIL‐140 architectures

2021 ◽  
Author(s):  
Stephen J. I. Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Building Blocks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

Activation of Peroxymonosulfate by CuNi@C Derived from Metal–Organic Frameworks Precursor

2018 ◽  
Vol 71 (11) ◽  
pp. 874 ◽  
Author(s):  
Xue Huang ◽  
Jing Zhang ◽  
Xiao Zhang ◽  
Qing-Ping Wu ◽  
Chun-Hui Yan
Keyword(s):  
Photoelectron Spectroscopy ◽  
Metallic Copper ◽  
Metal Organic Frameworks ◽  
Aqueous Media ◽  
Oxidative Degradation ◽  
Acid Orange 7 ◽  
X Ray Diffraction ◽  
X Ray ◽  
Initial Ph ◽  
Metal Organic

Calcined Cu-based metal–organic frameworks impregnated with nickel nitrate catalysts (CuNi@C) were synthesised. X-Ray diffraction, scanning electronic microscopy, energy dispersive X-ray spectrometry, and X-ray photoelectron spectroscopy techniques were applied for the characterisation of the synthesised catalyst, which revealed an octahedral particle shape, rough surface, and metallic copper (Cu, CuO) and nickel (Ni, NiO) particles. CuNi@C was fabricated as a novel peroxymonosulfate (PMS) activator for the oxidative degradation of Acid Orange 7 (AO7) in aqueous media. Results showed that the CuNi@C/PMS system can efficiently degrade nearly 100 % of 0.02 mmol L−1 AO7 within 60 min. In addition, the trapping experiments confirmed the participation of sulfate radicals (SO4•−) and hydroxyl radicals (HO•) as reactive species in the system. Furthermore, the effects of parameters including catalyst and PMS dosages, initial concentration of AO7, and pH were studied. Results showed that the decolourisation efficiency increased with the increase of catalyst dosage, but decreased with the increase of AO7 concentration. The optimal PMS concentration was 0.675 mmol L−1, and initial pH showed no significant effect on the degradation of AO7. Moreover, the CuNi@C could be reused four times with good activity and reusability. Findings revealed that the CuNi@C/PMS system shows potential for degrading contaminants in the environment, due to its catalytic activity and non-negligible adsorption.

In situ identification and absolute separation of small molecules by single crystal X-ray diffraction in metal–organic frameworks

CrystEngComm ◽  
2016 ◽  
Vol 18 (29) ◽  
pp. 5429-5433 ◽  
Author(s):  
Heng Ya Gao ◽  
Le Zhang ◽  
Chang Sheng Yan ◽  
Li Na Meng ◽  
Jian Qiang Li ◽  
...  
Keyword(s):  
Single Crystal ◽  
Small Molecules ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Building Blocks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

Facile Preparation of In-Situ S-Doped Flake Carbon Materials from Metal-Organic Frameworks and Its Application in Electrochemical Detection of Hg (II)

NANO ◽  
2020 ◽  
Vol 15 (10) ◽  
pp. 2050133
Author(s):  
Shenghai Zhou ◽  
Hongbo Xu ◽  
Jing Gao
Keyword(s):  
Electron Microscope ◽  
Photoelectron Spectroscopy ◽  
Electrode Materials ◽  
Carbon Materials ◽  
Metal Organic Frameworks ◽  
Calibration Plot ◽  
Active Electrode ◽  
X Ray ◽  
Metal Organic

S-doped carbon materials have recently attracted much attention as electrode materials for electrocatalysis and sensors applications. Herein, we report a facile route for the preparation in situ of flake S-doped carbon nanomaterial by using plate-like sulfur-containing metal-organic frameworks (MOFs) as a pyrolytic precursor without additional carbon and sulfur sources. The resultant MOFs-derived carbon (denoted as PSMC) was further characterized and analyzed by scanning electron microscope, transmission electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy and Raman spectroscopy. Then a highly sensitive electrochemical sensor for selective determination of Hg (II) was achieved by designing PSMC as the active electrode material. The sensitivity of Hg (II) at the sensor is 2.12[Formula: see text][Formula: see text]A[Formula: see text]ppb[Formula: see text][Formula: see text]cm[Formula: see text] according to the slope of the calibration plot and electrode area. Finally, the PSMC-based sensor was proved feasible in river water sample analyses. This work may also provide a valuable clue for the preparation of flake S-doped carbon sensing material as a new application of MOFs-based materials.¡abs¿

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2021 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic ◽  
Two Phases

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as reagents, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

Synthesis, crystal structure, luminescence, and photocatalytic properties of a 2D Cu(II) metal-organic frameworks based on 3,5-di(1H-benzimidazol-1-yl)pyridine and 4,4′-oxybis(benzoate) ligands

2020 ◽  
Vol 75 (8) ◽  
pp. 727-732
Author(s):  
Chen Zhang ◽  
Jian-Qing Tao
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Uv Light ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Uv Light Irradiation ◽  
Photocatalytic Activities ◽  
Metal Organic

AbstractA new Cu(II) metal-organic framework, [Cu(L)(OBA)·H2O]n (1) [H2OBA = 4,4′-oxybis(benzoic acid), L = 3,5-di(1H-benzimidazol-1-yl)pyridine] was hydrothermally synthesized and characterized through IR spectroscopy, elemental and thermal analysis and single-crystal X-ray diffraction. Complex 1 is a four-connected uni-nodal 2D net with a (44·62) topology which shows an emission centered at λ ∼393 nm upon excitation at λ = 245 nm. Moreover, complex 1 possesses high photocatalytic activities for the decomposition of Rhodamine B (RhB) under UV light irradiation.

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