Use of open source monitoring hardware to improve the production of MOFs: using STA-16(Ni) as a case study

Massingberd‐Mundy, Felicity; Poulston, Stephen; Bennett, Stephen C.; Yeung, Hamish H.‐M.; Johnson, Timothy J.

doi:10.1038/s41598-020-73780-z

Cited by 6 publications

(3 citation statements)

References 30 publications

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“…Since it is not carbonized or crystallized, the peaks located at 6.8 and 24° are assigned to the framework and rGO, respectively. It is in agreement with the results reflected in the materials reported in refs and . The D (defect) band and G (graphic) band can be observed in Figure b, which are located at 1350 and 1580 cm –1 , respectively.…”

Section: Resultssupporting

confidence: 92%

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Liu

et al. 2023

ACS Appl. Nano Mater.

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The faradaic process of transition-metal-based oxides or/and hydroxides is widely utilized to increase the capacity of electrochemical energy storage significantly. However, poor electrical conductivity and low stability of these materials are two crucial factors hindering the maximization of their potential application. To address this issue, carbon–transition-metal oxide composites are strategized to combine the high electrical conductivity of carbon materials and the capacity of transition metals. Here, inspired by the self-assembly process of metal–organic frameworks, a hollow carbon nanosphere (HCNS)@Ni precursor/rGO is synthesized by a one-pot hydrothermal method. HCNS@Ni nanoparticles/rGO (HCNS@Ni NP/rGO) is derived in subsequent calcination. The synthesized HCNS@Ni NP/rGO was assembled as an electrode and evaluated with outstanding electrochemical properties and performances. A high specific capacity of 1589 F g–1 at a current density of 0.3 A g–1 and even 733.33 F g–1 at 50 A g–1 are obtained, with 46.2% of capacity remaining. After 1600 charge–discharge cycles at 10 A g–1, the assembled electrode exhibits the desirable capacity retention of 77.9%.

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Section: Resultssupporting

confidence: 92%

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Liu

et al. 2023

ACS Appl. Nano Mater.

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“…The luminance values within the color-corrected images evolve during the reaction, which we propose serves as a photometric measure of the solution turbidity. This reflects the TiO 2 product concentration, increasing as TiO 2 particles form, then decreasing as the TiO 2 colloid destabilizes and sediments to the bottom of the reactor. , Thus, the images allow us to quantify the kinetics of TiO 2 formation and separation, resolving heterogeneity in the TiO 2 distribution as a continuous function of height within the reactor and how these depend on reagent concentration.…”

Section: Resultsmentioning

confidence: 99%

Real-Time Multiscale Imaging of Heterogeneous Multistage Reactions: Insights into Nanoscale TiO₂ Synthesis

Sanchez Monserrate,

Beauvais,

Vornholt

et al. 2024

J. Am. Chem. Soc.

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Hydrothermal methods are widely used to synthesize functional inorganic materials. The interplay between the reactive species, solution chemistry, and the nanoscale product makes it challenging to control the reaction pathway to achieve a uniform product. Here, we resolve the heterogeneity that arises during hydrothermal synthesis across different length scales. We combine spatially resolved in situ X-ray pair distribution function (PDF) and small-angle X-ray scattering analysis, which are sensitive to structure on the atomic and nanoscale, with a novel time-lapse optical imaging strategy that reveals heterogeneity and phase separations across the entire reaction. For TiO 2 synthesis via hydrothermal hydrolysis of TiCl 4 , we identify multiple cycles of TiO 2 formation and separation that contribute to nonuniformity in the polymorphic product. The PDF data show that the characteristics of TiO 2 formed during each formation−separation cycle differ, contributing to the ongoing challenge of precisely identifying reaction controls. The imaging strategy pioneered here provides an efficient in situ means to systematically compare how the reaction evolves under different chemical conditions, thereby advancing our understanding of functional inorganic material synthesis.

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“…[1][2][3] Since the majority of MOF syntheses is carried out starting from liquid reaction mixtures, the formation of the solid product can be followed in situ employing scattering techniquessuch as X-ray diffraction (XRD), [4][5][6][7][8] small angle X-ray scattering (SAXS), [9][10][11] static/dynamic light scattering (SLS/DLS), [12][13] -or turbidity measurements. [14][15] SAXS, SLS/DLS and turbidity are especially suited to study the earliest stages of crystallisation because they can detect particles with subnanometric size, but they provide no information about the crystal structure of the scattering objects. 1 On the other hand, XRD is limited to crystallites having size at least in the nanometre range and is blind to amorphous matter, making it not suitable for studying the earliest stages of crystallisation.…”

Section: Introductionmentioning

confidence: 99%

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

Shearan¹,

Jacobsen²,

Costantino³

et al. 2021

Preprint

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We report on the results of a thorough in situ 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 in situ in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO3) and amount of the coordination modulator acetic acid (AcOH). When only HNO3 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 HNO3, 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 HNO3 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 HNO3 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 HNO3. Based on these in situ 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.

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Use of open source monitoring hardware to improve the production of MOFs: using STA-16(Ni) as a case study

Cited by 6 publications

References 30 publications

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Real-Time Multiscale Imaging of Heterogeneous Multistage Reactions: Insights into Nanoscale TiO₂ Synthesis

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

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Use of open source monitoring hardware to improve the production of MOFs: using STA-16(Ni) as a case study

Cited by 6 publications

References 30 publications

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Metal–Organic Framework-Derived Hollow Carbon Nanosphere@Ni/Reduced Graphene Oxide Composites for Supercapacitor Electrodes with Enhanced Performance

Real-Time Multiscale Imaging of Heterogeneous Multistage Reactions: Insights into Nanoscale TiO2 Synthesis

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

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Real-Time Multiscale Imaging of Heterogeneous Multistage Reactions: Insights into Nanoscale TiO₂ Synthesis