Crystalline microstructure of boehmites studied by multi-peak analysis of powder X-ray diffraction patterns

Pardo, Pablo; Kojdecki, Marek Andrzej; Calatayud, José Miguel; Amigó, José M.; Alarcón, Javier

doi:10.1017/s0885715617000641

Cited by 5 publications

(5 citation statements)

References 58 publications

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“…XRD patterns show two typical peaks at 2θ of 10.9°and 13.1°for H-M and MIL-100 (Fe) nanoparticles, indicating the crystal structure of MIL-100 (Fe). The relative intensity of these two peaks is consistent with samples prepared using similar synthesis conditions (room temperature, ambient pressure, and water as the solvent) [26], and is slightly different from published literature with an organic solvent at high pressure and temperature [27,28]. Figure 2(g) also indicates the semi-amorphous nature of the Fe-BTC sample as no certain peak is observed in the XRD spectrum.…”

Section: Materials Characterizationsupporting

confidence: 75%

Green synthesis of DOX-loaded hollow MIL-100 (Fe) nanoparticles for anticancer treatment by targeting mitochondria

Zhang¹,

Gu²,

Yun³

et al. 2022

Nanotechnology

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Fe-based Metal-Organic Frameworks (MOFs) are promising drug delivery materials due to their large surface area, high stability, and biocompatibility. However, their drug loading capacity is constrained by their small pore size, and a further improvement in their drug capacity is needed. In this work, we report an effective and green structural modification strategy to improve drug loading capacity for Fe-based MOFs. Our strategy is to grow MIL-100 (Fe) on carboxylate-terminated polystyrene (PS-COOH) via a sustainable route, which creates a large inner cavity as well as exposure of more functional groups that benefit drug loading capacity. We perform the scanning electron microscope and transmission electron microscope to confirm the hollow structure of MIL-100 (Fe). Up to 30% of drug loading capacity has been demonstrated in our study. We also conduct cell viability tests to investigate its therapeutic effects on breast cancer cells (MDA-MB-231). Confocal laser scanning microscopy imaging confirms cellular uptake and mitochondrial targeting function of doxorubicin-loaded H-M (DOX@H-M) nanoparticles. JC-1 staining of cancer cells reveals a significant change in the mitochondrial membrane potential, indicating the mitochondrial dysfunction and apoptosis of tumor cells. Our study paves the way for facile synthesis of hollow structural MOFs, and demonstrates the potential of applying Fe-based MOFs in breast cancer treatment.

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Section: Materials Characterizationsupporting

confidence: 75%

Green synthesis of DOX-loaded hollow MIL-100 (Fe) nanoparticles for anticancer treatment by targeting mitochondria

Zhang¹,

Gu²,

Yun³

et al. 2022

Nanotechnology

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“…Multipeak analysis of the PXRD patterns was applied to determine the reflection positions of the 200 and 400 planes . These changes are presented in Figure a,b.…”

Section: Resultsmentioning

confidence: 99%

“…Multipeak analysis of the PXRD patterns was applied to determine the reflection positions of the 200 and 400 planes. 42 These changes are presented in Figure 8a,b. On the basis of the results, the presence of the shoulders for the 200 and 400 diffracted planes implies the formation of the two hydrated phases as a function of the humidity for Z 5 HN.…”

Section: ■ Experimental Sectionmentioning

confidence: 91%

Structural Analysis and Conduction Mechanisms in Polycrystalline Zinc Hydroxide Nitrate

Ruiz¹,

Rodríguez‐Castellón

Giraldo³

2018

Inorg. Chem.

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The conduction and dielectric properties in zinc hydroxide nitrate (ZHN) were studied in detail as a function of the temperature and relative humidity by impedance spectroscopy, and the structure was investigated by X-ray diffraction (XRD). Elemental analysis indicated a layered material containing carbonate anions [Zn(OH)(NO)(CO)·1.7HO] due to the high capability of adsorption of ZHN, which makes this material appropriate for applications in real conditions. The water content affected the interlayer distance, conductivity, and dielectric response of the layered material. An electrostatic repulsive interaction after reduction of the water content as a function of the temperature causes an increase of the interlayer distance and a decrease in the conductivity response and dielectric behavior. The highest conductivity, 10 Ω cm, was obtained at a shorter interlayer distance for the sample heat-treated at 25 °C. The ZHN synthesized was also characterized at different temperatures using thermogravimetric analysis and Fourier transform infrared and Raman spectroscopy. Multipeak analysis of the XRD patterns at various relative humidity levels showed the formation of a most hydrated phase and an increase of the interlayer distance related with the adsorption of water molecules. This layered material presented a conductivity of 10 Ω cm at high relative humidity (92%). The dipole-dipole interaction appeared to be the dominant mechanism for the dielectric behavior at the lowest temperatures and highest humidity due to the high water content in the ZHN structure. Taking into account its crystallization water and high adsorption of water molecules in the interlayer region, a conduction pathway in the ZHN structure was proposed, which provides the route for proton transport by hydrogen-bonding networks on the basis of a Grotthuss-type mechanism in facilitating the long-range proton hopping at 25 °C. The results for high relative humidity imply that a vehicular conduction mechanism also may contribute to the electrical response.

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“…Boehmite has been studied for multiple applications, such as catalysts, adsorbents, and common precursors for γ-Al 2 O 3 . Boehmite has an orthorhombic structure (space group Cmc 2 1 ) with lattice parameters of approximately a = 3.694 Å, b = 12.214 Å, and c = 2.868 Å . Its crystal structure has been characterized as double-sheet layers bound by hydrogen bonds .…”

Section: Introductionmentioning

confidence: 99%

“…5 Boehmite has an orthorhombic structure (space group Cmc2 1 ) with lattice parameters of approximately a = 3.694 Å, b = 12.214 Å, and c = 2.868 Å. 6 Its crystal structure has been characterized as doublesheet layers bound by hydrogen bonds. 7 The hydrogen bonds organize into parallel chains along the [001] crystallographic direction.…”

Section: Introductionmentioning

confidence: 99%

Energy Barrier of Proton Transfer in 3d Transition Metal-Doped Boehmite

Yang

Xie

et al. 2021

J. Phys. Chem. C

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The crystal structure of boehmite contains a large number of hydrogen-bond chains, which are deemed protontransfer channels that are essential for proton-exchange-membrane materials. The efficiency of proton transfer along these chains is expected to change with the nearby chemical environment, whereas the dependency remains largely unknown. In this study we calculate energy barriers of proton transfer along hydrogenbond chains of 3d transition metal-doped boehmite, using the nudged elastic band method based on density functional theory. Eight 3d transition metals from Sc to Ni are considered with variable doping concentrations from 1/12 to 1/4. Our results show that the energy barriers vary largely with dopant types and concentrations. Ti dopant consistently reduces the energy barrier by up to 2.5 kJ mol −1 compared to pure boehmite. It is found that short hydrogen-bond lengths are generally associated with low energy barriers, and this enables us to search for potential proton conductors in materials of similar structures.

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Crystalline microstructure of boehmites studied by multi-peak analysis of powder X-ray diffraction patterns

Cited by 5 publications

References 58 publications

Green synthesis of DOX-loaded hollow MIL-100 (Fe) nanoparticles for anticancer treatment by targeting mitochondria

Green synthesis of DOX-loaded hollow MIL-100 (Fe) nanoparticles for anticancer treatment by targeting mitochondria

Structural Analysis and Conduction Mechanisms in Polycrystalline Zinc Hydroxide Nitrate

Energy Barrier of Proton Transfer in 3d Transition Metal-Doped Boehmite

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