Phase Transitions in Metal–Organic Frameworks Directly Monitored through In Situ Variable Temperature Liquid-Cell Transmission Electron Microscopy and In Situ X-ray Diffraction

2020 ◽  
Vol 142 (10) ◽  
pp. 4609-4615 ◽  
Author(s):  
Jiafei Lyu ◽  
Xinyi Gong ◽  
Seung-Joon Lee ◽  
Karthikeyan Gnanasekaran ◽  
Xuan Zhang ◽  
...  
2015 ◽  
Vol 137 (23) ◽  
pp. 7322-7328 ◽  
Author(s):  
Joseph P. Patterson ◽  
Patricia Abellan ◽  
Michael S. Denny ◽  
Chiwoo Park ◽  
Nigel D. Browning ◽  
...  

Author(s):  
Stephen J. I. Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  

ACS Nano ◽  
2020 ◽  
Vol 14 (7) ◽  
pp. 8735-8743 ◽  
Author(s):  
Karthikeyan Gnanasekaran ◽  
Kristina M. Vailonis ◽  
David M. Jenkins ◽  
Nathan C. Gianneschi

Clay Minerals ◽  
2005 ◽  
Vol 40 (2) ◽  
pp. 191-203 ◽  
Author(s):  
F. Khormali ◽  
A. Abtahi ◽  
H. R. Owliaie

AbstractClay minerals of calcareous sedimentary rocks of southern Iran, part of the old Tethys area, were investigated in order to determine their origin and distribution, and to reconstruct the palaeoclimate of the area. Chemical analysis, X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and thin-section studies were performed on the 16 major sedimentary rocks of the Fars and Kuhgiluyeh Boyerahmad Provinces.Kaolinite, smectite, chlorite, illite, palygorskite and illite-smectite interstratified minerals were detected in the rocks studied. The results revealed that detrital input is possibly the main source of kaolinite, smectite, chlorite and illite, whilein situneoformation during the Tertiary shallow saline and alkaline environment could be the dominant cause of palygorskite occurrences in the sedimentary rocks.The presence of a large amount of kaolinite in the Lower Cretaceous sediments and the absence or rare occurrence of chlorite, smectite, palygorskite and illite are in accordance with the warm and humid climate of that period. Smaller amounts of kaolinite and the occurrence of smectite in Upper Cretaceous sediments indicate the gradual shift from warm and humid to more seasonal climate. The occurrence of palygorskite and smectite and the disappearance of kaolinite in the late Palaeocene sediments indicate the increase in aridity which has probably continued to the present time.


2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.


2013 ◽  
Vol 320 ◽  
pp. 483-487 ◽  
Author(s):  
Ming Li ◽  
Deng Bing Li ◽  
Jing Pan ◽  
Guang Hai Li

W-doped VO2 (B) nanoneedles were successfully synthesized by solgel combing with hydrothermal treatment, in which the polyethylene glycol (PEG) was used as both surfactant and reducing. The metastable VO2 (B) was completely transformed to thermochromic VO2 (M) after annealing at high purity N2 atmosphere. The DSC results exhibit a strong crystallographic transition, and the phase transition temperature of VO2 (M) can be reduced to about 38 °C by W-doping. Field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HR-TEM) were used to characterize the morphology and crystalline structure of the samples. The variable-temperature infrared transmittance spectra of VO2 (M) demonstrate their potential applications in energy saving field.


2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  

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.


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