On iodido bismuthates, bismuth complexes and polyiodides with bismuth in the system BiI3/18-crown-6/I2

Abstract The iodido bismuthates [Bi(18-crown-6)I2][BiI4] (1) and [Bi(18-crown-6)I2][Bi3I10] (2), the neutral complex [Bi(C6H14O4)I3](18-crown-6) (3) as well as the polyiodides [Bi(18-crown-6)I2][I5](18-crown-6) (4), [Bi(18-crown-6)I2]2[I14] (5) and [Bi(18-crown-6)I2]2[I19] (6) were prepared by reaction of BiI3, 18-crown-6, and I2 at T = 60–120 °C. The compounds 1–5 were prepared in [n-Bu3MeN][N(Tf)2] as an ionic liquid ([n-Bu3MeN]: tributylmethylammonium, [N(Tf)2]: bis(trifluoromethylsulfonyl)imide), whereas 6 was obtained only by direct reaction of the starting materials. The title compounds exhibit two different constitutions of the [Bi(18-crown-6)I2]+ cation as well as a non-charged, molecular [Bi(C6H14O4)I3] unit with a triethylene glycol ligand generated in situ by cleavage of the crown ether. Infinite chain-like [ BiI 2 / 1 I 4 / 2 ] − ∞ 1 ${}_{\infty }{}^{1}[{{\text{BiI}}_{2/1}{\text{I}}_{4/2}]}^{-}$ and [ Bi 6 I 18 / 1 I 4 / 2 ∞ 1 ] − ${{}_{\infty }{}^{1}[{\text{Bi}}_{6}{\text{I}}_{18/1}{\text{I}}_{4/2}]}^{-}$ anions occur in 1 and 2, whereas various polyiodide anions (e.g. [I3]−, [I5]−, [I7]−, [I9]−) with partly complex interaction are observed in 4, 5, and 6. The title compounds were characterized by single-crystal X-ray diffraction analysis and infrared spectroscopy. In the case of 1 and 2, the optical band gap was determined to be E g = 1.91 and 1.62 eV, respectively. Especially, the ionic-liquid-based synthesis affords the different metastable compounds with variable composition and structure in a narrow temperature range.

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Modification of clays with styrenic ionic liquid by Synthesis of in-situ Polystyrene Nanocomposite

e-Polymers ◽

10.1515/epoly-2013-0131 ◽

2013 ◽

Vol 13 (1) ◽

Author(s):

Mohammad Galehassadi ◽

Fatemeh Hosseinzadeh ◽

Mehrdad Mahkam

Keyword(s):

Electron Microscopy ◽

Ionic Liquid ◽

Clay Nanocomposites ◽

X Ray Diffraction ◽

X Ray ◽

Modified Montmorillonite ◽

Transmission Electron ◽

Insitu Polymerization ◽

Thermal Stability Of

Abstract Nanocomposites of polystyrene (PS) was prepared with new styrenic ionic liquid, N-(4-vinyl benzyl)-(N,N-dimethylamino) pyridinium chloride[VBMAP], surfactants used as organic modifications for the clays. Sodium montmorillonite (Na-MMT) was successfully modified by [VBMAP] to become OMMT through cation exchange technique which is shown by the increase of basalspacing of clay by XRD. The composite material based on polystyrene and organo-modified montmorillonite (OMMT) was prepared by insitu polymerization and characterized. The morphology of the polymer/clay hybrids was evaluated by X-ray diffraction (XRD) ,transmission electron microscopy (TEM) and scanning electron microscopy (SEM), showing good overall dispersion of the clay. The thermal stability of the polymer/clay nanocomposites were enhanced, as evaluated by thermogravimetric analysis.

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Direct observation of α- to β-glycine transformation during the ionic liquid-mediated crystallization process

CrystEngComm ◽

10.1039/c7ce02247f ◽

2018 ◽

Vol 20 (19) ◽

pp. 2705-2712

Author(s):

Liangfei Ouyang ◽

Tengfei Zheng ◽

Liang Shen

Keyword(s):

Ionic Liquid ◽

Direct Observation ◽

Liquid Water ◽

Polymorphic Transformation ◽

Crystallization Process ◽

Water System ◽

X Ray Diffraction ◽

X Ray

The application of in situ powder X-ray diffraction (XRD) to monitor the polymorphic transformation and crystallization of glycine from an ionic liquid–water system is introduced.

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In Situ High-Pressure Synthesis of New Outstanding Light-Element Materials under Industrial P-T Range

Materials ◽

10.3390/ma14154245 ◽

2021 ◽

Vol 14 (15) ◽

pp. 4245

Author(s):

Yann Le Godec ◽

Alexandre Courac

Keyword(s):

High Pressure ◽

Light Element ◽

X Ray Diffraction ◽

Exciting Field ◽

X Ray ◽

High Pressure Synthesis ◽

Time Space ◽

Pressure Synthesis ◽

Metastable Compounds

High-pressure synthesis (which refers to pressure synthesis in the range of 1 to several GPa) adds a promising additional dimension for exploration of compounds that are inaccessible to traditional chemical methods and can lead to new industrially outstanding materials. It is nowadays a vast exciting field of industrial and academic research opening up new frontiers. In this context, an emerging and important methodology for the rapid exploration of composition-pressure-temperature-time space is the in situ method by synchrotron X-ray diffraction. This review introduces the latest advances of high-pressure devices that are adapted to X-ray diffraction in synchrotrons. It focuses particularly on the “large volume” presses (able to compress the volume above several mm3 to pressure higher than several GPa) designed for in situ exploration and that are suitable for discovering and scaling the stable or metastable compounds under “traditional” industrial pressure range (3–8 GPa). We illustrated the power of such methodology by (i) two classical examples of “reference” superhard high-pressure materials, diamond and cubic boron nitride c-BN; and (ii) recent successful in situ high-pressure syntheses of light-element compounds that allowed expanding the domain of possible application high-pressure materials toward solar optoelectronic and infra-red photonics. Finally, in the last section, we summarize some perspectives regarding the current challenges and future directions in which the field of in situ high-pressure synthesis in industrial pressure scale may have great breakthroughs in the next years.

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Progress in Microanalysis

Microscopy Today ◽

10.1017/s1551929513000400 ◽

2013 ◽

Vol 21 (3) ◽

pp. 7-7

Author(s):

Charles Lyman

Keyword(s):

Light Microscopy ◽

Spatial Resolution ◽

Equilibrium Phase ◽

X Ray Diffraction ◽

Bulk Analysis ◽

X Ray ◽

Analysis Techniques ◽

Composition And Structure

Many researchers view microanalysis as the determination of composition and structure of individual phases at a spatial resolution of 1 μm or better. It is remarkable to me that much of what we know about the phases shown in equilibrium phase diagrams was determined using bulk analysis techniques like powder X-ray diffraction in combination with light microscopy of flat-polished sections of materials. The identities and amounts of phases were deduced from systematic experiments because there was no way to analyze micrometer-sized phases in situ.

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The Effect of Acetate on the Electrodeposition of Manganese on Polycrystalline Au without SeO2 Additives

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.937.34 ◽

2014 ◽

Vol 937 ◽

pp. 34-40

Author(s):

Wen Po Li ◽

Xiu Li Zuo ◽

Jun Ying Yang ◽

Sheng Tao Zhang

Keyword(s):

Spectroscopic Ellipsometry ◽

Quartz Crystal ◽

Single Layer ◽

Electrochemical Quartz Crystal Microbalance ◽

X Ray Diffraction ◽

Energy Dispersion Spectroscopy ◽

X Ray ◽

Composition And Structure ◽

Single Layer Model

The influence of acetate additives on the mechanism of manganese electrodeposition from chloride-based acidic solution was investigated by electrochemical quartz crystal microbalance and spectroscopic ellipsometry. The EQCM data were represented as plots △m versusE.Because they are not affected by interference from the hydrogen evolution reaction, they clearly show the manganese reduction and oxidation processes. The in situ spectroscopic ellipsometry ( SE) data were analyzed with a single-layer model ( substrate Au - deposition Mn layer) and the thicknesses of Mn layer were obtained by fitting experimental data with the model.Morphology, chemical composition and structure of the manganese deposits were analyzed by scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), and X-ray diffraction (XRD). The results showed that in the absence of acetate additives, Mn (OH)2is formed. In the presence of acetate additives, the formation of α-Mn was observed and the deposition rate of Mn electrodeposition on the Au electrode slowed down.

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Electrochemical and in-situ X-ray diffraction studies of Ti 3 C 2 T x MXene in ionic liquid electrolyte

Electrochemistry Communications ◽

10.1016/j.elecom.2016.08.023 ◽

2016 ◽

Vol 72 ◽

pp. 50-53 ◽

Cited By ~ 58

Author(s):

Zifeng Lin ◽

Patrick Rozier ◽

Benjamin Duployer ◽

Pierre-Louis Taberna ◽

Babak Anasori ◽

...

Keyword(s):

Ionic Liquid ◽

Liquid Electrolyte ◽

X Ray Diffraction ◽

X Ray ◽

Ionic Liquid Electrolyte

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In Situ Growth of PbZrxTi1-xO3 Thin Films by Pulsed Laser Deposition

MRS Proceedings ◽

10.1557/proc-191-25 ◽

1990 ◽

Vol 191 ◽

Cited By ~ 16

Author(s):

D. B. Chrisey ◽

J. S. Horwitz ◽

K. S. Grabowski

Keyword(s):

Thin Films ◽

Substrate Temperature ◽

Laser Deposition ◽

X Ray Diffraction ◽

X Ray ◽

Composition And Structure ◽

Elastic Backscattering ◽

Deposited Film ◽

Deposited Films

ABSTRACTWe have investigated the composition and structure of thin films of PbZrxTi1-xO3 (x-0.54) produced in situ by pulsed excimer laser deposition from a stoichiometric pressed oxide target. Thin films were deposited onto (100) MgO and SrTiO3 substrates as a function of substrate temperature between room temperature and 750 °C, and oxygen background pressures between vacuum and 300 mtorr. The deposited films were very smooth with particulates covering less than 0.5% of the surface. Elastic backscattering spectroscopy was used to determine the relative atomic fractions. In the deposited films, the Pb stoichiometry was found to be very sensitive to both the substrate temperature and the O2 background pressure. Above ∼600 °C, the Pb content dropped rapidly with increasing substrate temperature for a 50 mtorr 02 background. At 550 °C the Pb content was near-stoichiometric for O2 background pressures between 200 and 300 mtorr but dropped monotonically to ∼20% of the expected value for depositions in a vacuum (i.e., no O2 background). Over this entire range of pressures and temperatures the Ti/Zr stoichiometry ratio was relatively uneffected. The structure and orientation of the deposited films, as determined by x-ray diffraction, followed the Pb deficiency via the production of other phases and orientations. Crystallation of the deposited film was observed at temperatures as low as 400 °C for 200 mtorr O2 background. At 550 °C and 200 –300 mtorr, (100) oriented PbZrxTi1-xO3 was observed on SrTiO3 substrates.

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The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071107 ◽

1973 ◽

Vol 31 ◽

pp. 132-133 ◽

Cited By ~ 1

Author(s):

R. E. Herfert

Keyword(s):

Surface Characterization ◽

Analytical Techniques ◽

X Ray Diffraction ◽

Depth Of Penetration ◽

X Ray ◽

The Past ◽

Transmission Electron ◽

Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

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