Single Crystal Formation by Solid-State Reaction Between p-Benzoquinone and 2,4,5-Trichlorophenol

2002 ◽  
Vol 55 (4) ◽  
pp. 271 ◽  
Author(s):  
N. B. Singh ◽  
A. Pathak ◽  
R. Fröhlich

Vapours of p-benzoquinone (BQ) have been found to react with solid 2,4,5-trichlorophenol (TCP). The reaction product (BQ-TCP) separated in the form of monoclinic single crystals, the structure of which was determined by X-ray diffraction to reveal that the two molecules are linked by a single hydrogen bond between the carbonyl oxygen of BQ and the phenolic hydrogen of TCP.

2021 ◽  
Author(s):  
Sivasubramani Vediyappan ◽  
Arumugam Raja ◽  
Ro Mu Jauhar ◽  
Ramachandran Kasthuri ◽  
Vishwanathan Vijayan ◽  
...  

Abstract 2-amino-5-nitropyridine 4-chlorobenzoic acid (1:1) (2A5NP4CBA), a potentially useful organic adduct compound has been synthesized and grown as optically transparent single crystals by conventional slow evaporation solution technique (SEST) for the first time in the literature. The formation of the new crystalline material was confirmed by the single-crystal X-ray diffraction (SXRD) analysis and the crystal structure of the grown crystal was found to be monoclinic. Fourier transform infrared (FTIR) spectrum has been recorded by the KBr pellet technique to determine the various vibrational functional groups in the title material. The powder X-ray diffraction (PXRD) and high-resolution X-ray diffraction (HRXRD) analyses have been carried out and the obtained results reveal that the grown crystal has a single-phase and is free from structural grain boundaries. The obtained less value (32 arc-s) of full width at half maximum (FWHM) for (001) plane indicates the excellent crystalline quality of the title 2A5NP4CBA single crystal. The linear optical properties were evaluated by the UV-vis-NIR absorption and transmittance analyses and the obtained results reveal that the grown crystal possesses more than 70% of optical transmittance window with the cut-off edge at 419 nm. The thermal analysis discloses that the grown crystal possesses good thermal stability of about 187°C. To determine the appropriateness of the grown crystal for the high-power laser application, laser damage threshold (LDT) analysis has been carried out by Nd: YAG laser of a wavelength of 1064 nm. The third-order nonlinear optical coefficients such as nonlinear absorption (β), nonlinear refraction (n 2 ) and nonlinear susceptibility (χ (3) ) have been evaluated by utilizing the single beam Z-scan technique using a solid-state laser of wavelength 532 nm. The calculated ꭓ (3) value is found to be reasonably good compared to other organic single crystals which are reported in the literature. The optical limiting (OL) behavior of the title crystal was evaluated using a solid-state laser at 532 nm and the limiting threshold was found to be 7.8 mW/cm 2 .


2007 ◽  
Vol 62 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Nachiappan Arumugam ◽  
Eva-Maria Peters ◽  
Martin Jansen

A new potassium molybdenum oxide, K6Mo10O33, was synthesized by solid state reaction from the appropriate quantities of pre-dried MoO3 and K2MoO4, fired at around 650 °C for 2 d. The structure has been solved by using single crystal X-ray diffraction. The compound adopts the space group P1, with the lattice constants a = 7.7100(5), b = 11.9659(8), c = 17.1321(12) A° , α = 86.42 (10), β = 77.18(10), γ = 74.14(10)°. The structure is built up of infinite chains of edge-sharing MoO6 octahedra and groups of four MoO6 octahedra forming Mo4O17 units. These sub-units are connected together by common vertices.


Author(s):  
Hirokazu Kimura ◽  
Hiroshi Sakabe ◽  
Hitoshi Morita ◽  
Takashi Itoh ◽  
Takashi Konishi

It is well known that several ω-amino acids are polymerized in the solid state. A single crystal of ε-aminocaproic acid has been reported to be polymerized in the solid state to be the biaxially oriented nylon 6. We also reported in the previous paper that the thermal solid state polymerization of glycine single crystal produced poly(glycine-I) crystal.In this paper,structure of poly(β-alanine) polymerized in the solid state is investigated by means of scanning electron microscopy (SEM).transmission electron microscopy (TEM) and X-ray diffraction.Commercial β-alanine (Nakarai Tesque,Inc.,Kyoto) was recrystallized three times from the distilled-water solution (lg/ml) at 80°C. The single crystal continued to grow gradually during 24 hr. The obtained single crystals with rhombic habit had clear cleavage planes. These single crystals about 10 mm in size were used as the original specimens. The polymerization procedure was carried out on the single crystals at temperatures between 140 and 170°C in an evacuated and subsequently sealed tube.


CrystEngComm ◽  
2014 ◽  
Vol 16 (48) ◽  
pp. 10987-10996 ◽  
Author(s):  
Rita De Zorzi ◽  
Giovanna Brancatelli ◽  
Monica Melegari ◽  
Roberta Pinalli ◽  
Enrico Dalcanale ◽  
...  

The solid-state selectivity of a cavitand receptor towards short alkyl chain alcohols was evaluated by analysis of X-ray diffraction data of isomorphous single crystals grown in competition binding experiments.


Author(s):  
В.А. Кульбачинский ◽  
В.Г. Кытин ◽  
Д.А. Зиновьев ◽  
Н.В. Маслов ◽  
P. Singha ◽  
...  

AbstractAntimony-telluride-based nanocomposite samples containing different weight fractions of graphite (Sb_2Te_3 + x % graphite, where x = 0.0, 0.5, 1.0, and 2.5%) are synthesized and studied. The samples are produced by a solid-state reaction with the use of a ball mill. X-ray diffraction measurements show that the Sb_2Te_3 phase is present in the nanocomposites. All of the diffraction peaks are identified as corresponding to the rhombohedral structure of symmetry $$R\bar {3}m$$ . No additional peaks related to graphite are observed because of its low content. Moreover, the X-ray data show the insolubility of graphite in Sb_2Te_3: the peaks related to Sb_2Te_3 remain unchanged upon the addition of graphite. The thermal conductivity, thermoelectric power, and resistivity of the samples are studied in the temperature range 80 K ≤ T ≤ 320 K. The thermal conductivity k of the nanocomposite decreases several times compared to the thermal conductivity of single-crystal Sb_2Te_3 and reaches k ≈ 0.95 W m^–1 K^–1 at x = 0.5%. The parameter k unsteadily depends on the content of graphite. The thermoelectric power of the nanocomposites with graphite at x = 1.0% is higher compared to that of nanostructured Sb_2Te_3.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Durga Sankar Vavilapalli ◽  
Ambrose A. Melvin ◽  
F. Bellarmine ◽  
Ramanjaneyulu Mannam ◽  
Srihari Velaga ◽  
...  

AbstractIdeal sillenite type Bi12FeO20 (BFO) micron sized single crystals have been successfully grown via inexpensive hydrothermal method. The refined single crystal X-ray diffraction data reveals cubic Bi12FeO20 structure with single crystal parameters. Occurrence of rare Fe4+ state is identified via X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS). The lattice parameter (a) and corresponding molar volume (Vm) of Bi12FeO20 have been measured in the temperature range of 30–700 °C by the X-ray diffraction method. The thermal expansion coefficient (α) 3.93 × 10–5 K−1 was calculated from the measured values of the parameters. Electronic structure and density of states are investigated by first principle calculations. Photoelectrochemical measurements on single crystals with bandgap of 2 eV reveal significant photo response. The photoactivity of as grown crystals were further investigated by degrading organic effluents such as Methylene blue (MB) and Congo red (CR) under natural sunlight. BFO showed photodegradation efficiency about 74.23% and 32.10% for degrading MB and CR respectively. Interesting morphology and microstructure of pointed spearhead like BFO crystals provide a new insight in designing and synthesizing multifunctional single crystals.


2021 ◽  
Vol 3 (4) ◽  
Author(s):  
Yogesh Kumar ◽  
Rabia Sultana ◽  
Prince Sharma ◽  
V. P. S. Awana

AbstractWe report the magneto-conductivity analysis of Bi2Se3 single crystal at different temperatures in a magnetic field range of ± 14 T. The single crystals are grown by the self-flux method and characterized through X-ray diffraction, Scanning Electron Microscopy, and Raman Spectroscopy. The single crystals show magnetoresistance (MR%) of around 380% at a magnetic field of 14 T and a temperature of 5 K. The Hikami–Larkin–Nagaoka (HLN) equation has been used to fit the magneto-conductivity (MC) data. However, the HLN fitted curve deviates at higher magnetic fields above 1 T, suggesting that the role of surface-driven conductivity suppresses with an increasing magnetic field. This article proposes a speculative model comprising of surface-driven HLN and added quantum diffusive and bulk carriers-driven classical terms. The model successfully explains the MC of the Bi2Se3 single crystal at various temperatures (5–200 K) and applied magnetic fields (up to 14 T).


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