scholarly journals Influence of pairs of alkali metal cations on the formation of complex phosphates at the crystallization of multicomponent self-fluxes

2020 ◽  
pp. 54-61
Author(s):  
N.Yu. Strutynska ◽  
◽  
M.S. Slobodyanik ◽  
Keyword(s):  
Thermal Analysis ◽  
Single Crystals ◽  
Potassium Phosphate ◽  
Diffraction Method ◽  
Molar Ratio ◽  
Crystal Formation ◽  
Cell Parameters ◽  
Molar Ratios ◽  
Cubic System ◽  
Complex Phosphates

The regularities of phase formation in the systems (МІ1 + МІ2)2O—P2O5—TiO2—МІІO (МІ — Na, K, Rb; MII — Mg, Co, Ni) at the crystallization of multicomponent self-fluxes at the values of molar ratios: (МІ1 + МІ2)/Р = 1.0; Ti/Р = 0.25; MII/Ті = 1.0, and М І 1/М І 2 = 1.0 and 2.0 over the temperature interval of 1000-780 °C have been investigated. For mixed sodium-potassium-phosphate systems, regardless of the ratio of Na/K (1.0 or 2.0), the solidification without crystal formation was found. For Na/Rb-containing systems, the increasing of the so dium amount in the initial melt to the value of molar ratio Na/Rb = 2.0 promoted the crystalization of single crystals of NaTi2(PO4)3 doped by divalent metals ions. In the case of K-Rb-phosphate self-fluxes, it was found that the value of K/Rb = 2.0 is optimal for the growing of langbeinite-related single crystals (K/Rb)2MII0,5Ti1,5(PO4)3 (MII — Mg, Co, Ni) which belong to cubic system (space group P213). The calculated cell parameters for new phosphates (K/Rb)2MII 0.5Ti1.5(PO4)3 depend on the nature of MII: a = 9.851(6) Å for Mg, a = 9.853(9) Å for Co and a = 9.850 (1) - for Ni. In the FTIR spectra of phosphates (K/Rb)2MII0.5Ti1.5(PO4)3, the characteristic modes in the region of 520-650 сm–1 and 1000-1250 сm-1 which have been assigned to symmetric and asymmetric stretching vibrations (ν4, ν1 and ν3) of phosphate tetrahedron confirmed the presence of orthophosphate type anion in their composition. According to results of thermal analysis, the melting points of (K/Rb)2MII0.5Ti1.5(PO4)3 are at a temperatures of 1082 °С for MII — Ni, 1057 °С for MII — Co, and above 1100 °С for MII — Mg. The synthesized complex phosphates have been investigated using the powder X-Ray diffraction method, thermogravimetry, differential thermal analysis, and FTIR-spectroscopy.

scholarly journals Growth and Characterization of Pure and Doped L-Alanine Tartrate Single Crystals

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
K. Rajesh ◽  
B. Milton Boaz ◽  
P. Praveen Kumar
Keyword(s):  
Single Crystals ◽  
Vickers Microhardness ◽  
Diffraction Method ◽  
Dielectric Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Single crystals of pure and Lanthanum doped L-Alanine Tartrate were grown by slow evaporation method. The cell parameters were determined using single crystal X-ray diffraction method. To improve the physical properties of the LAT crystal, Lanthanum dopant was added by 2 mol%. ICP studies confirm the presence of Lanthanum in the grown LAT crystal. Transparency range of the crystal was determined using UV-VIS-NIR spectrophotometer. The functional groups of pure and doped LAT crystals were analyzed by FT-IR spectroscopy. Using Vickers microhardness tester, mechanical strength of the material was found. Dielectric studies of pure and doped LAT single crystals were carried out. The doped LAT crystal is found to have efficiency higher than that of pure LAT crystal.

Syntheses and Crystal Structures of the Solid Solution Sr4OBr2.89(2)Cl3.11(2) and the Elusive Ba2OBr2

2011 ◽  
Vol 66 (10) ◽  
pp. 1000-1004
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Solid Solution ◽  
Solid State ◽  
Single Crystals ◽  
Crystal Structures ◽  
Solid State Reactions ◽  
Molar Ratio ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters

Transparent and colorless single crystals of the compounds Sr4OBr2.89(2)Cl3.11(2) and Ba2OBr2 were obtained by solid-state reactions of SrCl2, SrBr2 and SrO (3 : 3 : 2 molar ratio) or by using an excess of BaO together with BaBr2 and Ba as a flux with the molar ratio 3 : 2 : 2, respectively. Ba2OBr2 crystals are isopointal to K2ZnO2 adopting the orthorhombic space group Ibam (no. 72, Z = 4) with the cell parameters a = 7247.44(10), b = 1297.76(20) and c = 657.43(10) pm. Sr4OBr2.89(2)Cl3.11(2) is isotypic to Ba4OCl6 (or isopointal to K6ZnO4) and crystallizes in the hexagonal space group P63mc (no. 186, Z = 2) with the cell parameters a = 982.20(4) and c = 750.41(7) pm.

Sol-gel Synthesis of Li–ZrSiO4

2000 ◽  
Vol 15 (7) ◽  
pp. 1490-1495 ◽  
Author(s):  
Heriberto Pfeiffer ◽  
Pedro Bosch ◽  
Jose A. Odriozola ◽  
Alberto Lopez ◽  
Jorge A. Ascencio ◽  
...  
Keyword(s):  
Theoretical Analysis ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
Molar Ratio ◽  
Spectroscopy Analysis ◽  
Gel Method ◽  
X Ray ◽  
Cell Parameters ◽  
Molar Ratios ◽  
Sol Gel Synthesis

Li–ZrSiO4 was synthesized by the sol-gel method. Reactions were performed with different Li:Zr molar ratios: 1, 3, 5, and 6. Cell parameters changed as follows: a0 decreased and c0 increased as the Li:Zr molar ratio increased. The x-ray photoelectron spectroscopy analysis showed two kinds of oxygen atoms. The first one was attributed to ZrSiO4 oxygens. The second one was attributed to Li–O bonds. All these results were supported by a theoretical analysis. It was concluded that lithium atoms were held in interstitial positions of the ZrSiO4 structure.

On the accuracy of determining the unit cell parameters of single crystals on modern laboratory diffractometers

2021 ◽  
Vol 62 (5) ◽  
Author(s):  
П.C. Серебренникова ◽  
В.Ю. Комаров ◽  
А.С. Сухих ◽  
С.А. Громилов
Keyword(s):  
Single Crystals ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Cell Parameters

Studies on the Temperature Stability of Pure and Doped Triglycine Sulphate Crystals Using TGA/DTA

2020 ◽  
Vol 10 (3) ◽  
pp. 206-212
Author(s):  
Vijeesh Padmanabhan ◽  
Maneesha P. Madhu ◽  
Supriya M. Hariharan
Keyword(s):  
Thermal Analysis ◽  
Temperature Dependence ◽  
Single Crystals ◽  
Temperature Stability ◽  
Bandgap Energy ◽  
Dsc Analysis ◽  
Slow Cooling ◽  
As Doping ◽  
Similar Dependence ◽  
Temperature Ranges

Aim: To study the temperature stability of TGS doped with ZnSO4, CdCl2, BaCl2, and compare it with that of pure TGS. Objectives: Synthesizing pure and doped TGS and studying their temperature dependence using TGA, DTA, and DSC analysis. Methods: Slow cooling solution growth was used to grow single crystals of pure and doped TGS. The TGA, DTA and DSC analysis was conducted for determining the temperature stability. Results: The thermal analysis of pure and doped TGS shows that the doped samples show a similar dependence on temperature as pure TGS. The temperature of decomposition of pure and doped samples (BTGS, ZTGS, CdTGS) was 226.60°C, 228.38°C, 229.13°C, and 239.13°C respectively. The melting onset of these samples was 214.51°C, 216.04°C, 217.69°C and 216.04°C respectively. Conclusion: The study shows that doping TGS with the above three described materials did not alter their temperature stability considerably. It is a good result as doping TGS, for varying its characteristics like absorbance, reflectance, bandgap energy, etc., which did not alter its temperature stability. Therefore, TGS doped with the above three dopants can be used at the same temperature ranges as of pure TGS but with much-improved efficiency.

scholarly journals Struvite Grown in Gel, Its Crystal Structure at 90 K and Thermoanalytical Study

Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 89 ◽  
Author(s):  
Jolanta Prywer ◽  
Lesław Sieroń ◽  
Agnieszka Czylkowska
Keyword(s):  
Thermal Analysis ◽  
Sodium Metasilicate ◽  
X Ray Diffraction ◽  
Gel Growth ◽  
Growth Technique ◽  
Thermoanalytical Study ◽  
X Ray ◽  
Cell Parameters ◽  
Thermal Analysis Techniques ◽  
Derivative Thermogravimetry

In this article, we report the crystallization of struvite in sodium metasilicate gel by single diffusion gel growth technique. The obtained crystals have a very rich morphology displaying 18 faces. In this study, the habit and morphology of the obtained struvite crystals are analyzed. The crystals were examined and identified as pure struvite by single X-ray diffraction (XRD). The orthorhombic polar noncentrosymmetric space group Pmn21 was identified. The structure of the crystal was determined at a temperature of 90 K. Our research indicates a lack of polymorphism, resulting from the temperature lowering to 90 K, which has not been previously reported. The determined unit cell parameters are as follows a = 6.9650(2) Å, b = 6.1165(2) Å, c = 11.2056(3) Å. The structure of struvite is presented here with a residual factor R1 = 1.2% at 0.80 Å resolution. We also present thermoanalytical study of struvite using thermal analysis techniques such as thermogravimetry (TG), derivative thermogravimetry (DTG) and differential thermal analysis (DTA).

scholarly journals Photocatalytic Reduction of CO2 to Methanol Using a Copper-Zirconia Imidazolate Framework

Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 346
Author(s):  
Sonam Goyal ◽  
Maizatul Shima Shaharun ◽  
Ganaga Suriya Jayabal ◽  
Chong Fai Kait ◽  
Bawadi Abdullah ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Catalyst Support ◽  
Oxidation Potential ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Optimum Parameters ◽  
Reduction Of Co2 ◽  
Enhanced Yield

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.

scholarly journals Growth of sillenite Bi12FeO20 single crystals: structural, thermal, optical, photocatalytic features and first principle calculations

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Durga Sankar Vavilapalli ◽  
Ambrose A. Melvin ◽  
F. Bellarmine ◽  
Ramanjaneyulu Mannam ◽  
Srihari Velaga ◽  
...  
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Photoelectron Spectroscopy ◽  
Diffraction Method ◽  
Lattice Parameter ◽  
First Principle ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Principle Calculations ◽  
Photodegradation Efficiency

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.

scholarly journals Lipozyme 435-Mediated Synthesis of Xylose Oleate in Methyl Ethyl Ketone

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3317
Author(s):  
Maria Carolina Pereira Gonçalves ◽  
Jéssica Cristina Amaral ◽  
Roberto Fernandez-Lafuente ◽  
Ruy de Sousa Junior ◽  
Paulo Waldir Tardioli
Keyword(s):  
Oleic Acid ◽  
Methyl Ethyl Ketone ◽  
Molar Ratio ◽  
Methyl Ethyl ◽  
Sugar Ester ◽  
Molar Ratios ◽  
Emulsion Capacity ◽  
Ping Pong ◽  
Commercial Sugar ◽  
Repeated Use

In this paper, we have performed the Lipozyme 435-catalyzed synthesis of xylose oleate in methyl ethyl ketone (MEK) from xylose and oleic acid. The effects of substrates’ molar ratios, reaction temperature, reaction time on esterification rates, and Lipozyme 435 reuse were studied. Results showed that an excess of oleic acid (xylose: oleic acid molar ratio of 1:5) significantly favored the reaction, yielding 98% of xylose conversion and 31% oleic acid conversion after 24 h-reaction (mainly to xylose mono- and dioleate, as confirmed by mass spectrometry). The highest Lipozyme 435 activities occurred between 55 and 70 °C. The predicted Ping Pong Bi Bi kinetic model fitted very well to the experimental data and there was no evidence of inhibitions in the range assessed. The reaction product was purified and presented an emulsion capacity close to that of a commercial sugar ester detergent. Finally, the repeated use of Lipozyme 435 showed a reduction in the reaction yields (by 48 and 19% in the xylose and oleic acid conversions, respectively), after ten 12 h-cycles.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

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