Solvothermal synthesis of nano-sized skutterudite Co1−xNixSb3 powders

2013 ◽  
Vol 28 (S1) ◽  
pp. S17-S21 ◽  
Author(s):  
J.Q. Li ◽  
Z.P. Zhang ◽  
R.M. Luo ◽  
W.Q. Ao ◽  
F.S. Liu
Keyword(s):  
Solvothermal Synthesis ◽  
Figure Of Merit ◽  
Single Phase ◽  
Cell Parameter ◽  
Triethylene Glycol ◽  
Diffraction Field ◽  
X Ray Diffraction ◽  
X Ray ◽  
Synthesis Conditions ◽  
Glycol Solution

Nanostructuring is one of the effective approaches to lower the thermal conductivity of thermoelectric materials for improving its figure of merit. The nano-sized uniform skutterudite Co1−xNixSb3 (x = 0, 0.05, 0.075, 0.125, 0.15, and 0.25) thermoelectric powders were synthesized in triethylene glycol solution by using CoCl2, NiCl2, and SbCl3 as precursors and NaBH4 as the reductant. Different synthesis conditions were studied to pursue pure and uniform skutterudite CoSb3 powders. The powders were characterized by X-ray diffraction, field emission scanning electron microscope, and energy-dispersive X-ray analysis. Experimental results show that a Ni-doped skutterudite Co1−xNixSb3 single phase was obtained at 290 °C for 12 h. The powders are spherical, small, and uniform. As x increases from 0 to 0.25, the unit-cell parameter a increases from 0.9044 to 0.9065 nm and the particle size increases from 10 to 30 nm.

scholarly journals Modifying Crystal Morphology And Framework Composition Of Composition Of Zeolite L (LTL) – A Co-Solvent Approach

2021 ◽  
Author(s):  
Adriana Gaona-Gomez
Keyword(s):  
Crystal Morphology ◽  
Triethylene Glycol ◽  
Research Field ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Synthesis Conditions ◽  
Zeolite L ◽  
Higher Temperature ◽  
Catalytic Performances

The first part of this study investigates synthesis protocols to tune the size and the morphology of zeolite L (LTL) crystals using three different glycols. The outcomes clearly demonstrate that the formation of pure LTL phase is greatly facilitated at 150 ºC for 6 days only when using triethylene glycol (TEG) as the co-solvent, verified by powder X-ray diffraction (PXRD). SEM images show that LTL crystals present a cylinder-like structure with an aspect ratio of one. The formation of pure LTL phase is dramatically deteriorated when the synthesis conditions are changed to higher temperature (180 ºC), various synthesis durations (1-3 days) and aging time, and using other co-solvents (ethylene glycol and diethylene glycol). Inspired by published results indicating the interactions between Ge and glycols, I developed three synthesis approaches exploring the feasibility of incorporating germanium (Ge) into LTL framework using TEG in the second part of this study. Moreover, studies report that the incorporation of Ge in zeolite frameworks can enhance zeolites’ catalytic performances. The results from my investigation show that highly crystalline and well-defined LTL crystals are attained at 150 ºC for 3 days. X-ray fluorescence (XRF) shows the presence of Ge in LTL samples, indicating that the incorporation of Ge is very promising using the developed synthesis approaches. The outcomes are expected to be very useful to other researchers in the zeolites research field.

scholarly journals Modifying Crystal Morphology And Framework Composition Of Composition Of Zeolite L (LTL) – A Co-Solvent Approach

2021 ◽  
Author(s):  
Adriana Gaona-Gomez
Keyword(s):  
Crystal Morphology ◽  
Triethylene Glycol ◽  
Research Field ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Synthesis Conditions ◽  
Zeolite L ◽  
Higher Temperature ◽  
Catalytic Performances

The first part of this study investigates synthesis protocols to tune the size and the morphology of zeolite L (LTL) crystals using three different glycols. The outcomes clearly demonstrate that the formation of pure LTL phase is greatly facilitated at 150 ºC for 6 days only when using triethylene glycol (TEG) as the co-solvent, verified by powder X-ray diffraction (PXRD). SEM images show that LTL crystals present a cylinder-like structure with an aspect ratio of one. The formation of pure LTL phase is dramatically deteriorated when the synthesis conditions are changed to higher temperature (180 ºC), various synthesis durations (1-3 days) and aging time, and using other co-solvents (ethylene glycol and diethylene glycol). Inspired by published results indicating the interactions between Ge and glycols, I developed three synthesis approaches exploring the feasibility of incorporating germanium (Ge) into LTL framework using TEG in the second part of this study. Moreover, studies report that the incorporation of Ge in zeolite frameworks can enhance zeolites’ catalytic performances. The results from my investigation show that highly crystalline and well-defined LTL crystals are attained at 150 ºC for 3 days. X-ray fluorescence (XRF) shows the presence of Ge in LTL samples, indicating that the incorporation of Ge is very promising using the developed synthesis approaches. The outcomes are expected to be very useful to other researchers in the zeolites research field.

Raman And Fluorescence Spectra Observed in Laser Microprobe Measurements of Several Compositions in the Ln-Ba-Cu-O System

1990 ◽  
Vol 48 (2) ◽  
pp. 278-279
Author(s):  
Edgar S. Etz ◽  
Thomas D. Schroeder ◽  
Winnie Wong-Ng
Keyword(s):  
Fluorescence Spectra ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Ceramic Powders ◽  
Conventional Solid State Reaction ◽  
X Ray ◽  
Raman Microprobe ◽  
Methods Of Synthesis ◽  
Compositional Homogeneity ◽  
Processing Techniques

We are investigating by Raman microprobe measurements the superconducting and related phases in the LnBa2Cu3O7-x (for x=0 to 1) system where yttrium has been replaced by several of the lanthanide (Ln = Nd,Sm,Eu,Ho,Er) elements. The aim is to relate the observed optical spectra (Raman and fluorescence) to the compositional and structural properties of these solids as part of comprehensive materials characterization. The results are correlated with the methods of synthesis, the processing techniques of these materials, and their superconducting properties. Of relevance is the substitutional chemistry of these isostructural systems, the differences in the spectra, and their microanalytical usefulness for the detection of impurity phases, and the assessment of compositional homogeneity. The Raman spectra of most of these compounds are well understood from accounts in the literature.The materials examined here are mostly ceramic powders prepared by conventional solid state reaction techniques. The bulk samples are of nominally single-phase composition as determined by x-ray diffraction.

Observation of pseudo 10-fold symmetry in the ordered iron-zinc delta phase

1992 ◽  
Vol 50 (1) ◽  
pp. 36-37
Author(s):  
L. A. Giannuzzi ◽  
A. S. Ramani ◽  
P. R. Howell ◽  
H. W. Pickering ◽  
W. R. Bitler
Keyword(s):  
Single Phase ◽  
X Ray Diffraction ◽  
Rich Region ◽  
Average Cell ◽  
X Ray ◽  
Delta Phase ◽  
Cell Dimensions ◽  
Δ Phase ◽  
Morphological Differences ◽  
Concentration Discontinuity

The δ phase is a Zn-rich intermetallic, having a composition range of ∼ 86.5 - 92.0 atomic percent Zn, and is stable up to 665°C. The stoichiometry of the δ phase has been reported as FeZn7 and FeZn10 The deviation in stoichiometry can be attributed to variations in alloy composition used by each investigator. The structure of the δ phase, as determined by powder x-ray diffraction, is hexagonal (P63mc or P63/mmc) with cell dimensions a = 1.28 nm, c = 5.76 nm, and 555±8 atoms per unit cell. Later work suggested that the layer produced by hot-dip galvanizing should be considered as two distinct phases which are characterized by their morphological differences, namely: the iron-rich region with a compact appearance (δk) and the zinc-rich region with a columnar or palisade microstructure (δp). The sub-division of the δ phase was also based on differences in diffusion behavior, and a concentration discontinuity across the δp/δk boundary. However, work utilizing Weisenberg photographs on δ single crystals reported that the variation in lattice parameters with composition was small and hence, structurally, the δk phase and the δp phase were the same and should be thought of as a single phase, δ. Bastin et al. determined the average cell dimensions to be a = 1.28 nm and c = 5.71 nm, and suggested that perhaps some kind of ordering process, which would not be observed by x-ray diffraction, may be responsible for the morphological differences within the δ phase.

Selective catalytic reduction of NO by Co-Mn based nanocatalysts

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Vahid Zabihi ◽  
Mohammad Hasan Eikani ◽  
Mehdi Ardjmand ◽  
Seyed Mahdi Latifi ◽  
Alireza Salehirad
Keyword(s):  
Selective Catalytic Reduction ◽  
Catalytic Reduction ◽  
Energy Dispersive ◽  
Diffraction Field ◽  
X Ray Diffraction ◽  
X Ray ◽  
Analysis Techniques ◽  
Acidic Sites ◽  
Temperature Window ◽  
Temperature Programmed

Abstract One of the most significant aspects in selective catalytic reduction (SCR) of nitrogen oxides (NOx) is developing suitable catalysts by which the process occurs in a favorable way. At the present work SCR reaction by ammonia (NH3-SCR) was conducted using Co-Mn spinel and its composite with Fe-Mn spinel, as nanocatalysts. The nanocatalysts were fabricated through liquid routes and then their physicochemical properties such as phase composition, degree of agglomeration, particle size distribution, specific surface area and also surface acidic sites have been investigated by X-ray diffraction, Field Emission Scanning Electron Microscope, Energy-dispersive X-ray spectroscopy, energy dispersive spectroscopy mapping, Brunauer–Emmett–Teller, temperature-programmed reduction (H2-TPR) and temperature-programmed desorption of ammonia (NH3-TPD) analysis techniques. The catalytic activity tests in a temperature window of 150–400 °C and gas hourly space velocities of 10,000, 18,000 and 30,000 h−1 revealed that almost in all studied conditions, CoMn2O4/FeMn2O4 nanocomposite exhibited better performance in SCR reaction than CoMn2O4 spinel.

scholarly journals Preparation of high-entropy carbides by different sintering techniques

2021 ◽  
Vol 56 (19) ◽  
pp. 11237-11247 ◽  
Author(s):  
Johannes Pötschke ◽  
Manisha Dahal ◽  
Mathias Herrmann ◽  
Anne Vornberger ◽  
Björn Matthey ◽  
...  
Keyword(s):  
Grain Size ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Vacuum Sintering ◽  
X Ray ◽  
High Entropy ◽  
Mean Grain Size ◽  
The Mean ◽  
Gas Pressure Sintering ◽  
Hardness Values

AbstractDense (Hf, Ta, Nb, Ti, V)C- and (Ta, Nb, Ti, V, W)C-based high-entropy carbides (HEC) were produced by three different sintering techniques: gas pressure sintering/sinter–HIP at 1900 °C and 100 bar Ar, vacuum sintering at 2250 °C and 0.001 bar as well as SPS/FAST at 2000 °C and 60 MPa pressure. The relative density varied from 97.9 to 100%, with SPS producing 100% dense samples with both compositions. Grain size measurements showed that the substitution of Hf with W leads to an increase in the mean grain size of 5–10 times the size of the (Hf, Ta, Nb, Ti, V,)C samples. Vacuum-sintered samples showed uniform grain size distribution regardless of composition. EDS mapping revealed the formation of a solid solution with no intermetallic phases or element clustering. X-ray diffraction analysis showed the structure of mostly single-phase cubic high-entropy carbides. Hardness measurements revealed that (Hf, Ta, Nb, Ti, V)C samples possess higher hardness values than (Ta, Nb, Ti, V, W)C samples.

scholarly journals Rapid four-component synthesis of dihydropyrano[2,3-c]pyrazoles using nano-eggshell/Ti(IV) as a highly compatible natural based catalyst

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi Bi Fatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi
Keyword(s):  
Thermo Gravimetric Analysis ◽  
Reaction Times ◽  
Diffraction Field ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solvent Free Conditions ◽  
High Yields ◽  
Work Up

AbstractNano-eggshell/Ti(IV) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives. The characterization of nano-eggshell/Ti(IV) was performed using Fourier Transform Infrared spectroscopy, X-ray Diffraction, Field Emission Scanning Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and Thermo Gravimetric Analysis. Dihydropyrano[2,3-c]pyrazoles were synthesized in the presence of nano-eggshell/Ti(IV) via a four component reaction of aldehydes, ethyl acetoacetate, malononitrile and hydrazine hydrate at room temperature under solvent free conditions. The principal affairs of this procedure are mild condition, short reaction times, easy work-up, high yields, reusability of the catalyst and the absence of toxic organic solvents.

scholarly journals Influence of Li2CO3 addition on electrical and magnetic properties of Ni0.6Mg0.4Fe2O4

2020 ◽  
Vol 10 (03) ◽  
pp. 2050003
Author(s):  
M. R. Hassan ◽  
M. T. Islam ◽  
M. N. I. Khan
Keyword(s):  
Magnetic Properties ◽  
Single Phase ◽  
Low Frequency ◽  
Solid State Reaction Method ◽  
Charge Carriers ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electrical And Magnetic Properties ◽  
Frequency Regime ◽  
Xrd Patterns

In this research, influence of adding Li2CO3 (at 0%, 2%, 4%, 6%) on electrical and magnetic properties of [Formula: see text][Formula: see text]Fe2O4 (with 60% Ni and 40% Mg) ferrite has been studied. The samples are prepared by solid state reaction method and sintered at 1300∘C for 6[Formula: see text]h. X-ray diffraction (XRD) patterns show the samples belong to single-phase cubic structure without any impurity phase. The magnetic properties (saturation magnetization and coercivity) of the samples have been investigated by VSM and found that the higher concentration of Li2CO3 reduces the hysteresis loss. DC resistivity increases with Li2CO3 contents whereas it decreases initially and then becomes constant at lower value with temperature which indicates that the studied samples are semiconductor. The dielectric dispersion occurs at a low-frequency regime and the loss peaks are formed in a higher frequency regime, which are due to the presence of resonance between applied frequency and hopping frequency of charge carriers. Notably, the loss peaks are shifted to the lower frequency with Li2CO3 additions.

Impedance Spectroscopy Study of LiTaO3 Powder Synthesized via Sol-Gel Method

2012 ◽  
Vol 545 ◽  
pp. 275-278 ◽  
Author(s):  
Lili Widarti Zainuddin ◽  
Norlida Kamarulzaman
Keyword(s):  
Room Temperature ◽  
Single Phase ◽  
Sol Gel ◽  
Rhombohedral Structure ◽  
Spectroscopy Study ◽  
X Ray Diffraction ◽  
Gel Method ◽  
X Ray ◽  
Sol Gel Method ◽  
Impedance Spectroscopy Study

A ceramics sample of LiTaO3 was prepared using a sol-gel method. The sample is annealed at 750 °C for 48 hours. X-ray diffraction analysis indicate the formation of single phase, rhombohedral structure. An ac impedance study was used to analyse the conductivity of LiTaO3 at room temperature and at various temperatures.

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

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