Mapping the redox chemistry of common solvents in solvothermal synthesis through in situ X-ray diffraction

Nanoscale ◽  
2020 ◽  
Vol 12 (15) ◽  
pp. 8511-8518 ◽  
Author(s):  
Nils Lau Nyborg Broge ◽  
Frederik Søndergaard-Pedersen ◽  
Martin Roelsgaard ◽  
Xenia Hassing-Hansen ◽  
Bo Brummerstedt Iversen
Keyword(s):  
Solvothermal Synthesis ◽  
Redox Chemistry ◽  
Redox Properties ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solvothermal Conditions

The redox properties of five common solvents under solvothermal conditions are demonstrated through synthesis and characterization of 3d metal based materials.

Synthesis and Characterization of the PANI/ITO Conducting Nanocomposites

2010 ◽  
Vol 663-665 ◽  
pp. 542-545 ◽  
Author(s):  
Bing Jie Zhu ◽  
Xin Wei Wang ◽  
Mei Fang Zhu ◽  
Qing Hong Zhang ◽  
Yao Gang Li ◽  
...  
Keyword(s):  
Doping Concentration ◽  
In Situ Polymerization ◽  
Synthesis And Characterization ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Conductivity ◽  
Scanning Electron

The PANI/ITO conducting nanocomposites have been synthesized by in-situ polymerization. The obtained nanocomposites were characterized by X-ray diffraction pattern, scanning electron microscopy and Fourier transform infrared. Electrical conductivity measurements on the samples pressed into pellets showed that the maximum conductivity attained 2.0 ± 0.05 S/cm for PANI/ITO nanocomposites, at ITO doping concentration of 10 wt%. The results of the present work may provide a simple, rapid and efficient approach for preparing PANI/ITO nanocomposites.

Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter
Keyword(s):  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

Solvothermal Synthesis and Characterization of Lithium Tantalate Nanoparticles

2014 ◽  
Vol 602-603 ◽  
pp. 19-22 ◽  
Author(s):  
Lin Qiang Gao ◽  
Hai Yan Chen ◽  
Zhen Wang ◽  
Xin Zou
Keyword(s):  
Electron Microscopy ◽  
Solvothermal Synthesis ◽  
Room Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Particle Size And Morphology ◽  
Size And Morphology

Nanoscale LiTaO3 powders with perovskite structure were synthesized using the solvothermal technique with glycol as solvent at 240°C for 12h. The powders were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). XRD was used to elucidate room temperature structures using Rietveld refinement. The powders were pure single pervoskite phase with high crystallinity. FESEM and TEM were used to determine particle size and morphology. The average LiTaO3 grain size was estimated to be < 200nm, and TEM images indicated that LiTaO3 particles had a brick-like morphology. In addition, the effect of the temperature on the LiTaO3 power characterisitics was also detailed studied.

Synthesis and Characterization of Copper(II) Complexes with Long Chain Dithiocarbamates

2014 ◽  
Vol 976 ◽  
pp. 164-168 ◽  
Author(s):  
Nayely Torres-Gomez ◽  
Alfredo R. Vilchis-Nestor ◽  
Rosa Maria Gomez-Espinosa ◽  
Ivan Garcia-Orozco
Keyword(s):  
Infrared Spectroscopy ◽  
Copper Complexes ◽  
Nanocrystalline Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Long Chain ◽  
Scanning Electron

Copper complexes of dithiocarbamates ligands were obtained from RNH2 (R = C6H13-, C12H25- y C18H37-) and an excess of CS2 in the presence of NaOH. Sodium hexyldithiocarbamate is not possible to isolate from solution but the other two were obtained and characterizedby infrared spectroscopy, UV-vis and powder X-ray diffraction. Copper complexes were obtained in situ from ligand solution as greenish powders. All the complexes were characterized by infrared spectroscopy, UV-vis, powder X-ray diffraction and Scanning Electron Microscopy. The complexes show an amorphous phase in the case of DCu12 and nanocrystalline structure for DCu18, as observed in XRD.

Synthesis and Characterization of Composite Structure Zeolite Y

2011 ◽  
Vol 233-235 ◽  
pp. 1790-1793 ◽  
Author(s):  
Wei Shen ◽  
Bao Jian Shen
Keyword(s):  
Silica Gel ◽  
Composite Structure ◽  
Zeolite Y ◽  
Synthesis And Characterization ◽  
Organic Additives ◽  
X Ray Diffraction ◽  
Y Zeolite ◽  
X Ray

Y zeolite was synthesized form silica gel microsphere by in- situ hydrothermal method, with appropriate amount of other constituents, such as sodium silicate, water, without adding any organic additives. The as-synthesized samples were characterized using powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and N2 sorption. The results show that the synthesized sample not only has a composite structure with zeolite Y and silica gel, but also retains the shape of silica gel microsphere. The pore distribution of the composite materials indicated that the composite material contains two types of pore that are micropores and large pores.

Solvothermal Synthesis and Characterization of Two Iron Complexes

2011 ◽  
Vol 492 ◽  
pp. 324-327
Author(s):  
Ya Wei Hu ◽  
Yang Min Ma
Keyword(s):  
Solvothermal Synthesis ◽  
Layer Structure ◽  
Iron Complexes ◽  
Synthesis And Characterization ◽  
Molecular Architecture ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Two iron complexes, Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2(1) and Fe(bpy)(Hdtdb)(H2O) (2) were solvothermally synthesized and characterized by single crystal X-ray diffraction. Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2 (1) shows 2D layer structure crystallized in a triclinic with space group P-1 and cell parameters, a = 8.5591(10) nm, b = 11.2502(13) nm, c = 11.4370(14) nm, α = 90.687(2)º, β = 110.275(2)º , γ = 90.712(2)º, and Z = 1. Fe(bpy)(Hdtdb)(H2O) (2) shows surper- molecular architecture crystallized in a triclinic with space group P-1 and cell parameters, a = 8.286(12) nm, b = 11.5937(16) nm, c = 11.8477(17) nm, α = 93.932(3)º, β = 102.442(3)º, γ = 97.117(3)º, and Z = 1.

Solvothermal Synthesis and Characterization of Hierarchical Calcium Carbonate Spheres

2014 ◽  
Vol 912-914 ◽  
pp. 318-320 ◽  
Author(s):  
Yin Xia Chen ◽  
Xian Bing Ji ◽  
Yu Lian Quan
Keyword(s):  
Calcium Carbonate ◽  
Solvothermal Synthesis ◽  
Mixed Solvents ◽  
Average Diameter ◽  
Synthesis And Characterization ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Experimental Parameters

Hierarchical calcium carbonate spheres composed of nanoparticles has been successfully synthesized via a solvothermal process. The structures are fabricated by the reaction of Ca (CH3COO)2with (CO(NH2)2) at 110 °C in diethylene glycolwater mixed solvents in the presence of polyvinylpyrrolidone. The as-prepared products were characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The characterization results revealed that the average diameter of the hierarchical calcium carbonate spheres is about 5 μm, and the size of the nanoparticals range from 50 to 100 nm. In addition, a small amount of bundle-like aragonite calcium carbonate is also obtained in the experimental parameters.

Synthesis and Characterization of New Polyimide/Organoclay Nanocomposites Derived From 3,3′,4,4′-Biphenyltetracarboxylic Dianhydride and 1,2-Bis(4-Aminophenoxy)Ethane

2013 ◽  
Vol 32 (2) ◽  
pp. 171-178 ◽  
Author(s):  
Akram Feyzi ◽  
Khalil Faghihi ◽  
Abdol Ali Zolanvari
Keyword(s):  
Clay Content ◽  
Nanocomposite Films ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Biphenyltetracarboxylic Dianhydride ◽  
Ft Ir Spectroscopy

AbstractA series of nanocomposites consist of organic polyimide and organo-modified clay content varying from 0 to 10 mass%, were successfully prepared by in situ polymerization. Polyimide used as a matrix of nanocomposite was prepared through the reaction of 1,2-bis(4-aminophenoxy)ethane (BAE) and 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA) in N,N-dimethylacetamide (DMAC). The resulting nanocomposite films were characterized by FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA).

Solvothermal Synthesis and Characterization of Zn(NH3)CO3 Single Crystal

2004 ◽  
Vol 817 ◽  
Author(s):  
Fushan Wen ◽  
Jiesheng Chen ◽  
Jin Hyeok Kim ◽  
Taeun Kim ◽  
Wenlian Li
Keyword(s):  
Solvothermal Synthesis ◽  
Room Temperature ◽  
Raw Materials ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Photoluminescent Property ◽  
X Ray ◽  
3 Dimensional ◽  
Zinc Carbonate

AbstractA new 3-dimensional zinc carbonate Zn(NH3)CO3 has been synthesized from a glycol system with urea and zinc acetate as raw materials. The crystal structure and photoluminescent properties have been investigated using X-ray diffraction, smart CCD and FL. The compound had an orthorhombic system with space group of Pna21 with M = 142.41, a = 9.1449(18) Å, b = 7.5963(15) Å, c = 5.4982(11) Å, V = 381.95(13) Å3, Z = 4, R = 0.0285 and RW = 0.0745. The NH3 and CO32- were connected through the Zn-N bond and Zn-O bond in the symmetric unit. Photoluminescent property was observed in the compound at room temperature and the exited and emission peaks were located at about 350 nm and 426 nm, respectively.

Study of Cellulose-Dibutyl Sebacate Copolymer Synthesis and Characterization of Crosslinked Cellulose-Dibutyl Sebacate Copolymers for Oil Absorbency

2011 ◽  
Vol 311-313 ◽  
pp. 2075-2083
Author(s):  
Halidan Mamat
Keyword(s):  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Reaction Conditions ◽  
X Ray ◽  
Oil Absorbency ◽  
Dibutyl Sebacate ◽  
Oil Absorbent

A novel cellulose-based oil absorbent crosslinked cellulose-dibutyl sebacate copolymers was prepared by the graft crosslinking polymerization of in situ synthesized dibutyl sebacate and cotton cellulose using potassium persulfate as an initiator. The copolymers were characterized by infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetry, differential scanning calorimetry, etc. The effects of reaction conditions, such as, ratio of reaction regents, reaction temperature, reaction time, etc, on the efficiency of oil absorbency were examined. The optimized reaction conditions for the synthesis of crosslinked cellulose-dibutyl sebacate copolymers were: m(cotton pulp):m(K2S2O8 initiator):m(dibutyl sebacate) = 1 0.025 2.0(W/W)，75°C，and 5-6 h. The resulting crosslinked cellulose-dibutyl sebacate copolymers were floppy and exhibited excellent oil absorbency efficiency.

Sign in / Sign up

Export Citation Format

Share Document