Preparation and characterization of uniform submicrometer metal niobate particles. I. Lead niobate

1991 ◽  
Vol 6 (4) ◽  
pp. 840-850 ◽  
Author(s):  
Myung Jin Kim ◽  
Egon Matijević

Colloidal amorphous lead niobate particles of different composition and morphologies were obtained by a metal-chelate decomposition method. The nature of the dispersions depended on the conditions of the preparation of the complexes, pH, aging time, and temperature. The structural and chemical changes of the so prepared powders on calcination were investigated by thermal and x-ray diffraction analyses. Chemical mechanisms of the formation and transformation of the particles are suggested.

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Changyu Li ◽  
Shouxin Liu

Mesoporous nanosheets of single-crystallineβ-nickel hydroxide (β-Ni(OH)2) were successfully synthesized via a facile hydrothermal method using Ni(NO3)2 · 6H2O as precursor in a mixed solution of sodium hydroxide (NaOH) and sodium dodecylbenzenesulfonate (SDBS). Single-crystalline nickel oxide (NiO) mesoporous nanosheets can be obtained through a thermal decomposition method usingβ-Ni(OH)2mesoporous nanosheets as precursor. The influences of SDBS and hydrothermal treatment were carefully investigated; the results showed that they played important roles in the formation ofβ-Ni(OH)2mesoporous nanosheets. The as-obtainedβ-Ni(OH)2and NiO were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal gravity-differential thermal analysis (TG-DTA), and specific surface area, and pore size test.


2012 ◽  
Vol 1418 ◽  
Author(s):  
Kubra Celik ◽  
Celaletdin Ergun ◽  
Huseyin Kizil

ABSTRACTIn this study, Ag doped hydroxyapatite (HA) samples prepared by EDTA chelate decomposition method were characterized with X-Ray Diffraction Spectroscopy (XRD), Scanning Electron Microscopy (SEM) and antimicrobial sensitivity test. Hydroxyapatite (Ca10(PO)6(OH)2) and NaCaPO4 (rhenanite) phases were observed while Ag was present in the form of Ag2O. Results showed that microstructurally controlled HA-based composites with NaCaPO4 interphase can be prepared, which significantly enhances sinterability of hydroxyapatite at 1100° C without formation of any undesired second phases, such as tricalcium phosphate (TCP) known to decrease the stability of HA. The antibacterial sensitivity was tested with E.Coli gram-negative bacteria. The radius of circle enclosing the sample increases with increasing Ag content in the structure as an indication of the region of non-bacterial activity.


2020 ◽  
Vol 52 (2) ◽  
pp. 219-229
Author(s):  
Marija Ivanovic ◽  
Ljiljana Kljajevic ◽  
Jelena Gulicovski ◽  
Marijana Petkovic ◽  
Ivona Jankovic-Castvan ◽  
...  

This paper outlines the production of an inorganic polymer/geopolymer using a metakaolin by an environmental friendly, energy saving, clean technology to conserve natural environment and resources. The influence of alkali activation, i.e. different concentration of NaOH as a component of alkali activator mixture on the process of geopolymerization of metakaolin is investigated. Also, process of aging time of geopolymer is followed by several analytical methods. The structure of metakaolin and metakaolin based geopolymers and their physicochemical properties were studied using X-ray diffraction (XRD), Fourier transformation infrared spectroscopy (FTIR) and after 28days scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) was applied for the surface characterization of the samples. A shift of the Si-O or Si-O-X (X=Al, Si, Na...) bands as the molarity of activator increasing during geopolymerization process was observed by FTIR. Mass spectra of geopolymers were characterized by MALDI TOF mass spectrometer. Structural reorganization of geopolymer samples occurs during the curing/aging in accordance with a geopolymerization mechanism.


Author(s):  
R. E. Herfert

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.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.


2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.


Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.


Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2160
Author(s):  
Alexander Bogdanov ◽  
Ekaterina Kaneva ◽  
Roman Shendrik

Elpidite belongs to a special group of microporous zirconosilicates, which are of great interest due to their capability to uptake various molecules and ions, e.g., some radioactive species, in their structural voids. The results of a combined electron probe microanalysis and single-crystal X-ray diffraction study of the crystals of elpidite from Burpala (Russia) and Khan-Bogdo (Mongolia) deposits are reported. Some differences in the chemical compositions are observed and substitution at several structural positions within the structure of the compounds are noted. Based on the obtained results, a detailed crystal–chemical characterization of the elpidites under study was carried out. Three different structure models of elpidite were simulated: Na2ZrSi6O15·3H2O (related to the structure of Russian elpidite), partly Ca-replaced Na1.5Ca0.25ZrSi6O15·2.75H2O (close to elpidite from Mongolia), and a hypothetical CaZrSi6O15·2H2O. The vibration spectra of the models were obtained and compared with the experimental one, taken from the literature. The strong influence of water molecule vibrations on the shape of IR spectra of studied structural models of elpidite is discussed in the paper.


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