Study of the phase composition of Fe2O3 and Fe2O3/TiO2 nanoparticles using X-ray diffraction and Debye formula

2010 ◽  
Vol 7 (5) ◽  
pp. 1399-1404 ◽  
Author(s):  
Václav Valeš ◽  
Jana Poltierová-Vejpravová ◽  
Václav Holý ◽  
Václav Tyrpekl ◽  
Petr Brázda ◽  
...  
2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


2019 ◽  
Vol 484 (1) ◽  
pp. 41-43
Author(s):  
E. A. Malinina ◽  
V. K. Skachkova ◽  
I. V. Kozerozhets ◽  
V. V. Avdeeva ◽  
L. V. Goeva ◽  
...  

The method of nanoscaled sodium dodecahydro-closo-dodecaborate Na2[B12H12] synthesis is presented. The composite is heated to 200°C to yield the desired product, forming with the introduction of triethyl- ammonium salt [Et3NH]2[B12H12] into the silicate matrix of a sodium liquid glass. The morphology and phase composition of the synthesized sample are studied through SEM and X-ray diffraction methods, in comparison to those of a standard salt sample Na2[B12H12]. Based on the obtained data, the sample under study is an amorphous composite, on the surface of which nanoscale crystals of Na2[B12H12] form.


2004 ◽  
Vol 37 (6) ◽  
pp. 967-976 ◽  
Author(s):  
Andrew C. Jupe ◽  
Stuart R. Stock ◽  
Peter L. Lee ◽  
Nikhila N. Naik ◽  
Kimberly E. Kurtis ◽  
...  

Spatially resolved energy dispersive X-ray diffraction, using high-energy synchrotron radiation (∼35–80 keV), was used nondestructively to obtain phase composition profiles along the radii of cylindrical cement paste samples to characterize the progress of the chemical changes associated with sulfate attack on the cement. Phase distributions were acquired to depths of ∼4 mm below the specimen surface with sufficient spatial resolution to discern features less than 200 µm thick. The experimental and data analysis methods employed to obtain quantitative composition profiles are described. The spatial resolution that could be achieved is illustrated using data obtained from copper cylinders with a thin zinc coating. The measurements demonstrate that this approach is useful for nondestructively visualizing the sometimes complex transformations that take place during sulfate attack on cement-based materials. These transformations can be spatially related to microstructure as seen by computed microtomography.


2013 ◽  
Vol 710 ◽  
pp. 170-173
Author(s):  
Lian Ping Chen ◽  
Yuan Hong Gao

It is hardly possible to obtain rare earth doped CaWO4thin films directly through electrochemical techniques. A two-step method has been proposed to synthesize CaWO4:(Eu3+,Tb3+) thin films at room temperature. X-ray diffraction, energy dispersive X-ray analysis, spectrophotometer were used to characterize their phase, composition and luminescent properties. Results reveal that (Eu3+,Tb3+)-doped CaWO4films have a tetragonal phase. When the ratio of n (Eu)/n (Tb) in the solution is up to 3:1, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Tb element; on the contrary, when the ratio in the solution is lower than 1:4, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Eu element. Under the excitation of 242 nm, sharp emission peaks at 612, 543, 489 and 589 nm have been observed for CaWO4:(Eu3+,Tb3+) thin films.


2017 ◽  
Vol 17 (2) ◽  
pp. 107-110
Author(s):  
K. Stec ◽  
J. Podwórny ◽  
B. Psiuk ◽  
Ł. Kozakiewicz

Abstract Using the available analytical methods, including the determination of chemical composition using wavelength-dispersive X-ray fluorescent spectroscopy technique and phase composition determined using X-ray diffraction, microstructural observations in a highresolution scanning microscope equipped with an X-ray microanalysis system as well as determination of characteristic softening and sintering temperatures using high-temperature microscope, the properties of particular chromite sands were defined. For the study has been typed reference sand with chemical properties, physical and thermal, treated as standard, and the sands of the regeneration process and the grinding process. Using these kinds of sand in foundries resulted in the occurrence of the phenomenon of the molding mass sintering. Impurities were identified and causes of sintering of a moulding sand based on chromite sand were characterized. Next, research methods enabling a quick evaluation of chromite sand suitability for use in the preparation of moulding sands were selected.


2017 ◽  
Vol 12 (1) ◽  
pp. 63-77 ◽  
Author(s):  
Siriporn Sirikingkaew ◽  
Nuta Supakata

This study presents the development of geopolymer bricks synthetized from industrial waste, including fly ash mixed with concrete residue containing aluminosilicate compound. The above two ingredients are mixed according to five ratios: 100:0, 95:5, 90:10, 85:15, and 80:20. The mixture's physico-mechanical properties, in terms of water absorption and the compressive strength of the geopolymer bricks, are investigated according to the TIS 168-2546 standard. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses are used to investigate the microstructure and the elemental and phase composition of the brick specimens. The results indicate that the combination of fly ash and concrete residue represents a suitable approach to brick production, as required by the TIS 168–2546 standard.


2021 ◽  
Vol 1016 ◽  
pp. 1790-1796
Author(s):  
Maxim Syrtanov ◽  
Egor Kashkarov ◽  
Tatyana Murashkina ◽  
Nahum Travitzky

This paper describes the influence of sintering temperature on phase composition and microstructure of paper-derived Ti3AlC2 composites fabricated by spark plasma sintering. The composites were sintered at 100 MPa pressure in the temperature range of 1150-1350 °C. Phase composition and microstructure were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The multiphase structure was observed in the sintered composites consisting of Ti3AlC2, Ti2AlC, TiC and Al2O3 phases. The decomposition of the Ti3AlC2 phase into Ti2AlC and TiC carbide phases was observed with temperature rise. The total content of Ti3AlC2 and Ti2AlC phases was reduced from 84.5 vol.% (1150 °C) to 69.5 vol.% (1350 °C). The density of composites affected by both the content of TiC phase and changes in porosity.


Materials ◽  
2019 ◽  
Vol 12 (24) ◽  
pp. 4171 ◽  
Author(s):  
Paweł Rutkowski ◽  
Jan Huebner ◽  
Adrian Graboś ◽  
Dariusz Kata ◽  
Dariusz Grzybek ◽  
...  

In this study, the influence of the addition of rare earth oxides on the phase composition and density of KNN piezoelectric ceramics was investigated. The initial powders of Na2CO3 and K2CO3 were dried at 150 °C for 2 h. Then, a powder mixture for synthesis was prepared by adding a stoichiometric amount of Nb2O5 and 5 and 10 wt % overabundance of Na2CO3. All powders were mixed by ball-milling for 24 h and synthesized at 950 °C. The phase composition of the reaction bed was checked by means of X-ray diffraction (XRD). It had an appearance of tetragonal and monoclinic K0.5Na0.5NbO3 (KNN) phases. Then, 1 and 2 wt % of Er2O3 and Yb2O3, were added to the mixture. Green samples of 25 mm diameter and 3 mm thickness were prepared and sintered by hot pressing at 1000 °C for 2 h under 25 MPa pressure. The final samples were investigated via scanning electron microscopy (SEM)-energy-dispersive X-ray spectroscopy (EDS), XRD, Rietveld, and ultrasonic methods. Phase analysis showed tetragonal and orthorhombic KNN phases, and a contamination of (K2CO3·1.5H2O) was present. The obtained KNN polycrystals had a relative density above 95%. Texturing of the material was confirmed as a result of hot pressing.


2018 ◽  
Vol 34 (6) ◽  
pp. 3140-3144
Author(s):  
Ritu Vershney ◽  
Komal Chelaramani ◽  
Arpan Bhardwaj ◽  
Nayma Siddiqui ◽  
Suresh Kumar Verma

The synthesis of Ni doped titania (TiO2) nanoparticles were achieved via simple novel sol gel technique, in which Titanium-n-butoxide and NiCl2 were taken as precursors. Effect of different wt% of dopant in TiO2 was studied on photocatalytic degradation of Aniline blue and Toluidine Blue. The study suggested the increased photocatalytic degradation with increased time duration. The synthesized samples were analyzed by surface electron microscopy (SEM) and X-ray diffraction studies. The antibacterial activity was investigated against Gram-positive Staphylococcus aureus bacteriae. Studies revealed that on increasing the dopant concentration, the diameter of zone of inhibition also increased upto 1.5 wt%.


Materials ◽  
2019 ◽  
Vol 12 (17) ◽  
pp. 2817 ◽  
Author(s):  
Feng Zhan ◽  
Lei Xiong ◽  
Fang Liu ◽  
Chenying Li

In this study, we proposed a novel and facile method to modify the surface of TiO2 nanoparticles and investigated the influence of the surface-modified TiO2 nanoparticles as an additive in a polyurethane (PU) coating. The hyperbranched polymers (HBP) were grafted on the surface of TiO2 nanoparticles via the thiol-yne click chemistry to reduce the aggregation of nanoparticles and increase the interaction between TiO2 and polymer matrices. The grafting of HBP on the TiO2 nanoparticles surface was investigated by means of X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Fourier transform infrared (FT-IR), nuclear magnetic resonance (NMR) and thermogravimetry analysis (TGA). The thermal and mechanical properties of nanocomposite coatings containing various amounts of TiO2 nanoparticles were measured by dynamic mechanical thermal (DMTA) and tensile strength measurement. Moreover, the surface structure and properties of the newly prepared nanocomposite coatings were examined. The experimental results demonstrate that the incorporation of the surface-modified TiO2 nanoparticles can improve the mechanical and thermal properties of nanocomposite coatings. The results also reveal that the surface modification of TiO2 with the HBP chains improves the nanoparticle dispersion, and the coating surface shows a lotus leaf-like microstructure. Thus, the functional nanocomposite coatings exhibit superhydrophobic properties, good photocatalytic depollution performance, and high stripping resistance.


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