Synthesis and Characterisation of Titania Nanotubes: Effect of Phase and Crystallite Size on Nanotube Formation

2007 ◽  
Vol 29-30 ◽  
pp. 211-214 ◽  
Author(s):  
D.L. Morgan ◽  
E.R. Waclawik ◽  
R.L Frost

Nanotubes were produced from commercial and self-prepared anatase and rutile which were treated with 7.5 M NaOH over a temperature range of 100 – 200°C in 20°C increments. The formation of nanotubes was examined as a function of starting material type and size. Products were characterised by X-Ray Diffraction (XRD), Transmission Electron Spectroscopy (TEM), and Raman Spectroscopy. The results indicated that both phase and crystallite size affected the nanotube formation. Rutile was observed to require a greater driving force than anatase to form nanotubes, and increases in crystallite sizes appeared to impede formation slightly.

1998 ◽  
Vol 13 (10) ◽  
pp. 2920-2931 ◽  
Author(s):  
Youn Joong Kim ◽  
Waltraud M. Kriven

The crystallography, microstructures, and phase transformation mechanisms in dysprosia (Dy2O3) have been studied. The lattice parameters of B and C phases were refined by x-ray diffraction (XRD). The modulated structures and decomposed structures in the CaO-doped samples were characterized by transmission electron spectroscopy (TEM). A new twin was observed in the modulated B phase. Contrary to the previous studies, the B to C transformation was induced by grinding. The A to B transformation was considered to be ferroelastic and the spontaneous strain was calculated. The major driving force for the B (monoclinic) to C (cubic) transformation is suggested to be the release of lattice strains and cation charge repulsions in the B structure, which is analogous to the β (monoclinic) to γ (orthorhombic) transformation in Ca2SiO4. This transformation can be displacive, if some conditions are provided to overcome the bonding energy of the interlayer oxygens in the B structure.


2022 ◽  
Vol 8 (1) ◽  
pp. 4
Author(s):  
Petros Kasaira Mubari ◽  
Théotime Beguerie ◽  
Marc Monthioux ◽  
Elsa Weiss-Hortala ◽  
Ange Nzihou ◽  
...  

Structural properties of carbonized cellulose were explored to conjugate the outcomes from various characterization techniques, namely X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy. All these techniques have evidenced the formation of graphene stacks with a size distribution. Cellulose carbonized at 1000 and 1800 °C at a heating rate of 2 °C/min showed meaningful differences in Raman spectroscopy, whereas in XRD, the differences were not well pronounced, which implies that the crystallite sizes calculated by each technique have different significations. In the XRD patterns, the origin of a specific feature at a low scattering angle commonly reported in the literature but poorly explained so far, was identified. The different approaches used in this study were congruous in explaining the observations that were made on the cellulose-derived carbon samples. The remnants of the basic structural unit (BSU) are developed during primary carbonization. Small graphene-based crystallites inherited from the BSUs, which formerly developed during primary carbonization, were found to coexist with larger ones. Even if the three techniques give information on the average size of graphenic domains, they do not see the same characteristics of the domains; hence, they are not identical, nor contradictory but complementary. The arguments developed in the work to explain which characteristics are deduced from the signal obtained by each of the three characterization techniques relate to physics phenomena; hence, they are quite general and, therefore, are valid for all kind of graphenic materials.


Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


2015 ◽  
Vol 68 (8) ◽  
pp. 1293 ◽  
Author(s):  
Pakvipar Chaopanich ◽  
Punnama Siriphannon

Hydroxyapatite (HAp) nanoparticles were successfully synthesized from an aqueous mixture of Ca(NO3)2·4H2O and (NH4)2HPO4 by a facile single-step refluxing method using polystyrene sulfonate (PSS) as a template. The effects of reaction times, pH, and PSS concentration on the HAp formation were investigated. It was found that the crystalline HAp was obtained under all conditions after refluxing the precursors for 3 and 6 h. The longer refluxing time, the greater the crystallinity and the larger the crystallite size of the HAp nanoparticles. The HAp with poor crystallinity was obtained at pH 8.5; however, the well-crystallized HAp was obtained when reaction pH was increased to 9.5 and 10.5. In addition, the X-ray diffraction patterns revealed that the presence of PSS template caused the reduction of HAp crystallite size along the (002) plane from 52.6 nm of non-template HAp to 43.4 nm and 41.4 nm of HAp with 0.05 and 0.2 wt-% PSS template, respectively. Transmission electron microscopy images of the synthesized HAp revealed the rod-shaped crystals of all samples. The synthesized HAp nanoparticles were modified by l-aspartic acid (Asp) and l-arginine (Arg), having negative and positive charges, respectively. It was found that the zeta potential of HAp was significantly changed from +5.46 to –24.70 mV after modification with Asp, whereas it was +4.72 mV in the Arg-modified HAp. These results suggested that the negatively charged amino acid was preferentially adsorbed onto the synthesized HAp surface.


1997 ◽  
Vol 3 (4) ◽  
pp. 381-396
Author(s):  
S. Chandra ◽  
D. Van Gemert

Abstract Interior plaster from the Abbot's Palace of the Abbey of Villers-la-Ville, Brabant Wallon province, Belgium has been investigated. It is done by using chemical analysis, x-ray diffraction analysis, scanning electron microscopy, energy dispersive electron spectroscopy, and transmission electron microscopy. It is found that the rendering was made with lime rich mortar and animal hairs. The sand used was very fine and the hairs were very short. The solid constituents and the hairs were uniformly dispersed, which could have been obtained by the addition of some other natural polymer, containing protein.


2018 ◽  
Vol 32 (19) ◽  
pp. 1840044
Author(s):  
Aditya Dalal ◽  
Animesh Mandal ◽  
Shubhada Adhi ◽  
Kiran Adhi

Aluminum (0.5 at.%)-doped ZnO (AZO) thin films were deposited by pulsed laser deposition technique (PLD) in oxygen ambient of 10[Formula: see text] Torr. The deposited thin films were characterized by x-ray diffraction (XRD), photoluminescence (PL), Raman spectroscopy and uv–visible spectroscopy (UV–vis). Next, graphene oxide (GO) was synthesized by Hummers method and was characterized by XRD, UV–vis spectroscopy, Raman spectroscopy and transmission electron microscopy (TEM). Thereafter, GO solution was drop-casted on AZO thin films. These films were then characterized by Raman Spectroscopy, UV–vis spectroscopy and PL. Attempt is being made to comprehend the modifications in properties brought about by integration.


Clay Minerals ◽  
2018 ◽  
Vol 53 (3) ◽  
pp. 471-485 ◽  
Author(s):  
Angel Sanz ◽  
Joaquín Bastida ◽  
Angel Caballero ◽  
Marek Kojdecki

ABSTRACTCompositional and microstructural analysis of mullites in porcelain whitewares obtained by the firing of two blends of identical triaxial composition using a kaolin B consisting of ‘higher-crystallinity’ kaolinite or a finer halloysitic kaolin M of lower crystal order was performed. No significant changes in the average Al2O3 contents (near the stoichiometric composition 3:2) of the mullites were observed. Fast and slow firing at the same temperature using B or M kaolin yielded different mullite contents. The Warren–Averbach method showed increase of the D110 mullite crystallite size and crystallite size distributions with small shifts to greater values with increasing firing temperature for the same type of firing (slow or fast) using the same kaolin, as well as significant differences between fast and slow firing of the same blend at different temperatures for each kaolin. The higher maximum frequency distribution of crystallite size observed at the same firing temperature using blends with M kaolin suggests a clearer crystallite growth of mullite in this blend. The agreement between thickening perpendicular to prism faces and mean crystallite sizes <D110> of mullite were not always observed because the direction perpendicular to 110 planes is not preferred for growth.


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