scholarly journals Synthesis and Characterization of PVP-Stabilized Palladium Nanoparticles by XRD, SAXS, SP-ICP-MS, and SEM

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Katharina Walbrück ◽  
Fabian Kuellmer ◽  
Steffen Witzleben ◽  
Klaus Guenther

Due to increased emissions of palladium nanoparticles in recent years, it is important to develop analytical techniques to characterize these particles. The synthesis of defined and stable particles plays a key role in this process, as there are not many materials commercially available yet which could act as reference materials. Polyvinylpyrrolidone- (PVP-) stabilized palladium nanoparticles were synthesized through the reduction of palladium chloride by tetraethylene glycol (TEG) in the presence of KOH. Four different methods were used for particle size analysis of the palladium nanoparticles. Palladium suspensions were analyzed by scanning electron microscopy (SEM), small angle X-ray scattering (SAXS), single-particle ICP-MS (SP-ICP-MS), and X-ray diffraction (XRD). Secondary particles between 30 nm and 130 nm were detected in great compliance with SAXS and SP-ICP-MS. SEM analysis showed that the small particulates tend to form agglomerates.

2020 ◽  
Author(s):  
Xiaojian Bai ◽  
Chen Jia ◽  
Zhigen Chen ◽  
Yuxuan Gong ◽  
Huwei Cheng ◽  
...  

Abstract The painted statues of Tutang Buddha and two attendants Buddha in Jingyin Temple, with exquisite design and unique style, are precious cultural heritages of China. The statue of Tutang Buddha which was carved from a mound and painted by ancient craftsmen, is rarely found in ancient China. However, on account of the influence of natural factors and artificial harms, the statues were severly damaged. Obviously, it requires urgently carrying out appropriate protection and restoration of the statues. In this study, the samples taken from the statues were analysed by multiple analytical techniques, including scanning electron microscopy with energy dispersive spectrometry (SEM-EDS), Raman spectroscopy, X-ray diffraction (XRD), biological microscopy and particle size analysis. The analysis enabled us to infer the techniques used by the creators in making the statues. This research provides reliable evidence for the conservation and future protection of these and similar statues.


2011 ◽  
Vol 699 ◽  
pp. 153-165
Author(s):  
M. Ambika ◽  
R. Saravanan

In this work, lead sulphide has been characterized using X- ray diffraction, SEM, EDX and UV-Visible techniques. X-ray analysis is done by using the Rietveld refinement method of matching the observed and calculated profiles, and then the results obtained from the refinement process are used in finding the electron density distribution by using maximum entropy method (MEM). The local structure analysis of PbS is done by the pair distribution function (PDF). Particle size analysis is done with the use of XRD data, SEM analysis is done in finding the surface structure and EDX in finding the elemental composition of PbS sample. The energy gap of PbS is found from UV-Visible spectrum.


2021 ◽  
Author(s):  
Othman Y Alothman ◽  
H.M. Shaikh ◽  
Basheer A. Alshammari ◽  
Mohammad Jawaid

Abstract In this century, the development of nano-sized filler from biomass material has become the main focus of industries in achieving their final green composite product for wide range of applications. From commercial and environmental point of view, fragmentation and downsizing of waste lignocellulosic fibers without chemical treatments into small size particles is a viable option. In this study, an attempt was made to produce nano-sized lignocellulosic fillers from date palm micro fibers via simple mechanical ball milling process. The resultant nanofillers as well as the microfibers were characterized in details by various analytical techniques, including transmission electron microscopy (TEM), scanning electron microscopy (SEM), particle size analysis (PSA), Energy Dispersive X-Ray (EDX), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) to assess their structure­—property relationship. From microscopy examination, the nanofillers showed a heterogeneous mix of irregular shaped particles, and while having a size ranging of 30-110 nm in width and 1-10 mm length dimensions. Also, the crystallography analysis revealed the crystallinity had mildly declined from microfibers (71.8%) to nanofiller (68.9%) due to amorphization effect. As for thermal analysis, the nanofillers exhibited relatively stable in both heat resistance and thermos changing behavior, suggesting its suitability for composite fabrication process at high temperature. Thus, the produced nanofillers can be used as a low cost reinforcing agent in the future for versatile polymer-based composite systems.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 232
Author(s):  
Pedro J. Sánchez-Soto ◽  
Eduardo Garzón ◽  
Luis Pérez-Villarejo ◽  
George N. Angelopoulos ◽  
Dolores Eliche-Quesada

In this work, an examination of mining wastes of an albite deposit in south Spain was carried out using X-ray Fluorescence (XRF), X-ray diffraction (XRD), particle size analysis, thermo-dilatometry and Differential Thermal Analysis (DTA) and Thermogravimetric (TG) analysis, followed by the determination of the main ceramic properties. The albite content in two selected samples was high (65–40 wt. %), accompanied by quartz (25–40 wt. %) and other minor minerals identified by XRD, mainly kaolinite, in agreement with the high content of silica and alumina determined by XRF. The content of Na2O was in the range 5.44–3.09 wt. %, being associated with albite. The iron content was very low (<0.75 wt. %). The kaolinite content in the waste was estimated from ~8 to 32 wt. %. The particle size analysis indicated values of 11–31 wt. % of particles <63 µm. The ceramic properties of fired samples (1000–1350 °C) showed progressive shrinkage by the thermal effect, with water absorption and open porosity almost at zero at 1200–1250 °C. At 1200 °C, the bulk density reached a maximum value of 2.38 g/cm3. An abrupt change in the phase evolution by XRD was found from 1150 to 1200 °C, with the disappearance of albite by melting in accordance with the predictions of the phase diagram SiO2-Al2O3-Na2O and the system albite-quartz. These fired materials contained as main crystalline phases quartz and mullite. Quartz was present in the raw samples and mullite was formed by decomposition of kaolinite. The observation of mullite forming needle-shape crystals was revealed by Scanning Electron Microscopy (SEM). The formation of fully densified and vitrified mullite materials by firing treatments was demonstrated.


2010 ◽  
Vol 61 (5) ◽  
pp. 1235-1243 ◽  
Author(s):  
Y. F. He ◽  
F. R. Li ◽  
R. M. Wang ◽  
F. Y. Li ◽  
Y. Wang ◽  
...  

Xanthate was successfully grafted onto bentonite by a relatively simple solution reaction. The obtained xanthated bentonite (XBent) was characterized by FT-IR spectrophotometer, thermogravimetric analysis (TG), particle size analysis, x-ray diffraction (XRD) and scanning electron microscopy (SEM). XBent acting as a type of environmentally friendly adsorbent was applied to remove lead ions from aqueous solutions. The optimum conditions were as follows: [Pb2 + ] = 500 mg L−1, [XBent] = 2 g L−1, pH = 5.0; oscillating 60 min under 200 rpm at 25°C. The removal rate of lead was up to 99.9%. It was found that the lead(II) ions—XBent adsorption isotherm model fitted well to the Freundlich isotherm. The adsorption mechanism was also investigated by SEM and XRD, which concluded that lead ions were complexed or chelated with XBent. XBent appears to have potential to be used later in water treatment as a type of inorganic polymer reagent.


Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1413
Author(s):  
Rafał Panek ◽  
Jarosław Madej ◽  
Lidia Bandura ◽  
Grzegorz Słowik

Nowadays, using fly ash for zeolites production has become a well-known strategy aimed on sustainable development. During zeolite synthesis in a hydrothermal conversion large amount of post-reaction solution is generated. In this work, the solution was used as a substrate for Na-A and Na-X zeolites synthesis at laboratory and technical scale. Obtained materials were characterized using particle size analysis, X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), transmission electron microscopy (TEM), Fourier transformed infrared spectroscopy (FTIR), and nitrogen adsorption/desorption isotherm. Produced zeolites revealed high purity (>98%) and monomineral zeolitic phase composition. The SiO2 content was in the range 39–42% and 40–38%, whereas Al2O3 content was 23–22% and 25–26% for Na-X and Na-A, respectively. TEM and BET analyses revealed Na-X zeolite pores were almost identical to commercial 13X with SBET in the range 671–734 m2/g. FTIR indicated slight differences between materials obtained at laboratory and technical scale in Si-O-(Si/Al) bridges of the zeolitic skeleton. The results showed good replicability of the laboratory process in the larger scale. The proposed method allows for waste solution reusability with a view to highly pure zeolites production in line with circular economy assumptions.


2012 ◽  
Vol 727-728 ◽  
pp. 1164-1169 ◽  
Author(s):  
Mônica Beatriz Thürmer ◽  
Rafaela Silveira Vieira ◽  
Juliana Machado Fernandes ◽  
Wilbur Trajano Guerin Coelho ◽  
Luis Alberto Santos

Calcium phosphate cements have bioactivity and osteoconductivity and can be molded and replace portions of bone tissue. The aim of this work was to study the obtainment of α-tricalcium phosphate, the main phase of calcium phosphate cement, by wet reaction from calcium nitrate and phosphoric acid. There are no reports about α-tricalcium phosphate obtained by this method. Two routes of chemical precipitation were evaluated and the use of two calcinations temperatures to obtain the phase of cement. The influence of calcination temperature on the mechanical properties of cement was evaluated. Cement samples were characterized by particle size analysis, X-ray diffraction, mechanical strength and scanning electron microscopy. The results demonstrate the strong influence of synthesis route on the crystalline phases of cement and the influence of concentration of reactants on the product of the reaction, as well as, on the mechanical properties of cement.


2021 ◽  
Author(s):  
Maame Croffie ◽  
Paul N. Williams ◽  
Owen Fenton ◽  
Anna Fenelon ◽  
Karen Daly

&lt;p&gt;Soil texture is an essential factor for effective land management in agricultural production. Knowledge of soil texture and particle size at field scale can aid with on-going soil management decisions. Standard soil physical and gravimetric methods for particle size analysis are time-consuming and X-ray fluorescence spectrometry (XRF) provides a rapid and cost-effective alternative. The objective of this study was to explore the use of XRF as a predictor for particle size. An extensive archive of Irish soils with particle size and soil texture data was used to select samples for XRF analysis. Regression and correlation analyses on XRF determined results showed that the relationship between Rb and % clay varied with soil type and was dependent on the parent material. There was a strong relationship (R &gt; 0.62, R&lt;sup&gt;2&lt;/sup&gt;&gt;0.30, p&lt;0.05) between Rb and clay for soils originating from bedrock such as limestones and slate. Contrastingly, no significant relationship (R&lt;0.03, R&lt;sup&gt;2&lt;/sup&gt;=0.00, p&gt;0.05) exists between Rb and % clay for soils originating from granite and gneiss. Furthermore, there was a significant negative correlation (p&lt;0.05) between Rb and % sand. The XRF is a useful technique for rough screening of particle size distribution in soils originating from certain parent materials. Thus, this may contribute to the rapid prediction of soil texture based on knowledge of the particle size distribution.&lt;/p&gt;&lt;p&gt;&amp;#160;&lt;/p&gt;


Author(s):  
Fredy Kurniawan ◽  
Rahmi Rahmi

SnO2 nanoparticles have been synthesized by high voltage electrolysis. Tin bare was used for anode and cathode. The effect of potentials and electrolyte were studied. The particles obtained after electrolysis was characterized using X-ray Diffraction (XRD). The diffractogram is in agreement with the standard diffraction pattern of SnO2 which is identified as tetragonal structure. The Fourier Transform Infrared (FTIR) spectrum indicates that there is a vibration of Sn–O asymmetric at 580 cm-1. The optimum potential for SnO2 nanoparticles synthesis is 60 V at 0.06 M HCl which shows the highest UV-Vis spectrum. The absorption peak of SnO2 nanoparticles by UV-Vis spectrophotometer appears at about 207 nm. The particle size analysis shows that the SnO2 nanoparticles obtained have the size distribution in a range of 25-150 nm with the highest volume at 83.11 nm. Copyright © 2017 BCREC Group. All rights reservedReceived: 15th November 2016; Revised: 26th February 2017; Accepted: 27th February 2017How to Cite: Rahmi, R., Kurniawan, F. (2017). Synthesis of SnO2 Nanoparticles by High Potential Electrolysis. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (2): 281-286 (doi:10.9767/bcrec.12.2.773.281-286)Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.2.773.281-286 


1989 ◽  
Vol 169 ◽  
Author(s):  
Rollin E. Lakis ◽  
Sidney R. Butler

AbstractY1Ba2Cu3O7 has been prepared by the evaporative decomposition of solutions method. Nitrate and mixed anion solutions were atomized and decomposed at temperatures ranging from 300°C to 950°C. The resulting materials have been characterized using x-ray powder diffraction, Thermal Gravimetric Analysis (TGA), particle size analysis, Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The powder consists of 0.3 micron agglomerated hollow spheres with a primary particle size of 0.06 micron. TGA and x-ray diffraction indicate the presence of barium nitrate and barium carbonate due to incomplete decomposition and/or product contamination by the process environment.


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