Tensile stress effect on epitaxial BiFeO 3 thin film grown on KTaO 3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bae, In-Tae; Ichinose, Tomohiro; Han, Myung-Geun

Comprehensive crystal structural study is performed for BiFeO 3 (BFO) film grown on KTaO 3 (KTO) substrate using transmission electron microscopy (TEM) and x-ray diffraction (XRD). Nano beam electron diffraction (NBED) combined with structure factor calculation and high resolution TEM images clearly reveal that the crystal structure within BFO thin film is rhombohedral BFO, i.e., bulk BFO phase. Epitaxial relationship found by NBED indicates the BFO film grows in a manner that minimizes lattice mismatch with KTO. It further suggests BFO film is under slight biaxial tensile stress (~0.35%) along in-plane direction. XRD reveals BFO lattice is under compressive stressmore » (~1.6%), along out-of-plane direction as a result of the biaxial tensile stress applied along in-plane direction. This leads to Poisson’s ratio of ~0.68. In addition, we demonstrate (1) why hexagonal notation rather than pseudocubic one is required for accurate BFO phase evaluation and (2) a new XRD method that shows how rhombohedral BFO can readily be identified among other phases by measuring a rhombohedral specific Bragg’s peak.« less

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

Ostwald ripening and interparticle-diffraction effects for illite crystals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.

1988-01-01

The Warren-Averbach method, an X-ray diffraction (XRD) method used to measure mean particle thickness and particle-thickness distribution, is used to restudy sericite from the Silverton caldera. Apparent particle-thickness distributions indicate that the clays may have undergone Ostwald ripening and that this process has modified the K-Ar ages of the samples. The mechanism of Ostwald ripening can account for many of the features found for the hydrothermal alteration of illite. Expandabilities measured by the XRD peak-position method for illite/smectites (I/S) from various locations are smaller than expandabilities measured by transmission electron microscopy (TEM) and by the Warren-Averbach (W-A) method. This disparity is interpreted as being related to the presence of nonswelling basal surfaces that form the ends of stacks of illite particles (short-stack effect), stacks that, according to the theory of interparticle diffraction, diffract as coherent X-ray scattering domains. -from Authors

Coupling Graphene Sheets with Magnetic Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

sheets obtained from three different synthetic methods: (i) electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) [8], (ii...Figure 8d, the characteristic lattice fringes of ɤ-Fe2O3 nanoparticles in graphene sheet is shown. Typical X-ray diffraction ( XRD ) patterns of the HOPG ...pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG , exfoliated graphene, PyDop1

Improving the Mechanical Performance and Thermal Stability of a PVA-Clay Nanocomposite by Electron Beam Irradiation

NASA Astrophysics Data System (ADS)

Shokuhi Rad, A.; Ebrahimi, D.

2017-07-01

The effects of electron beam irradiation and presence of clay on the mechanical properties and thermal stability of montmorillonite clay-modified polyvinyl alcohol nanocomposites were studied. By using the X-ray diffraction (XRD) and transmission electron microscopy (TEM), the microstructure of the nanocomposites was investigated. The results obtained from TEM and XRD tests showed that montmorillonite clay nanoparticles were located in the polyvinyl alcohol phase. The XRD analysis confirmed the formation of an exfoliated structure in nanocomposites samples. Increasing the amount of clay to 20 wt.% increased the tensile strength and modulus of the nanocomposite. Irradiation up to an absorbed dose of 100 kGy increased its mechanical properties and thermal stability, but at higher irradiation levels, the mechanical strength and thermal stability declined. The sample with 20 wt.% of the nanofiller, exposed to 100 kGy, showed the highest mechanical strength and thermal stability.

X-ray peak profile analysis of zinc oxide nanoparticles formed by simple precipitation method

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick Joaquin; Magdaluyo, Eduardo

2017-12-01

Zinc oxide (ZnO) nanoparticles were successfully synthesized by a simple precipitation method using zinc acetate and tetramethylammonium hydroxide. The synthesized ZnO nanoparticles were characterized by X-ray Diffraction analysis (XRD) and Transmission Electron Microscopy (TEM). The XRD result revealed a hexagonal wurtzite structure for the ZnO nanoparticles. The TEM image showed spherical nanoparticles with an average crystallite size of 6.70 nm. For x-ray peak analysis, Williamson-Hall (W-H) and Size-Strain Plot (SSP) methods were applied to examine the effects of crystallite size and lattice strain on the peak broadening of the ZnO nanoparticles. Based on the calculations, the estimated crystallite sizes and lattice strains obtained are in good agreement with each other.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

Structural transformation of biochar black carbon by C60 superstructure: Environmental implications

USDA-ARS?s Scientific Manuscript database

Aqueous fullerene C60 nanoparticles (nC60) are frequently considered within the environmental engineering community as the aggregate of 60-carbon molecules. This study employed transmission electron microscopy (TEM) and x-ray diffraction (XRD) to demonstrate that nC60 formed via prolonged stirring ...

Organic Photonics: Toward a New Generation of Thin Film Photovoltaics and Lasers

DTIC Science & Technology

2011-03-07

plane. 39 Both electron and x - ray diffraction confirm the existence of crystalline domains of CuPc and C60. Crystalline domain sizes range from 5...nanocrystalline domains indicated by white curves that locate the domain boundaries. Scale bar=5 nm. b, X - ray diffraction pattern of an OVPD grown A... ray diffraction (XRD) and atomic force microscopy (AFM), as shown in Fig. 8. A cross-sectional TEM image of [CuPc(6.1nm)/C60(6.1nm)]10 is shown in

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

Microwave assisted scalable synthesis of titanium ferrite nanomaterials

NASA Astrophysics Data System (ADS)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Synthesis of nano-forsterite powder by making use of natural silica sand

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less

Ni@Fe2O3 heterodimers: controlled synthesis and magnetically recyclable catalytic application for dehalogenation reactions

NASA Astrophysics Data System (ADS)

Nakhjavan, Bahar; Tahir, Muhammad Nawaz; Natalio, Filipe; Panthöfer, Martin; Gao, Haitao; Dietzsch, Michael; Andre, Rute; Gasi, Teuta; Ksenofontov, Vadim; Branscheid, Robert; Kolb, Ute; Tremel, Wolfgang

2012-07-01

Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants.Ni@Fe2O3 heterodimer nanoparticles (NPs) were synthesized by thermal decomposition of organometallic reactants. After functionalization, these Ni@Fe2O3 heterodimers became water soluble. The pristine heterodimeric NPs were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetic susceptibility measurements. A special advantage of the heterodimers lies in the fact that nanodomains of different composition can be used as catalysts for the removal of environmentally hazardous halogenated pollutants. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr12121b

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Green synthesis of gold and silver nanoparticles using Hibiscus rosa sinensis

NASA Astrophysics Data System (ADS)

Philip, Daizy

2010-03-01

Biological synthesis of gold and silver nanoparticles of various shapes using the leaf extract of Hibiscus rosa sinensis is reported. This is a simple, cost-effective, stable for long time and reproducible aqueous room temperature synthesis method to obtain a self-assembly of Au and Ag nanoparticles. The size and shape of Au nanoparticles are modulated by varying the ratio of metal salt and extract in the reaction medium. Variation of pH of the reaction medium gives silver nanoparticles of different shapes. The nanoparticles obtained are characterized by UV-vis, transmission electron microscopy (TEM), X-ray diffraction (XRD) and FTIR spectroscopy. Crystalline nature of the nanoparticles in the fcc structure are confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes, bright circular spots in the selected area electron diffraction (SAED) and clear lattice fringes in the high-resolution TEM image. From FTIR spectra it is found that the Au nanoparticles are bound to amine groups and the Ag nanoparticles to carboxylate ion groups.

To study the effect of doping concentration of silver on structural and optical properties of cadmium oxide (CdO) nanostructure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Dept. of Physics, Vaish College of Engineering, Rohtak-124001, Haryana; Sharma, Ashwani

The present work deals with study of structural and optical properties of Silver (Ag) doped Cadmium oxide (CdO) nanostructured synthesized by Chemical Co-precipitation Techniques followed by calcinations at small temperature. The doping concentrations were changing from 0.1 to 10 at% respectively. Structural analysis study of these calcined materials is carried out by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The optical properties of calcined samples were investigating by Fourier transformation infrared (FTIR)spectroscopy, UV-Visible Spectroscopy (UV-Vis). The structural properties analysis results revels that crystallite size are in the range of nano region and TEM results aremore » quite in accordance with XRD results.« less

Structural, magnetic and electronic structural properties of Mn doped CeO2 nanoparticles

NASA Astrophysics Data System (ADS)

Kumari, Kavita; Vij, Ankush; Hashim, Mohd.; Chae, K. H.; Kumar, Shalendra

2018-05-01

Nanoparticles of Ce1-xMnxO2, (x=0.0, 0.01, and 0.05) have been synthesized by using co-precipitation method, and then characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), near edge x-ray absorption fine structure (NEXAFS) spectroscopy and dc magnetization measurements. XRD results clearly showed that the all the samples have single phase nature and exclude the presence of any secondary phase. The average particle size calculated using XRD TEM measurements found to decrease with increase in Mn doping in the range of 4.0 - 9.0 nm. The structural parameters such as strain, interplaner distance and lattice parameter is observed to decrease with increase in doping. The morphology of Ce1-xMnxO2 nanoparticles measured using TEM micrographs indicate that nanoparticle have spherical shape morphology. Magnetic hysteresis curve for Ce1-xMnxO2, (x = 0.0, 0.01, and 0.05) confirms the ferromagnetic ordering room temperature. The value of saturation magnetization is observed to decrease with increase in temperature from 10 K to 300 K. The NEXAFS spectra measured at Ce M4,5 edge reveals that Ce-ions are in +4 valance state.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz; Wei, Shanghai; Han, Jie

In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientationmore » has been studied in detail.« less

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Laser additive manufacturing bulk graphene-copper nanocomposites.

PubMed

Hu, Zengrong; Chen, Feng; Lin, Dong; Nian, Qiong; Parandoush, Pedram; Zhu, Xing; Shao, Zhuqiang; Cheng, Gary J

2017-11-03

The exceptional mechanical properties of graphene make it an ideal nanofiller for reinforcing metal matrix composites (MMCs). In this work, graphene-copper (Gr-Cu) nanocomposites have been fabricated by a laser additive manufacturing process. Transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy were utilized to characterize the fabricated nanocomposites. The XRD, Raman spectroscopy, energy dispersive spectroscopy and TEM results demonstrated the feasibility of laser additive manufacturing of Gr-Cu nanocomposites. The microstructures were characterized by high resolution TEM and the results further revealed the interface between the copper matrix and graphene. With the addition of graphene, the mechanical properties of the composites were enhanced significantly. Nanoindentation tests showed that the average modulus value and hardness of the composites were 118.9 GPa and 3 GPa respectively; 17.6% and 50% increases were achieved compared with pure copper, respectively. This work demonstrates a new way to manufacture graphene copper nanocomposites with ultra-strong mechanical properties and provides alternatives for applications in electrical and thermal conductors.

Laser additive manufacturing bulk graphene-copper nanocomposites

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Chen, Feng; Lin, Dong; Nian, Qiong; Parandoush, Pedram; Zhu, Xing; Shao, Zhuqiang; Cheng, Gary J.

2017-11-01

The exceptional mechanical properties of graphene make it an ideal nanofiller for reinforcing metal matrix composites (MMCs). In this work, graphene-copper (Gr-Cu) nanocomposites have been fabricated by a laser additive manufacturing process. Transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy were utilized to characterize the fabricated nanocomposites. The XRD, Raman spectroscopy, energy dispersive spectroscopy and TEM results demonstrated the feasibility of laser additive manufacturing of Gr-Cu nanocomposites. The microstructures were characterized by high resolution TEM and the results further revealed the interface between the copper matrix and graphene. With the addition of graphene, the mechanical properties of the composites were enhanced significantly. Nanoindentation tests showed that the average modulus value and hardness of the composites were 118.9 GPa and 3 GPa respectively; 17.6% and 50% increases were achieved compared with pure copper, respectively. This work demonstrates a new way to manufacture graphene copper nanocomposites with ultra-strong mechanical properties and provides alternatives for applications in electrical and thermal conductors.

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

of highly oriented pyrolytic graphite ( HOPG ) flake. Two electrode system containing platinum as counter electrode and HOPG as working electrode is... XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3 and PyDop1-ɤ-Fe2O3-graphene are given in Figure 1e. HOPG show a very sharp diffraction...atoms arranged in hexagonal pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG

Nanomechanical study of amorphous and polycrystalline ALD HfO2 thin films

Treesearch

K. Tapily; J.E. Jakes; D. Gu; H. Baumgart; A.A. Elmustafa

2011-01-01

Thin films of hafnium oxide (HfO2) were deposited by atomic layer deposition (ALD). The structural properties of the deposited films were characterised by transmission electron microscopy (TEM) and X-ray diffraction (XRD). We investigated the effect of phase transformations induced by thermal treatments on the mechanical properties of ALD HfO

Measurement of fundamental illite particle thicknesses by X-ray diffraction using PVP-10 intercalation

USGS Publications Warehouse

Eberl, D.D.; Nüesch, R.; Šucha, Vladimír; Tsipursky, S.

1998-01-01

The thicknesses of fundamental illite particles that compose mixed-layer illite-smectite (I-S) crystals can be measured by X-ray diffraction (XRD) peak broadening techniques (Bertaut-Warren-Averbach [BWA] method and integral peak-width method) if the effects of swelling and XRD background noise are eliminated from XRD patterns of the clays. Swelling is eliminated by intercalating Na-saturated I-S with polyvinylpyrrolidone having a molecular weight of 10,000 (PVP-10). Background is minimized by using polished metallic silicon wafers cut perpendicular to (100) as a substrate for XRD specimens, and by using a single-crystal monochromator. XRD measurements of PVP-intercalated diagenetic, hydrothermal and low-grade metamorphic I-S indicate that there are at least 2 types of crystallite thickness distribution shapes for illite fundamental particles, lognormal and asymptotic; that measurements of mean fundamental illite particle thicknesses made by various techniques (Bertant-Warren-Averbach, integral peak width, fixed cation content, and transmission electron microscopy [TEM]) give comparable results; and that strain (small differences in layer thicknesses) generally has a Gaussian distribution in the log-normal-type illites, but is often absent in the asymptotic-type illites.

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour

DOE Office of Scientific and Technical Information (OSTI.GOV)

Narayanan, Kannan Badri; Sakthivel, Natarajan, E-mail: puns2005@gmail.com

2011-10-15

Highlights: {yields} Synthesis of AgNPs using the leaf extract of Coleus amboinicus L. was described. {yields} UV-vis absorption spectra showed the formation of isotrophic AgNPs at 437 nm in 6 h. {yields} XRD analysis showed intense peaks corresponding to fcc structure of AgNPs. {yields} HR-TEM analysis revealed the formation of stable anisotrophic and isotrophic AgNPs. -- Abstract: In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmissionmore » electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.« less

Structural and optical characterization of bismuth sulphide nanorods

NASA Astrophysics Data System (ADS)

Shah, N. M.; Poria, K. C.

2017-05-01

In this work Bismuth sulfide (Bi2S3) nanorods with a high order of crystallinity is synthesized via hydrothermal method from aqueous solution of Bismuth Nitrate Pentahydrate and elemental Sulphur using Triethanolamine (TEA) as capping agent. The microstructures of Bi2S3 nanorods were investigated by X-ray diffraction (XRD) analysis. The positions and relative intensities of all the peaks in XRD pattern are in good agreement with those of the orthorhombic crystal structure of Bi2S3. TEM images shows that synthesized Bi2S3 has morphology of nanorods while selected area electron diffraction pattern indicates single crystalline nature. The analysis of diffuse reflectance (DR) spectrum of as synthesized Bi2S3 using Kubelka - Munk theory suggests direct energy band gap of 1.5 eV.

Nanobelt formation of magnesium hydroxide sulfate hydrate via a soft chemistry process.

PubMed

Zhou, Zhengzhi; Sun, Qunhui; Hu, Zeshan; Deng, Yulin

2006-07-13

The nanobelt formation of magnesium hydroxide sulfate hydrate (MHSH) via a soft chemistry approach using carbonate salt and magnesium sulfate as reactants was successfully demonstrated. X-ray diffraction (XRD), energy dispersion X-ray spectra (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analysis revealed that the MHSH nanobelts possessed a thin belt structure (approximately 50 nm in thickness) and a rectangular cross profile (approximately 200 nm in width). The MHSH nanobelts suffered decomposition under electron beam irradiation during TEM observation and formed MgO with the pristine nanobelt morphology preserved. The formation process of the MHSH nanobelts was studied by tracking the morphology of the MHSH nanobelts during the reaction. A possible chemical reaction mechanism is proposed.

CdO-NPs; synthesis from 1D new nano Cd coordination polymer, characterization and application as anti-cancer drug for reducing the viability of cancer cells

NASA Astrophysics Data System (ADS)

Afzalian Mend, Behnaz; Delavar, Mahmoud; Darroudi, Majid

2017-04-01

The hexagonal CdO nano-particles (CdO-NPs) was prepared using new nano Cd coordination polymer, [Cd(NO3)(bipy)(pzca)]n (1) as a precursor, through direct calcination process at 500 °C. The precursor (1) was synthesized by sonochemical method. The new nano compound (1) was characterized by IR spectroscopy, elemental analyses, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and thermal gravimetric analyses. The structure of nano coordination polymer was determined by comparing the XRD pattern of nano and single-crystal of compound (1). The nano CdO was characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). In addition, the activity and efficiency of nano CdO as an anti-cancer drug was studied on cancer cells with different concentration. The results shows that the viability of cancer cells reduced above 2 μg/mL of CdO-NPs concentration.

Extracellular synthesis of mycogenic silver nanoparticles by Cylindrocladium floridanum and its homogeneous catalytic degradation of 4-nitrophenol.

PubMed

Narayanan, Kannan Badri; Park, Hyun Ho; Sakthivel, Natarajan

2013-12-01

Green synthesis of extracellular mycogenic silver nanoparticles using the fungus, Cylindrocladium floridanum is reported. The synthesized mycogenic silver nanoparticles were characterized using UV-Vis absorption spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) techniques. The nanoparticles exhibit fcc structure with Bragg's reflections of (111), (200), (220) and (311) was evidenced by XRD pattern, high-resolution TEM lattice fringes and circular rings in selected-area electron diffraction (SAED) pattern. The morphology of nanoparticles was roughly spherical in shape with an average size of ca. 25 nm. From FTIR spectrum, it was found that the biomolecules with amide I and II band were involved in the stabilization of nanoparticles. These mycogenic silver nanoparticles exhibited the homogeneous catalytic potential in the reduction of pollutant, 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) using sodium borohydride, which followed a pseudo-first-order kinetic model. Thus, the synthesis of metal nanoparticles using sustainable microbial approach opens up possibilities in the usage of mycogenic metal nanoparticles as catalysts in various chemical reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Microstructures of GaN1-xPx layers grown on (0001) GaN substrates by gas source molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Seong, Tae-Yeon; Bae, In-Tae; Choi, Chel-Jong; Noh, D. Y.; Zhao, Y.; Tu, C. W.

1999-03-01

Transmission electron microscope (TEM), transmission electron diffraction (TED), and synchrotron x-ray diffraction (XRD) studies have been performed to investigate microstructural behavior of gas source molecular beam epitaxial GaN1-xPx layers grown on (0001) GaN/sapphire at temperatures (Tg) in the range 500-760 °C. TEM, TED, and XRD results indicate that the samples grown at Tg⩽600 °C undergo phase separation resulting in a mixture of GaN-rich and GaP-rich GaNP with zinc-blende structure. However, the samples grown at Tg⩾730 °C are found to be binary zinc-blende GaN(P) single crystalline materials. As for the 500 °C layer, the two phases are randomly oriented and distributed, whereas the 600 °C layer consists of phases that are elongated and inclined by 60°-70° clockwise from the [0001]α-GaN direction. The samples grown at Tg⩾730 °C are found to consist of two types of microdomains, namely, GaN(P)I and GaN(P)II; the former having twin relation to the latter.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

NASA Astrophysics Data System (ADS)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Nanocrystallization in Cu-Zr-Al-Sm Bulk Metallic Glasses

NASA Astrophysics Data System (ADS)

Sikan, Fatih; Yasar, Bengisu; Kalay, Ilkay

2018-04-01

The effect of rare-earth element (Sm) microalloying on the thermal stability and crystallization kinetics of melt-spun ribbons and suction-cast rods of Zr48Cu38.4Al9.6Sm4 alloy were investigated using differential scanning calorimetry (DSC), X-ray diffraction (XRD), transmission electron microscopy (TEM), and atom probe tomography (APT). The XRD results of constant heating rate annealing indicated that amorphous Zr48Cu38.4Al9.6Sm4 melt-spun ribbons devitrifies into Cu2Sm at 673 K (400 °C). The sequence continues with the precipitation of Cu10Zr7 and then these two phases coexist. XRD and TEM studies on 1 mm diameter as suction-cast rods indicated the precipitation of 30-nm-mean size Cu2Sm crystals during solidification. TEM investigation of the isothermal crystallization sequence of melt-spun ribbons and 1-mm-diameter suction-cast rods revealed the precipitation of Cu2Sm nanocrystals at the onset of crystallization and the restriction of the growth of these nanocrystals up to 10 nm diameter with further annealing. APT analysis of 1-mm-diameter suction-cast rods showed that the limited growth of Cu2Sm nanocrystals is due to sluggish diffusion of Sm and Al-Zr pile up at the interface.

XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide.

PubMed

Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L

2013-10-15

An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

X-ray diffraction study of low-temperature phase transformations in nickel-titanium orthodontic wires.

PubMed

Iijima, M; Brantley, W A; Guo, W H; Clark, W A T; Yuasa, T; Mizoguchi, I

2008-11-01

Employ conventional X-ray diffraction (XRD) to analyze three clinically important nickel-titanium orthodontic wire alloys over a range of temperatures between 25 and -110 degrees C, for comparison with previous results from temperature-modulated differential scanning calorimetry (TMDSC) studies. The archwires selected were 35 degrees C Copper Ni-Ti (Ormco), Neo Sentalloy (GAC International), and Nitinol SE (3M Unitek). Neo Sentalloy, which exhibits superelastic behavior, is marketed as having shape memory in the oral environment, and Nitinol SE and 35 degrees C Copper Ni-Ti also exhibit superelastic behavior. All archwires had dimensions of 0.016in.x0.022in. (0.41 mm x 0.56 mm). Straight segments cut with a water-cooled diamond saw were placed side-by-side to yield a 1 cm x 1cm test sample of each wire product for XRD analysis (Rint-Ultima(+), Rigaku) over a 2theta range from 30 degrees to 130 degrees and at successive temperatures of 25, -110, -60, -20, 0 and 25 degrees C. The phases revealed by XRD at the different analysis temperatures were in good agreement with those found in previous TMDSC studies of transformations in these alloys, in particular verifying the presence of R-phase at 25 degrees C. Precise comparisons are not possible because of the approximate nature of the transformation temperatures determined by TMDSC and the preferred crystallographic orientation present in the wires. New XRD peaks appear to result from low-temperature transformation in martensite, which a recent transmission electron microscopy (TEM) study has shown to arise from twinning. While XRD is a useful technique to study phases in nickel-titanium orthodontic wires and their transformations as a function of temperature, optimum insight is obtained when XRD analyses are combined with complementary TMDSC and TEM study of the wires.

Improvement of the piezoelectric properties in (K,Na)NbO3-based lead-free piezoelectric ceramic with two-phase co-existing state

NASA Astrophysics Data System (ADS)

Yamada, H.; Matsuoka, T.; Kozuka, H.; Yamazaki, M.; Ohbayashi, K.; Ida, T.

2015-06-01

Two phases of (K,Na)NbO3 (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K1-xNax)0.86Ca0.04Li0.02Nb0.85O3-δ-0.042K0.85Ti0.85Nb1.15O5-0.036BaZrO3-0.0016Co3O4- 0.0025Fe2O3-0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains of the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, kp = 0.56, has been observed at the composition x = 0.56.

Microstructural, optical and electrical transport properties of Cd-doped SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Mohsin Nizam Ansari, Mohd

2018-03-01

We have successfully investigated the structural, optical and dielectric properties of Cd assimilated SnO2 nanoparticles synthesized via very convenient precipitation route. The structural properties were studied by x-ray diffraction method (XRD) and Fourier Transform Infrared (FTIR) Spectroscopy. As-synthesized samples in the form of powder were examined for its morphology and average particle size by Transmission electron microscopy (TEM). The optical properties were studied by diffuse reflectance spectroscopy. Dielectric properties such that complex dielectric constant and ac conductivity were investigated by LCR meter. Average crystallite size calculated by XRD and average particle size obtained from TEM were found to be consistent and below 50 nm for all samples. The optical band gap of as-synthesized powder samples from absorption study was found in the range of 3.76 to 3.97 eV. The grain boundary parameters such that Rgb, Cgb and τ were evaluated using impedance spectroscopy.

Synthesis and structural characterization of CdS nanoparticles using nitrogen adducts of mixed diisopropylthiourea and dithiolate derivatives of Cd(II) complexes

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

[Cd(diptu)2(ced)], [Cd(diptu)2(ced)(bpy)], [Cd(diptu)2(ced)(phen)], (where diptu = diisopropyl thiourea; ced = 1-cyano-1-carboethoxylethylene-2,2‧-dithiolate; bpy = 2,2‧-bipyridine and phen = 1,10-phenanthroline) have been prepared and used as single source precursors for the preparation of hexadecylamine capped CdS nanoparticles. The precursor complexes were characterized by elemental analysis, FTIR and TGA. The structural properties of the nanoparticles were investigated using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy techniques (SEM). The optical properties of the nanoparticles were studied using UV-Visible and photoluminescence spectroscopy. The XRD analysis showed that the nanoparticles were indexed to the hexagonal phase of CdS and the TEM results showed CdS nanoparticles with average crystallite sizes of 4.00-8.80 nm.

Graphene/Ruthenium Active Species Aerogel as Electrode for Supercapacitor Applications.

PubMed

Gigot, Arnaud; Fontana, Marco; Pirri, Candido Fabrizio; Rivolo, Paola

2017-12-30

Ruthenium active species containing Ruthenium Sulphide (RuS₂) is synthesized together with a self-assembled reduced graphene oxide (RGO) aerogel by a one-pot hydrothermal synthesis. Ruthenium Chloride and L-Cysteine are used as reactants. The hydrothermal synthesis of the innovative hybrid material occurs at 180 °C for 12 h, by using water as solvent. The structure and morphology of the hybrid material are fully characterized by Raman, XRD, XPS, FESEM and TEM. The XRD and diffraction pattern obtained by TEM display an amorphous nanostructure of RuS₂ on RGO crystallized flakes. The specific capacitance measured in planar configuration in 1 M NaCl electrolyte at 5 mV s -1 is 238 F g -1 . This supercapacitor electrode also exhibits perfect cyclic stability without loss of the specific capacitance after 15,000 cycles. In summary, the RGO/Ruthenium active species hybrid material demonstrates remarkable properties for use as active material for supercapacitor applications.

Influence of reaction time and synthesis temperature on the physical properties of ZnO nanoparticles synthesized by the hydrothermal method

NASA Astrophysics Data System (ADS)

Wasly, H. S.; El-Sadek, M. S. Abd; Henini, Mohamed

2018-01-01

Influence of synthesis temperature and reaction time on the structural and optical properties of ZnO nanoparticles synthesized by the hydrothermal method was investigated using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray, Fourier transform infra-red spectroscopy, and UV-visible and fluorescence spectroscopy. The XRD pattern and HR-TEM images confirmed the presence of crystalline hexagonal wurtzite ZnO nanoparticles with average crystallite size in the range 30-40 nm. Their energy gap determined by fluorescence was found to depend on the synthesis temperature and reaction time with values in the range 2.90-3.78 eV. Thermal analysis, thermogravimetric and the differential scanning calorimetry were used to study the thermal reactions and weight loss with heat of the prepared ZnO nanoparticles.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Synthesis and characterization of silver-copper core-shell nanoparticles using polyol method for antimicrobial agent

NASA Astrophysics Data System (ADS)

Hikmah, N.; Idrus, N. F.; Jai, J.; Hadi, A.

2016-06-01

Silver and copper nanoparticles are well-known as the good antimicrobial agent. The nano-size of particles influences in enhancing the antimicrobial activity. This paper discusses the effect of molarity on the microstructure and morphology of silver-copper core-shell nanoparticles prepared by a polyol method. In this study, silver-copper nanoparticles are synthesized through the green approach of polyol method using ethylene glycol (EG) as green solvent and reductant, and polyoxyethylene-(80)-sorbitan monooleate (Tween 80) as a nontoxic stabilizer. The phase and morphology of silver-copper nanoparticles are characterized by X-ray diffraction (XRD) and Field emission scanning electron microscope (FESEM) and Transmission electron microscope (TEM). The results XRD confirm the pure crystalline of silver and copper nanoparticles with face-centered cubic (FCC) structure. FESEM and TEM analysis confirm the existence of Ag and Cu nanoparticles in core-shell shape.

Nanocomposite bulk of mechanically milled Al-Pb samples consolidated pore-free by the high-energy rate forming technique.

PubMed

Csanády, Agnes; Sajó, István; Lábár, János L; Szalay, András; Papp, Katalin; Balaton, Géza; Kálmán, Erika

2005-06-01

It is shown that pore-free bulk samples were produced by the high-energy rate forming axis-symmetrical powder compaction method for different application purposes in case of the very different, immiscible Al and Pb metal pair. The starting Al-Pb nanocomposites were made by mechanical milling of atomized Al and Pb powders either in a SPEX 9000 or a Fritsch Pulverisette 4 mill. Due to the conditions that milling was carried out in air, the PbO layer, originally existing at the surface of the atomized Pb powder, ruptured and was also dispersed in the composite. The presence of the nano PbO particles was proven by XRD and TEM (BF, DF, SAED). When the energy of milling was high, the PbO crystallites became so small that they could hardly be seen by XRD technique. Local distribution of the PbO nanoparticles was still visible in a TEM, using the process diffraction method. Both XRD and SAED proved to be useful for the evaluation of the results of the milling process and compaction.

Synthesis and characterization of hollow spherical copper phosphide (Cu 3P) nanopowders

NASA Astrophysics Data System (ADS)

Liu, Shuling; Qian, Yitai; Xu, Liqiang

2009-03-01

In this paper, hollow spherical Cu 3P nanopowders were synthesized by using copper sulfate pentahydrate (CuSO 4ṡ5H 2O) and yellow phosphorus in a mixed solvent of glycol, ethanol and water at 140-180 ∘C for 12 h. X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), electron diffraction pattern (ED) and transmission electronic microscopy (TEM) studies show that the as-synthesized nanocrystal is pure hexagonal phase Cu 3P with a hollow spherical morphology. Based on the TEM observations, a possible aggregation growth mechanism was proposed for the formation of Cu 3P hollow structures. Meanwhile, the effects of some key factors such as solvents, reaction temperature and reaction time on the final formation of the Cu 3P hollow structure were also discussed.

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

NASA Astrophysics Data System (ADS)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Morphology and thermal studies of zinc sulfide and cadmium sulfide nanoparticles in polyvinyl alcohol matrix

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2016-09-01

Zn(II) and Cd(II) metal complexes of 1-cyano-1-carboethoxyethylene-2,2-dithiolato-κS,S'-bis(N,N-dimethylthiourea-κS) have been synthesized and characterized with analytical and spectroscopic techniques. The complexes were thermolysed in hexadecylamine at 200 °C to prepare ZnS and CdS nanoparticles. The nanoparticles were characterized with scanning electron microscope (SEM), transmission electron microscope (TEM), and powder X-ray diffraction (p-XRD). TEM images showed spherically shaped nanoparticles, whose sizes are in the range 4.33-7.21 nm for ZnS and 4.95-7.7 nm CdS respectively and XRD confirmed cubic crystalline phases for the nanoparticles. The optical band gap energy evaluated from the absorption spectra are 2.88 eV (430 nm) and 2.81 eV (440 nm) for the ZnS and CdS nanoparticles respectively. The as-prepared metal sulfide nanoparticles were further incorporated into polyvinyl alcohol (PVA) to give ZnS/PVA and CdS/PVA composites. The polymer nanocomposites were studied to investigate their morphology and thermal properties relative to the pure PVA. XRD diffractions indicated that the crystalline phases of the nanoparticles and the sizes in PVA matrices remained unaltered. Infra-red spectra studies revealed interactions between the PVA and the metal sulfide nanoparticles and TGA studies show that the ZnS/PVA and CdS/PVA nanocomposites exhibit better thermal stability than the pure PVA.

Characterization of ZnAl cast alloys with Na addition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gancarz, Tomasz, E-mail: t.gancarz@imim.pl; Cempura, Grzegorz; Skuza, Wojciech

2016-01-15

This study was aimed at evaluating the microstructural change and thermal, electrical and mechanical properties with the addition of Na to eutectic ZnAl alloys. Solders based on eutectic ZnAl containing 0.2 to 3.0 (wt.%) of Na were developed for high temperature solder. Differential scanning calorimetry (DSC) measurements were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed over − 50 °C to 300 °C and 30 °C to 300 °C temperature ranges, respectively. The microstructure of the specimens was analyzed using scanning (SEM) and transmission electron microscopy (TEM) techniques. Chemical microanalysismore » was performed by energy-dispersive X-ray spectroscopy (EDS) on SEM and TEM. The precipitates of NaZn{sub 13} were confirmed by X-ray diffraction (XRD) measurements and selected area electron diffraction (SAED) techniques. The addition of Na to eutectic ZnAl alloy increased the electrical resistivity and reduced the coefficient of thermal expansion; however, the melting point did not change. The mechanical properties, strain and microhardness increased with Na content in alloys. - Highlights: • High temperature soldering materials of ZnAl with Na were designed and characterized. • Precipitates of NaZn{sub 13}were observed and confirmed using TEM and XRD. • Addition of Na to eutectic ZnAl cussed increased mechanical properties. • NaZn{sub 13} caused increased electrical resistivity and microhardness, and reduced the CTE.« less

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates.

PubMed

Silva, Chinthaka M; Rosseel, Thomas M; Kirkegaard, Marie C

2018-03-19

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18 , 4 × 10 19 , and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasing neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2 , with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. The cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.

Quantitative XRD analysis of {110} twin density in biotic aragonites.

PubMed

Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

2012-12-01

{110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

Facile and fast synthesis of SnS2 nanoparticles by pulsed laser ablation in liquid

NASA Astrophysics Data System (ADS)

Johny, J.; Sepulveda-Guzman, S.; Krishnan, B.; Avellaneda, D.; Shaji, S.

2018-03-01

Nanoparticles (NPs) of tin disulfide (SnS2) were synthesized using pulsed laser ablation in liquid (PLAL) technique. Effects of different liquid media and ablation wavelengths on the morphology and optical properties of the nanoparticles were studied. Nd: YAG laser wavelengths of 532 nm and 1064 nm (frequency 10 Hz and pulse width 10 ns) were used to irradiate SnS2 target immersed in liquid for the synthesis of SnS2 nanoparticles. Here PLAL was a fast synthesis technique, the ablation was only for 30 s. Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis absorption spectroscopy and photoluminescence spectroscopy were used to characterize the SnS2 NPs. TEM images showed that the liquid medium and laser wavelength influence the morphology of the NPs. SAED patterns and high resolution TEM (HRTEM) images confirmed the crystallinity of the particles. XRD and XPS analyses confirmed that SnS2 NPs were having exact crystalline structure and chemical states as that of the target. Raman analysis also supported the results obtained by XRD and XPS. Optical band gaps of the nanocolloids evaluated from their UV-vis absorption spectra were 2.4-3.05 eV. SnS2 NPs were having luminescence spectra in the blue-green region irrespective of the liquid media and ablation wavelength.

Electronic structure, magnetic and structural properties of Ni doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; Vats, Prashant; Gautam, S.

Highlights: • XRD, and HR-TEM results show the single phase nature of Ni doped ZnO nanoparticles. • dc magnetization results indicate the RT-FM in Ni doped ZnO nanoparticles. • Ni L{sub 3,2} edge NEXAFS spectra infer that Ni ions are in +2 valence state. • O K edge NEXAFS spectra show that O vacancy increases with Ni doping in ZnO. - Abstract: We report structural, magnetic and electronic structural properties of Ni doped ZnO nanoparticles prepared by auto-combustion method. The prepared nanoparticles were characterized by using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), near edge X-ray absorption finemore » structure (NEXAFS) spectroscopy, and dc magnetization measurements. The XRD and HR-TEM results indicate that Ni doped ZnO nanoparticles have single phase nature with wurtzite lattice and exclude the presence of secondary phase. NEXAFS measurements performed at Ni L{sub 3,2}-edges indicates that Ni ions are in +2 valence state and exclude the presence of Ni metal clusters. O K-edge NEXAFS spectra indicate an increase in oxygen vacancies with Ni-doping, while Zn L{sub 3,2}-edge show the absence of Zn-vacancies. The magnetization measurements performed at room temperature shows that pure and Ni doped ZnO exhibits ferromagnetic behavior.« less

Green synthesis of silver nanoparticles using tannins

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

The Structure and Infrastructure of the Global Nanotechnology Literature

DTIC Science & Technology

2005-01-01

transmiss.electron.microscopi 1.3%, morpholog 1.2%, zn 1.0%, cd 1.0%, microscopi 1.0%, synthesi 0.9%, diffract.xrd 0.8%, electron 0.8%, powder 0.8%, surfact 0.8...film 2.3%, product 2.3%, hydrotherm 1.1%, tem 1.0%, synthes 0.9%, reaction 0.9%, xrd 0.9%, layer 0.8%, zn 0.8%, surfac 0.7%, cd 0.7%, magnet 0.7...0.5%, sol.gel 0.5%, thick 0.5%, materi 0.5%, laser 0.5%, reaction 0.5%, capac 0.4%, synthesi 0.4%, thin 0.4%, surfac 0.4%, nanowir 0.4%, nanoparticl

Polymethacrylic acid as a new precursor of CuO nanoparticles

NASA Astrophysics Data System (ADS)

Hosny, Nasser Mohammed; Zoromba, Mohamed Shafick

2012-11-01

Polymethacrylic acid and its copper complexes have been synthesized and characterized. These complexes have been used as precursors to produce CuO nanoparticles by thermal decomposition in air. The stages of decompositions and the calcination temperature of the precursors have been determined from thermal analyses (TGA). The obtained CuO nanoparticles have been characterized by X-ray diffraction (XRD), scanning tunneling microscopy (STM) and transmission electron microscopy (TEM). XRD showed a monoclinic structure with particle size 8-20 nm for the synthesized copper oxide nanoparticles. These nanoparticles are catalytically active in decomposing hydrogen peroxide and a mechanism of decomposition has been suggested.

Synthesis and characterization of PVK/AgNPs nanocomposites prepared by laser ablation.

PubMed

Abd El-Kader, F H; Hakeem, N A; Elashmawi, I S; Menazea, A A

2015-03-05

Nanocomposites of Poly (n-vinylcarbazole) PVK/Ag nanoparticles were prepared by laser ablation of a silver plate in aqueous solution of chlorobenzene. The influences of laser parameters such as; time of irradiation, source power and wavelength (photon energy) on structural, morphological and optical properties have been investigated using X-ray diffraction (XRD), Transmission electron microscopy (TEM), Ultraviolet-visible (UV-Vis) and Photoluminescence (PL). A correlation between the investigated properties has been discussed. XRD, TEM and PL indicated that the complexation between AgNPs and PVK in the composite system is possible. Only the reflection peak at 2θ=38° of AgNPs appeared in the composite nanoparticles while the other reflection peaks were destroyed. The nanoparticles shape and size distribution were evaluated from TEM images. TEM analysis revealed a lower average particle size at long laser irradiation time 40min and short laser wavelength 532nm together with high laser power 570mW. From UV-Visible spectra the values of absorption coefficient, absorption edge and energy tail were calculated. The reduction of band tail value with increasing the laser ablation parameters confirms the decrease of the disorder in such composite system. The PL and UV-Vis. spectra confirm that nanocomposite samples showed quantum confinement effect. Copyright © 2014 Elsevier B.V. All rights reserved.

Trichoderma koningii assisted biogenic synthesis of silver nanoparticles and evaluation of their antibacterial activity

NASA Astrophysics Data System (ADS)

Tripathi, R. M.; Gupta, Rohit Kumar; Shrivastav, Archana; Singh, M. P.; Shrivastav, B. R.; Singh, Priti

2013-09-01

The present study demonstrates the biosynthesis of silver nanoparticles using Trichoderma koningii and evaluation of their antibacterial activity. Trichoderma koningii secretes proteins and enzymes that act as reducing and capping agent. The biosynthesized silver nanoparticles (AgNPs) were characterized by UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM) and x-ray diffraction (XRD). UV-Vis spectra showed absorbance peak at 413 nm corresponding to the surface plasmon resonance of silver nanoparticles. DLS was used to find out the size distribution profile. The size and morphology of the AgNPs was determined by TEM, which shows the formation of spherical nanoparticles in the size range of 8-24 nm. X-ray diffraction showed intense peaks corresponding to the crystalline silver. The antibacterial activity of biosynthesized AgNPs was evaluated by growth curve and inhibition zone and it was found that the AgNPs show potential effective antibacterial activity.

Diamonds in detonation soot

NASA Technical Reports Server (NTRS)

Greiner, N. Roy; Phillips, Dave; Johnson, J. D.; Volk, Fred

1990-01-01

Diamonds 4 to 7 nm in diameter have been identified and partially isolated from soot formed in detonations of carbon-forming composite explosives. The morphology of the soot has been examined by transmission electron microscopy (TEM), and the identity of the diamond has been established by the electron diffraction pattern of the TEM samples and by the X-ray diffraction (XRD) pattern of the isolated solid. Graphite is also present in the form of ribbons of turbostatic structure with a thickness of 2 to 4 nm. A fraction, about 25 percent of the soot by weight, was recovered from the crude soot after oxidation of the graphite with fuming perchloric acid. This fraction showed a distinct XRD pattern of diamond and the diffuse band of amorphous carbon. The IR spectrum of these diamonds closely matches that of diamonds recovered from meteorites (Lewis et al., 1987), perhaps indicating similar surface properties after the oxidation. If these diamonds are produced in the detonation itself or during the initial expansion, they exhibit a phenomenal crystal growth rate (5 nm/0.00001 s equal 1.8 m/hr) in a medium with a very low hydrogen/carbon ratio. Because the diamonds will be carried along with the expanding gases, they will be accelerated to velocities approaching 8 km/s.

Rapid green synthesis of spherical gold nanoparticles using Mangifera indica leaf

NASA Astrophysics Data System (ADS)

Philip, Daizy

2010-11-01

This paper reports the rapid biological synthesis of spherical gold nanoparticles at room temperature using fresh/dry leaf extract of Mangifera indica. This is a simple, cost-effective, stable for long time and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au nanoparticles of size ˜20 nm and 17 nm. The nanoparticles were obtained within 2 min of addition of the extract to the solution of HAuCl 4·3H 2O and the colloid is found to be stable for more than 5 months. Smaller and more uniformly distributed particles could be obtained with dried leaf extract. The nanoparticles obtained are characterized by UV-vis, transmission electron microscopy (TEM) and X-ray diffraction (XRD). Crystalline nature of the nanoparticles in the fcc structure is confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0), (2 2 0), (3 1 1) and (2 2 2) planes, bright circular spots in the selected area electron diffraction (SAED) and clear lattice fringes in the high-resolution TEM image. The possible biomolecules responsible for efficient stabilization are suggested by studying the FTIR spectrum of the sample. This environmentally benign method provides much faster synthesis and colloidal stability comparable to those of chemical reduction.

Bi2O3 nanoparticles encapsulated in surface mounted metal-organic framework thin films

NASA Astrophysics Data System (ADS)

Guo, Wei; Chen, Zhi; Yang, Chengwu; Neumann, Tobias; Kübel, Christian; Wenzel, Wolfgang; Welle, Alexander; Pfleging, Wilhelm; Shekhah, Osama; Wöll, Christof; Redel, Engelbert

2016-03-01

We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye.We describe a novel procedure to fabricate a recyclable hybrid-photocatalyst based on Bi2O3@HKUST-1 MOF porous thin films. Bi2O3 nanoparticles (NPs) were synthesized within HKUST-1 (or Cu3(BTC)2) surface-mounted metal-organic frame-works (SURMOFs) and characterized using X-ray diffraction (XRD), a quartz crystal microbalance (QCM) and transmission electron microscopy (TEM). The Bi2O3 semiconductor NPs (diameter 1-3 nm)/SURMOF heterostructures exhibit superior photo-efficiencies compared to NPs synthesized using conventional routes, as demonstrated via the photodegradation of the nuclear fast red (NFR) dye. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr00532b

Ultra-low thermal conductivity of TlIn5Se8 and structure of the new complex chalcogenide Tl0.98In13.12Se16.7Te2.3

NASA Astrophysics Data System (ADS)

Lefèvre, Robin; Berthebaud, David; Pérez, Olivier; Pelloquin, Denis; Boudin, Sophie; Gascoin, Franck

2017-06-01

TlIn5Se8 has been synthesized by means of solid-state reaction and densified by Spark Plasma Sintering. The compound is a semiconductor with a band gap of 1.62 eV estimated from reflectance measurements. Its thermal conductivity is about 0.45 W m-1. K-1 in the temperature range 300-673 K, an extremely low value attributed to its complex pseudo-1D structure reminiscent of the pseudo-hollandite. While attempting to dope TlIn5Se8 with Te, a new complex chalcogenide was discovered and characterized by the combination of TEM and XRD diffraction. It belongs to the A2In12X19 family, crystallizing in the R 3 ̅:H space group. Single crystal X-ray diffraction study led to a refined composition of Tl0.98In13.12Se16.7Te2.3 with cell parameters: a=13.839(5) Å and c=35.18(3) Å. A static disorder is found on one indium site situated in an octahedral environment. The single crystal XRD study is in agreement with TEM analyses in STEM-HAADF image mode that do not show any extended defects or disorder at atomic scale.

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Janeoo, Shashi; Sharma, Mamta, E-mail: mamta.phy85@gmail.com; Goswamy, J.

Polyaniline-indium oxide (In{sub 2}O{sub 3}/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In{sub 2}O{sub 3} nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In{sub 2}O{sub 3}/PANI nanocomposite. TEM analysis shows In{sub 2}O{sub 3} nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In{sub 2}O{sub 3} nanoparticles. The band gap and electronic transitions in In{sub 2}O{sub 3}/PANI nanocomposite is determined by using UV/Vis spectra.

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanningmore » electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.« less

In-field X-ray and neutron diffraction studies of re-entrant charge-ordering and field induced metastability in La0.175Pr0.45Ca0.375MnO3-δ

NASA Astrophysics Data System (ADS)

Sharma, Shivani; Shahee, Aga; Yadav, Poonam; da Silva, Ivan; Lalla, N. P.

2017-11-01

Low-temperature high-magnetic field (2 K, 8 T) (LTHM) powder X-ray diffraction (XRD) and time of flight powder neutron diffraction (NPD), low-temperature transmission electron microscopic (TEM), and resistivity and magnetization measurements have been carried out to investigate the re-entrant charge ordering (CO), field induced structural phase transitions, and metastability in phase-separated La0.175Pr0.45Ca0.375MnO3-δ (LPCMO). Low-temperature TEM and XRD studies reveal that on cooling under zero-field, paramagnetic Pnma phase transforms to P21/m CO antiferromagnetic (AFM) insulating phase below ˜233 K. Unlike reported literature, no structural signature of CO AFM P21/m to ferromagnetic (FM) Pnma phase-transition during cooling down to 2 K under zero-field was observed. However, the CO phase was found to undergo a re-entrant transition at ˜40 K. Neutron diffraction studies revealed a pseudo CE type spin arrangement of the observed CO phase. The low-temperature resistance, while cooled under zero-field, shows insulator to metal like transition below ˜105 K with minima at ˜25 K. On application of field, the CO P21/m phase was found to undergo field-induced transition to FM Pnma phase, which shows irreversibility on field removal below ˜40 K. Zero-field warming XRD and NPD studies reveal that field-induced FM Pnma phase is a metastable phase, which arise due to the arrest of kinetics of the first-order phase transition of FM Pnma to CO-AFM P21/m phase, below 40 K. Thus, a strong magneto-structural coupling is observed for this system. A field-temperature (H-T) phase-diagram has been constructed based on the LTHM-XRD, which matches very nicely with the reported H-T phase-diagram constructed based on magnetic measurements. Due to the occurrence of gradual growth of the re-entrant CO phase and the absence of a clear structural signature of phase-separation of CO-AFM P21/m and FM Pnma phases, the H-T minima in the phase-diagram of the present LPCMO sample has been attributed to the strengthening of AFM interaction during re-entrant CO transition and not to glass like "dynamic to frozen" transition.

Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

PubMed

Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

2014-04-23

In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

Synthesis, characterization and visible-light driven photocatalysis by differently structured CdS/ZnS sandwich and core-shell nanocomposites

NASA Astrophysics Data System (ADS)

Qutub, Nida; Pirzada, Bilal Masood; Umar, Khalid; Mehraj, Owais; Muneer, M.; Sabir, Suhail

2015-11-01

CdS/ZnS sandwich and core-shell nanocomposites were synthesized by a simple and modified Chemical Precipitation method under ambient conditions. The synthesized composites were characterized by XRD, SEM, TEM, EDAX and FTIR. Optical properties were analyzed by UV-vis. Spectroscopy and the photoluminescence study was done to monitor the recombination of photo-generated charge-carriers. Thermal stability of the synthesized composites was analyzed by Thermal Gravimetric Analysis (TGA). XRD revealed the formation of nanocomposites as mixed diffraction peaks were observed in the XRD pattern. SEM and TEM showed the morphology of the nanocomposites particles and their fine particle size. EDAX revealed the appropriate molar ratios exhibited by the constituent elements in the composites and FTIR gave some characteristic peaks which indicated the formation of CdS/ZnS nanocomposites. Electrochemical Impedance Spectroscopy was done to study charge transfer properties along the nanocomposites. Photocatalytic properties of the synthesized composites were monitored by the photocatalytic kinetic study of Acid Blue dye and p-chlorophenol under visible light irradiation. Results revealed the formation of stable core-shell nanocomposites and their efficient photocatalytic properties.

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Selvaraj, Mahalakshmi; Department of Material Science, School of Chemistry, Madurai Kamaraj University, Tamilnadu Madurai-625 021; Venkatachalapathy, V.

2015-11-15

Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO{sub 3}) nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C) employing barium dichloride (BaCl{sub 2}) and titanium tetrachloride (TiCl{sub 4}) as precursors and sodium hydroxide (NaOH) as mineralizer for synthesis of BaTiO{sub 3} nanopowders. The as-prepared BaTiO{sub 3} powders were investigated for structural characteristics using x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phasemore » directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula). SEM and TEM analysis verified that the BaTiO{sub 3} nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED) shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric) phases of undoped BaTiO{sub 3} nanopowders can be stabilized by the sol-hydrothermal method.« less

Green synthesis and characterization of graphene nanosheets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductantmore » but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.« less

Synthesis of High Valence Silver-Loaded Mesoporous Silica with Strong Antibacterial Properties

PubMed Central

Chen, Chun-Chi; Wu, Hsin-Hsien; Huang, Hsin-Yi; Liu, Chen-Wei; Chen, Yi-Ning

2016-01-01

A simple chemical method was developed for preparing high valence silver (Ag)-loaded mesoporous silica (Ag-ethylenediaminetetraacetic acid (EDTA)-SBA-15), which showed strong antibacterial activity. Ag-EDTA-SBA-15 exhibited stronger and more effective antibacterial activity than commercial Ag nanoparticles did, and it offered high stability of high valence silver in the porous matrix and long-lasting antibacterial activity. The synthesized materials were characterized using Fourier transform infrared spectroscopy, powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) analysis, and transmission electron microscopy (TEM). Ag existed in both surface complexation and Ag particles. EDTA anchored within a porous structure chelated Ag ions in higher oxidation states and prevented their agglomeration and oxidation reduction. The XRD results showed that most Ag in the Ag-EDTA-SBA-15 existed in higher oxidation states such as Ag(II) and Ag(III). However, the XPS and TEM results showed that Ag easily reduced in lower oxidation states and agglomerated as Ag particles on the exterior layer of the SBA-15. PMID:26742050

Combinatorial investigation of Fe–B thin-film nanocomposites

PubMed Central

Brunken, Hayo; Grochla, Dario; Savan, Alan; Kieschnick, Michael; Meijer, Jan D; Ludwig, Alfred

2011-01-01

Combinatorial magnetron sputter deposition from elemental targets was used to create Fe–B composition spread type thin film materials libraries on thermally oxidized 4-in. Si wafers. The materials libraries consisting of wedge-type multilayer thin films were annealed at 500 or 700 °C to transform the multilayers into multiphase alloys. The libraries were characterized by nuclear reaction analysis, Rutherford backscattering, nanoindentation, vibrating sample magnetometry, x-ray diffraction (XRD) and transmission electron microscopy (TEM). Young's modulus and hardness values were related to the annealing parameters, structure and composition of the films. The magnetic properties of the films were improved by annealing in a H2 atmosphere, showing a more than tenfold decrease in the coercive field values in comparison to those of the vacuum-annealed films. The hardness values increased from 8 to 18 GPa when the annealing temperature was increased from 500 to 700 °C. The appearance of Fe2B phases, as revealed by XRD and TEM, had a significant effect on the mechanical properties of the films. PMID:27877435

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods

NASA Astrophysics Data System (ADS)

Sivakami, R.; Dhanuskodi, S.; Karvembu, R.

2016-01-01

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55 eV. BET measurements show a high specific surface area (SSA) of 118-133 m2/g and pore diameter (10-25 nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM.

Interfacial microanalysis of rubber tyre-cord adhesion and the influence of cobalt

NASA Astrophysics Data System (ADS)

Fulton, W. Stephen; Smith, Graham C.; Titchener, Keith J.

2004-01-01

The effect of cobalt-containing adhesion promoters on the structure and morphology of rubber-brass and rubber-tyre-cord interfaces before and after ageing has been investigated by X-ray photoelectron spectroscopy (XPS) depth profiling, glancing incidence X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect the cobalt adhesion promoters had upon the interface morphology as they suppressed the growth of crystalline dendrites normally associated with the ageing process was imaged in TEM using samples prepared by the focused ion beam (FIB) milling technique. XPS depth profiling through the interfaces revealed that different types of adhesion promoter influenced the amount and distribution of cobalt ions in the bonding layer. XRD demonstrated the influence that cobalt had upon the structure of the interface and subsequent crystallinity, with a lesser degree of crystallinity being associated with better adhesion performance. From the results a model for the effect of the Co chemistry of the adhesion promotor has been developed.

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

Graphene/Ruthenium Active Species Aerogel as Electrode for Supercapacitor Applications

PubMed Central

Gigot, Arnaud; Fontana, Marco; Pirri, Candido Fabrizio; Rivolo, Paola

2017-01-01

Ruthenium active species containing Ruthenium Sulphide (RuS2) is synthesized together with a self-assembled reduced graphene oxide (RGO) aerogel by a one-pot hydrothermal synthesis. Ruthenium Chloride and L-Cysteine are used as reactants. The hydrothermal synthesis of the innovative hybrid material occurs at 180 °C for 12 h, by using water as solvent. The structure and morphology of the hybrid material are fully characterized by Raman, XRD, XPS, FESEM and TEM. The XRD and diffraction pattern obtained by TEM display an amorphous nanostructure of RuS2 on RGO crystallized flakes. The specific capacitance measured in planar configuration in 1 M NaCl electrolyte at 5 mV s−1 is 238 F g−1. This supercapacitor electrode also exhibits perfect cyclic stability without loss of the specific capacitance after 15,000 cycles. In summary, the RGO/Ruthenium active species hybrid material demonstrates remarkable properties for use as active material for supercapacitor applications. PMID:29301192

Templated synthesis of nanoporous titania/nanocarbon composites

NASA Astrophysics Data System (ADS)

Mistry, Jayur

Hexagonally patterned (honeycomb structured) nano-porous titania finds distinct applications in the field of material science, electronics, and catalysis. The preparation of titania/nanocarbon composites was carried out using titanium iso-propoxide precursor and a viscous surfactant templated system arranged into nanoscopic channels of water and iso-octane. Nanocarbon was introduced into the titania pores, as it was dispersed into the water (used to increase the W0), while making templets. Prepared titania/nanocarbon composites were analyzed under scanning electron microscopy (SEM), transmission electron microscope (TEM), and X-ray diffraction (XRD) after a specific heat treatment. SEM and TEM allows us to see the morphology of the hexagonally patterned templates and XRD shows the change in the crystallinity of the titania after the heat treatment. Further tests are run with the Solartron™ CellTest potentiostat syste, which, allows us to study the electrical properties of the nanocomposites. The composites synthesized have wide applications in number of fields, including energy, sensors and electronics.

Structural and photoluminescence properties of Ce, Dy, Er-doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jayachandraiah, C.; Kumar, K. Siva; Krishnaiah, G., E-mail: ginnerik@gmail.com

2015-06-24

Undoped ZnO and rare earth elements (Ce, Dy and Er with 2 at. %) doped nanoparticles were synthesized by wet chemical co-precipitation method at 90°C with Polyvinylpyrrolidone (PVP) as capping agent. The structural, morphological, compositional and photoluminescence studies were performed with X-ray diffraction (XRD), Transmission electron microscopy (TEM), Energy dispersive spectroscopy (EDS), FTIR spectroscopy and Photoluminescence (PL) respectively. XRD results revealed hexagonal wurtzite structure with average particle size around 18 nm - 14 nm and are compatible with TEM results. EDS confirm the incorporation of Ce, Dy and Er elements into the host ZnO matrix and is validated by FTIR analysis. PLmore » studies showed a broad intensive emission peak at 558 nm in all the samples. The intensity for Er- doped ZnO found maximum with additional Er shoulder peaks at 516nm and 538 nm. No Ce, Dy emission centers were found in spectra.« less

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

PubMed

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Synthesis and characterization of CdO nano particles by the sol-gel method

NASA Astrophysics Data System (ADS)

Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

2017-05-01

Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.

Thermal stability and electrochemical properties of PVP-protected Ru nanoparticles synthesized at room temperature

NASA Astrophysics Data System (ADS)

Kumar, Manish; Devi, Pooja; Shivling, V. D.

2017-08-01

Stable ruthenium nanoparticles (RuNPs) have been synthesized by the chemical reduction of ruthenium trichloride trihydrate (RuCl3 · 3H2O) using sodium borohydride (NaBH4) as a reductant and polyvinylpyrrolidone (PVP) as a protecting agent in the aqueous medium at room temperature. The nanoparticles thus prepared were characterized by their morphology and structural analysis from transmission electron microscopy (TEM), X-ray powder diffraction (XRD), UV-vis spectroscopy, Fourier transformation infrared and thermogravimetric analysis (TGA) techniques. The TEM image suggested a homogeneous distribution of PVP-protected RuNPs having a small average diameter of 2-4 nm with a chain-like network structure. The XRD pattern also confirmed that a crystallite size is around 2 nm of PVP-protected RuNPs having a single broad peak. The thermal stability studied using TGA, indicated good stability and the electrochemical properties of these nanoparticles revealed that saturation current increases for PVP-protected RuNPs/GC.

Experimental investigation of the ordering pathway in a Ni-33 at.%Cr alloy

DOE PAGES

Gwalani, B.; Alam, T.; Miller, C.; ...

2016-06-17

The present study involves a detailed experimental investigation of the concurrent compositional clustering and long-range ordering tendencies in a Ni-33 at.%Cr alloy, carried out by coupling synchrotron-based X-ray diffraction (XRD), transmission electron microscopy (TEM), and atom probe tomography (APT). Synchrotron-based XRD results clearly exhibited progressively increasing lattice contraction in the matrix with increasing isothermal aging time, at 475 degrees C, eventually leading to the development of long-range ordering (LRO) of the Pt2Mo-type. Detailed TEM and APT investigations revealed that this LRO in the matrix is manifested in the form of nanometer-scale ordered domains, and the spatial distribution, size, morphology andmore » compositional evolution of these domains have been carefully investigated. Here, the APT results also revealed the early stages of compositional clustering prior to the onset of long-range ordering in this alloy and such compositional clustering can potentially be correlated to the lattice contraction and previously proposed short-range ordering tendencies.« less

Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method

NASA Astrophysics Data System (ADS)

Wang, Shifa; Li, Danming; Xiao, Yuhua; Dang, Wenqiang; Feng, Jie

2017-10-01

A modified polyacrylamide gel route was used to prepare SrFe12O19 magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe12O19 magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm-1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe12O19 magnetic nanoparticles are uniform with the mean particle size of 60 nm. VSM measurement shows that the maximum magnetic energy product (BH)max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.

Structural and magnetic characterizations of Co2FeGa/SiO2 nanoparticles prepared via chemical route

NASA Astrophysics Data System (ADS)

Priyanka, Dhaka, Rajendra S.

2018-04-01

We report the synthesis of Co2FeGa/SiO2 nanoparticles by sol-gel method and characterization usingx-ray diffraction (XRD), transmission electron microscopy (TEM) and magnetic measurements. The Rietveld refinementsof XRD data with space group Fm-3m clearly show the formation of A2 disordersingle phase and the lattice constant isfound to be 5.738 Å. The energy-dispersive x-ray spectroscopy (EDX) confirm the elemental composition close the desired values. The value of coercivity is found to be around 283 Oe and 126 Oe, measured at 10 K and 300 K, respectively. We observed the saturation magnetization significantly lower than expected from Slater-Pauling rule. This decrease in the magnetic moment might be due to the presence of amorphous SiO2 during the synthesis process. A large content of small size SiO2 particles along with Co2FeGa nanoparticles are also found in TEM study.

Synthesis, characterization and antimicrobial activity of dextran stabilized silver nanoparticles in aqueous medium.

PubMed

Bankura, K P; Maity, D; Mollick, M M R; Mondal, D; Bhowmick, B; Bain, M K; Chakraborty, A; Sarkar, J; Acharya, K; Chattopadhyay, D

2012-08-01

A simple one-step rapid synthetic route is described for the preparation of silver nanoparticles by reduction of silver nitrate (AgNO3) using aqueous dextran solution which acts as both reducing and capping agent. The formation of silver nanoparticles is assured by characterization with UV-vis spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The absorbance of the silver nanoparticles is observed at 423 nm. The AFM image clearly shows the surface morphology of the well-dispersed silver nanoparticles with size range of 10-60 nm. TEM images show that the nanoparticles are spherical in shape with ∼5-10 nm dimensions. The crystallinity of Ag nanoparticles is assured by XRD analysis. The antimicrobial activity of as synthesized silver nanoparticles is tested against the bacteria, Bacillus subtilis, Bacillus cereus, Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa. The bacterial growth is inhibited by gradual reduction of the concentration of the silver nanoparticles. Copyright © 2012 Elsevier Ltd. All rights reserved.

Chitosan nanocomposite films based on Ag-NP and Au-NP biosynthesis by Bacillus Subtilis as packaging materials.

PubMed

Youssef, Ahmed M; Abdel-Aziz, Mohamed S; El-Sayed, Samah M

2014-08-01

Chitosan-silver (CS-Ag) and Chitosan-gold (CS-Au) nanocomposites films were synthesized by a simple chemical method. A local bacterial isolate identified as Bacillus subtilis ss subtilis was found to be capable to synthesize both silver nanoparticles (Ag-NP) and gold nanoparticles (Au-NP) from silver nitrate (AgNO3) and chloroauric acid (AuCl(4-)) solutions, respectively. The biosynthesis of both Ag-NP and Au-NP characterize using UV/vis spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD), and then added to chitosan by different ratios (0.5, 1 and 2%). The prepared chitosan nanocomposites films were characterize using UV, XRD, SEM and TEM. Moreover, the antibacterial activity of the prepared films was evaluated against gram positive (Staphylococcus aureus) and gram negative bacteria (Pseudomonas aerugenosa), fungi (Aspergillus niger) and yeast (Candida albicans). Therefore, these materials can be potential used as antimicrobial agents in packaging applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of biocompatible magnetite-carboxymethyl cellulose nanocomposite: characterization of nanocomposite by FTIR, XRD, FESEM and TEM.

PubMed

Habibi, Neda

2014-10-15

The preparation and characterization of magnetite-carboxymethyl cellulose nano-composite (M-CMC) material is described. Magnetite nano-particles were synthesized by a modified co-precipitation method using ferrous chloride tetrahydrate and ferric chloride hexahydrate in ammonium hydroxide solution. The M-CMC nano-composite particles were synthesized by embedding the magnetite nanoparticles inside carboxymethyl cellulose (CMC) using a freshly prepared mixture of Fe3O4 with CMC precursor. Morphology, particle size, and structural properties of magnetite-carboxymethyl cellulose nano-composite was accomplished using X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. As a result, magnetite nano-particles with an average size of 35nm were obtained. The biocompatible Fe3O4-carboxymethyl cellulose nano-composite particles obtained from the natural CMC polymers have a potential range of application in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Degradation product analysis from the photocatalytic oxidation/reduction of 2,4-dichlorophenol in the presence of mesoporous silica encapsulated TiO2 particles and TiO2 dispersions (presentation)

EPA Science Inventory

Thin films of Degussa P-25 TiO2 encapsulated in an SBA-15 mesoporous silica matrix were prepared. The TiO2/SBA-15 thin film structure was verified using transmission electron microscopy (TEM) and small angle X-ray diffraction (XRD). During irradiation with 350 nm light, the TiO...

Micro-emulsion-assisted synthesis of ZnS nanospheres and their photocatalytic activity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li Yao; He Xiaoyan; Cao Minhua

2008-11-03

ZnS nanospheres with rough surface were synthesized by using a micro-emulsion-assisted solvothemal process. The molar ratio of [water]/[surfactant] played an important role in controlling the size of the ZnS nanospheres. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field emission-scanning electron microscope (FE-SEM), and selected area electron diffraction (SAED) were used for the characterization of the resulting ZnS nanospheres. A possible formation mechanism was proposed. These ZnS nanospheres exhibited a good photocatalytic activity for degradation of an aqueous p-nitrophenol solution and the total organic carbon (TOC) of the degradation product has also been investigated.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamada, H., E-mail: hide-yamada@mg.ngkntk.co.jp; Matsuoka, T.; Kozuka, H.

Two phases of (K,Na)NbO{sub 3} (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K{sub 1−x}Na{sub x}){sub 0.86}Ca{sub 0.04}Li{sub 0.02}Nb{sub 0.85}O{sub 3−δ}–0.042K{sub 0.85}Ti{sub 0.85}Nb{sub 1.15}O{sub 5} –0.036BaZrO{sub 3}–0.0016Co{sub 3}O{sub 4}– 0.0025Fe{sub 2}O{sub 3}–0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains ofmore » the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, k{sub p} = 0.56, has been observed at the composition x = 0.56.« less

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

NASA Astrophysics Data System (ADS)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

Biogenic silver nanoparticles: efficient and effective antifungal agents

NASA Astrophysics Data System (ADS)

Netala, Vasudeva Reddy; Kotakadi, Venkata Subbaiah; Domdi, Latha; Gaddam, Susmila Aparna; Bobbu, Pushpalatha; Venkata, Sucharitha K.; Ghosh, Sukhendu Bikash; Tartte, Vijaya

2016-04-01

Biogenic synthesis of silver nanoparticles (AgNPs) by exploiting various plant materials is an emerging field and considered green nanotechnology as it involves simple, cost effective and ecofriendly procedure. In the present study AgNPs were successfully synthesized using aqueous callus extract of Gymnema sylvestre. The aqueous callus extract treated with 1nM silver nitrate solution resulted in the formation of AgNPs and the surface plasmon resonance (SPR) of the formed AgNPs showed a peak at 437 nm in the UV Visible spectrum. The synthesized AgNPs were characterized using Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and X-ray diffraction spectroscopy (XRD). FTIR spectra showed the peaks at 3333, 2928, 2361, 1600, 1357 and 1028 cm-1 which revealed the role of different functional groups possibly involved in the synthesis and stabilization of AgNPs. TEM micrograph clearly revealed the size of the AgNPs to be in the range of 3-30 nm with spherical shape and poly-dispersed nature; it is further confirmed by Particle size analysis that the stability of AgNPs is due its high negative Zeta potential (-36.1 mV). XRD pattern revealed the crystal nature of the AgNPs by showing the braggs peaks corresponding to (111), (200), (220) and (311) planes of face-centered cubic crystal phase of silver. Selected area electron diffraction pattern showed diffraction rings and confirmed the crystalline nature of synthesized AgNPs. The synthesized AgNPs exhibited effective antifungal activity against Candida albicans, Candida nonalbicans and Candida tropicalis.

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

Radiation-Induced Changes in Quartz, A Mineral Analog of Nuclear Power Plant Concrete Aggregates

DOE PAGES

Silva, Chinthaka M.; Rosseel, Thomas M.; Kirkegaard, Marie C.

2018-03-07

Quartz single-crystal samples consisting of α-quartz crystal structure were neutron irradiated to fluences of 5 × 10 18, 4 × 10 19, and 2 × 10 20 n/cm 2 (E > 0.1 MeV) at two temperatures (52 and 95 °C). The changes in the α-quartz phase as a function of these two conditions (temperature and fluence) were studied using X-ray powder diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM), and the results acquired using these complementary techniques are presented in a single place for the first time. XRD studies showed that the lattice parameters of α-quartz increased with increasingmore » neutron flux. The lattice growth was larger for the samples that were neutron irradiated at 52 °C than at 95 °C. Moreover, an amorphous content was determined in the quartz samples neutron irradiated at 4 × 10 19 n/cm 2, with the greater amount being in the 52 °C irradiated sample. Complete amorphization of quartz was observed at a fluence of 2 × 10 20 n/cm 2 (E > 0.1 MeV) using XRD and confirmed by TEM characterization and Raman spectroscopic studies. In conclusion, the cause for α-quartz lattice expansion and sample amorphization was also explored using XRD and Raman spectroscopic studies.« less

In situ supported MnOx-CeOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

NASA Astrophysics Data System (ADS)

Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

2013-01-01

The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods. Electronic supplementary information (ESI) available: SEM images and EDS analysis, TEM images, and XPS spectrum of samples. See DOI: 10.1039/c2nr33006g

X-ray diffraction study of the mineralogy of microinclusions in fibrous diamond

NASA Astrophysics Data System (ADS)

Smith, Evan; Kopylova, Maya; Dubrovinksy, Leonid

2010-05-01

Fibrous diamond, occurring both as cuboids and as coatings over non-fibrous diamond nuclei, is translucent due to the presence of millions of sub-micron-sized mineral and fluid inclusions. Diamond is strong and relatively inert, making it an excellent vessel to preserve trapped materials. These microinclusions represent direct samples of natural diamond-forming mantle fluids, and are critical for our understanding of diamond genesis. Traditionally, infrared spectroscopy, Raman spectroscopy, secondary ion mass spectrometry, electron microprobe, and FIB-TEM techniques have proven to be effective for the study of microinclusions in diamond. The abundance and random orientation of included minerals in fibrous diamond make them amenable to a powder-type X-ray diffraction (XRD) technique. This technique provides an accurate way to identify included minerals. It also has the advantage of analyzing thousands of inclusions simultaneously, rather than analyzing one inclusion at a time, as with common FIB-TEM techniques. XRD provides a bulk analysis, giving a superior measure of relative abundances of included minerals, as well as potentially accounting for small quantities of minerals that might otherwise be overlooked. We studied fibrous cuboid diamonds with microinclusions from the Democratic Republic of Congo (DRC) (23 samples), Brazil (4 samples), Jericho (1 sample), and Wawa conglomerates (9 samples). XRD analysis was performed at the Bayerisches Geoinstitut (BGI), University of Bayreuth, Germany. The unique XRD setup consists of a RIGAKU FR-D high-brilliance source, OSMIC Inc. Confocal Max-Flux optics, and a SMART APEX 4K CCD area detector. Preliminary XRD studies of microinclusions 8 fibrous diamonds from the DRC showed a prevalence of silicates with structural and coordinated H2O. Sheet silicates constituted 9 out of 13 detected minerals, with phlogopite-biotite micas being present in 4 out of 8 samples. Other detected minerals were 2 chlorite minerals, 2 clay phyllosilicates, serpentine, zircon, a hydrous carbonate and an unidentified zeolite. Many of these phases are deuteric, replacing high-T, high-P micas and carbonates that precipitate from the fluid in the diamond stability field. The ongoing XRD study will (1) elucidate the mineralogy of fluid inclusions in diamonds from Wawa, (2) compare XRD analyses to distinguish between diamonds with carbonatitic versus saline fluid compositions, and (3) reveal whether carbonates occur as crystalline phases or as dissolved or amorphous material in fibrous diamond.

Poly(vinylpyrrolidone) coated iron nanoparticles in polar aprotic solvent.

PubMed

Ban, Zhihui; Cushing, Brian L; O'Connor, Charles J

2008-04-01

Poly(vinylpyrrolidone) (PVP) coated iron nanoparticles which show well-defined core-shell structures have been successfully synthesized in a polar aprotic solvent. In this approach, PVP was employed not as capping agent, but as coating polymer directly applied to the metallic (iron) core nanoparticles. The morphologies, structures, compositions and magnetic properties of the products were investigated by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDXS), SQUID magnetometry and FTIR spectroscopy.

Photosynthetic microorganism-mediated synthesis of akaganeite (beta-FeOOH) nanorods.

PubMed

Brayner, Roberta; Yéprémian, Claude; Djediat, Chakib; Coradin, Thibaud; Herbst, Fréderic; Livage, Jacques; Fiévet, Fernand; Couté, Alain

2009-09-01

Common Anabaena and Calothrix cyanobacteria and Klebsormidium green algae are shown to form intracellularly akaganeite beta-FeOOH nanorods of well-controlled size and unusual morphology at room temperature. X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy X-ray energy dispersive spectrometry (SEM-EDS) analyses are used to investigate particle structure, size, and morphology. A mechanism involving iron-siderophore complex formation is proposed and compared with iron biomineralization in magnetotactic bacteria.

Discontinuous precipitation in a nickel-free high nitrogen austenitic stainless steel on solution nitriding

NASA Astrophysics Data System (ADS)

Mohammadzadeh, Roghayeh; Akbari, Alireza; Grumsen, Flemming B.; Somers, Marcel A. J.

2017-10-01

Chromium-rich nitride precipitates in production of nickel-free austenitic stainless steel plates via pressurised solution nitriding of Fe-22.7Cr-2.4Mo ferritic stainless steel at 1473 K (1200 °C) under a nitrogen gas atmosphere was investigated. The microstructure, chemical and phase composition, morphology and crystallographic orientation between the resulted austenite and precipitates were investigated using optical microscopy, X-ray Diffraction (XRD), Scanning and Transmission Electron Microscopy (TEM) and Electron Back Scatter Diffraction (EBSD). On prolonged nitriding, Chromium-rich nitride precipitates were formed firstly close to the surface and later throughout the sample with austenitic structure. Chromium-rich nitride precipitates with a rod or strip-like morphology was developed by a discontinuous cellular precipitation mechanism. STEM-EDS analysis demonstrated partitioning of metallic elements between austenite and nitrides, with chromium contents of about 80 wt.% in the precipitates. XRD analysis indicated that the Chromium-rich nitride precipitates are hexagonal (Cr, Mo)2N. Based on the TEM studies, (Cr, Mo)2N precipitates presented a (1 1 1)γ//(0 0 2)(Cr, Mo)2N, ?γ//?(Cr, Mo)2N orientation relationship with respect to the austenite matrix. EBSD studies revealed that the austenite in the regions that have transformed into austenite and (Cr, Mo)2N have no orientation relation to the untransformed austenite.

Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uvarov, Vladimir, E-mail: vladimiru@savion.huji.ac.il; Popov, Inna

2013-11-15

Crystallite size values were determined by X-ray diffraction methods for 183 powder samples. The tested size range was from a few to about several hundred nanometers. Crystallite size was calculated with direct use of the Scherrer equation, the Williamson–Hall method and the Rietveld procedure via the application of a series of commercial and free software. The results were statistically treated to estimate the significance of the difference in size resulting from these methods. We also estimated effect of acquisition conditions (Bragg–Brentano, parallel-beam geometry, step size, counting time) and data processing on the calculated crystallite size values. On the basis ofmore » the obtained results it is possible to conclude that direct use of the Scherrer equation, Williamson–Hall method and the Rietveld refinement employed by a series of software (EVA, PCW and TOPAS respectively) yield very close results for crystallite sizes less than 60 nm for parallel beam geometry and less than 100 nm for Bragg–Brentano geometry. However, we found that despite the fact that the differences between the crystallite sizes, which were calculated by various methods, are small by absolute values, they are statistically significant in some cases. The values of crystallite size determined from XRD were compared with those obtained by imaging in a transmission (TEM) and scanning electron microscopes (SEM). It was found that there was a good correlation in size only for crystallites smaller than 50 – 60 nm. Highlights: • The crystallite sizes for 183 nanopowders were calculated using different XRD methods • Obtained results were subject to statistical treatment • Results obtained with Bragg-Brentano and parallel beam geometries were compared • Influence of conditions of XRD pattern acquisition on results was estimated • Calculated by XRD crystallite sizes were compared with same obtained by TEM and SEM.« less

Facile synthesis of Co3O4 hexagonal plates by flux method

NASA Astrophysics Data System (ADS)

Han, Ji-Long; Meng, Qing-Fen; Gao, Sheng-Li

2018-01-01

Using a novel flux method, a hexagonal plate of Co3O4 was directly synthesized. In this method, CoCl2·6H2O, NaOH, and the cosolvent H3BO3 were heated to 750 °C for 2 h in a corundum crucible. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscope (HRTEM). Furthermore, XRD studies indicated that the product consisted of a cubic phase of Co3O4, and the phase existed in a completely crystalline form. Then, SEM results indicated that these hexagonal plates tiered up and they had diameters in the range of 2-10 μm. According to the results of SAED and HRTEM analyses, the interlayer spacing was about 0.24 nm, which corresponds to the interlayer distance of (3 1 1) crystal plane of cubic Co3O4.

Endophytic fungal isolate mediated biosynthesis of silver nanoparticles and their free radical scavenging activity and anti microbial studies.

PubMed

Netala, Vasudeva Reddy; Kotakadi, Venkata Subbaiah; Bobbu, Pushpalatha; Gaddam, Susmila Aparna; Tartte, Vijaya

2016-12-01

The present study reports that the biosynthesis of AgNPs using an endophytic fungus isolated from the ethnomedicinal plant Centella asiatica. The endophytic fungus was identified as Aspergillus versicolor ENT7 based on 18S rRNA gene sequencing (NCBI Accession number KF493864). The AgNPs synthesized were characterized by UV-visible spectroscopy, Fourier transform infra-red spectroscopy (FTIR), transmission electron microscopy (TEM), X-ray diffraction (XRD), particle size analyzer, and zeta potential measurements. The UV-Vis absorption spectra showed the peak at 429 nm which confirmed the synthesis of AgNPs. TEM analysis revealed that the AgNPs were spherical in shape with 3-40 nm in size; similar results were also obtained by Horiba particle size analyzer with 5-40 nm in size. The synthesized AgNPs were highly stable due to their high negative zeta potential value of -38.2 mV. XRD studies showed (111), (200), (220), (311), and (222) planes of the face-centered cubic (FCC) lattice, indicating the crystalline nature of the AgNPs. Selected area electron diffraction (SAED) pattern of the AgNPs showed five circular fringes which were in accordance with XRD data and confirmed the formation of high crystalline nature of AgNPs. FTIR measurements indicated the peaks at 3273, 2925, 1629, 1320, and 1020 cm -1 corresponding to different functional groups possibly involved in the synthesis and stabilization of AgNPs. The synthesized AgNPs exhibited effective free radical scavenging activity with the IC50 value of 60.64 µg/ml. The synthesized AgNPs were found to be highly toxic against both gram-positive and gram-negative bacteria and also showed a very good antifungal activity.

The use of castor oil and ricinoleic acid in lead chalcogenide nanocrystal synthesis

NASA Astrophysics Data System (ADS)

Kyobe, Joseph W. M.; Mubofu, Egid B.; Makame, Yahya M. M.; Mlowe, Sixberth; Revaprasadu, Neerish

2016-08-01

A green solution-based thermolysis method for the synthesis of lead chalcogenide (PbE, E = S, Se, Te) nanocrystals in castor oil (CSTO) and its isolate ricinoleic acid (RA) is described. The blue shift observed from the optical spectra of CSTO and RA-capped PbE nanocrystals (NCs) confirmed the evidence of quantum confinement. The dimensions of PbE NCs obtained from NIR absorption spectra, transmission electron microscopy (TEM), and X-ray diffraction (XRD) studies were in good agreement. The particle sizes estimated were in the range of 20, 25, and 130 nm for castor oil-capped PbS, PbSe, and PbTe, respectively. Well-defined close to cubic-shaped particles were observed in the scanning electron microscopy (SEM) images of PbSe and PbTe nanocrystals. The high-resolution TEM and selective area electron diffraction (SAED) micrographs of the as-synthesized crystalline PbE NCs showed distinct lattice fringes with d-spacing distances corroborating with the standard values reported in literature.

Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

NASA Astrophysics Data System (ADS)

Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

2013-06-01

Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed ( Kappaphycus alvarezii) Extract

NASA Astrophysics Data System (ADS)

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-06-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii ( K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm-1, which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.

Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed (Kappaphycus alvarezii) Extract.

PubMed

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-12-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii (K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm(-1), which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Structural, magnetic and dielectric properties of polyaniline/MnCoFe2O4 nanocomposites

NASA Astrophysics Data System (ADS)

Chitra, Palanisamy; Muthusamy, Athianna; Jayaprakash, Rajan

2015-12-01

Ferromagnetic PANI containing MnCoFe2O4 nanocomposites were synthesized by in-situ chemical polymerization of aniline incorporated MnCoFe2O4 nanoparticles (20%, 10% w/w of fine powders) with and without ultrasonic treatment. The MnCoFe2O4 nanoparticles were synthesized by auto combustion method. The PANI/MnCoFe2O4 nanocomposites were characterized with Fourier transform infrared (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The average particle size of the resulting PANI/MnCoFe2O4 nanocomposites was confirmed from the TEM and XRD analysis. The structure and morphology of the composites were confirmed by FT-IR spectroscopy, XRD and SEM. In addition, the electrical and magnetic properties of the nanocomposites were investigated. The PANI/MnCoFe2O4 nanocomposites under applied magnetic field exhibited the hysteresis loops of ferromagnetic nature at room temperature. The variation of Dielectric constant, Dielectric loss, and AC conductivity of PANI/MnCoFe2O4 nanocomposites at room temperature as a function of frequency in the range 50 Hz-5 MHz has been studied. Effect of ultrasonication on the PANI/MnCoFe2O4 nanocomposites was also investigated.

Surfactant-free bio-synthesised Tio2 nanorods from Turbinaria conoides-a study on photocatalytic and anti-bacterial activity

NASA Astrophysics Data System (ADS)

Subhapriya, S.; Gomathipriya, P.

2018-06-01

In this study, Titania nanorods were synthesised from aqueous extract of Turbinaria conoides (brown seaweeds) (TiO2NRs-TC) under surfactant free medium. The photocatalytic activity of the synthesised nanorods was tested towards the photocatalytic decolourization using simulated dye wastewater containing Navy Blue HER (NBHER). The synthesised Titania nanorods were characterized by using x-ray diffraction (XRD), UV–visible spectroscopy (UV–vis), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrophotometer (EDS) and Transmission Electron Microscopy (TEM). XRD pattern confirms the anatase phase formation and HR-SEM micrograph shows the presence of rod like structure with the size of about 50 nm. TEM analysis proves the rod like structure with a size of 45–50 nm which was in agreement with the XRD analysis and HR-SEM images. EDS and XDS confirmed the formation of Titania nanoparticles. The formation of TiO2NRs-TC has a beneficial influence on the dye Navy blue HER photodegradation. TiO2-TC nano rods also show superior photocatalytic ability in hydrogen generation (2.1 mmol/h‑1g‑1). The antibacterial activity of the synthesised nanoparticles was examined using disc diffusion method which showed diverse susceptibility of microorganisms to the Titania nanoparticles.

Biosorption and biotransformation of chromium by Serratia sp. isolated from tannery effluent.

PubMed

Srivastava, Shaili; Thakur, Indu Shekhar

2012-01-01

A bacterium isolated from soil and sediment ofa leather tanning mill's effluent was identified as Serratia sp. by the analysis of 16S rDNA. Scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX) and transmission electron microscopy (TEM) were used to assess morphological changes and confirm chromium biosorption in Serratia sp. both in a shake-flask culture containing chromium and in a tannery wastewater. The SEMEDX and the elemental analysis of the chromate-containing samples confirmed the binding of chromium with the bacterial biomass. The TEM exhibited chromium accumulation throughout the bacterial cell, with some granular deposits in the cell periphery and in the cytoplasm. X-ray diffraction analysis (XRD) was used to quantify the chromium and to determine the chemical nature of the metal-microbe interaction. The XRD data showed the crystalline character of the precipitates, which consisted of mainly calcium chromium oxide, chromium fluoride phosphate and related organo-Cr(III) complex crystals. The XRD data also revealed a strong involvement of cellular carboxyl and phosphate groups in chromium binding by the bacterial biomass. The results of the study indicated that a combined mechanism of ion-exchange, complexation, croprecipitation and immobilization was involved in the biosorption of chromium by bacterial cells in contaminated environments.

One step synthesis of porous graphene by laser ablation: A new and facile approach

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

Porous graphene (PG) was obtained using one step laser process. Synthesis was carried out by laser ablation of nickel-graphite target under ultra-high flow of argon gas. The field emission scanning electron microscopy (FE-SEM) results showed the formation of a porous structure and the transmission electron microscopy (TEM) revealed that the porosity of PGs increase under intense laser irradiation. Structural characterization study using Raman spectroscopy, X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) technique showed that the obtained PGs display high crystalline structure in the form of few layer rhombohedral graphitic arrangement that can be interpreted as the phase prior to the formation of other carbon nanostructures.

XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

PubMed

Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

2013-12-01

The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

A facile synthesis of metal nanoparticle - graphene composites for better absorption of solar radiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Bindu; Mulla, Rafiq; Rabinal, M. K., E-mail: mkrabinal@yahoo.com

2015-06-24

Herein, a facile chemical approach has been adopted to prepare silver nanoparticles (AgNPs)- graphene (G) composite to study photothermal effect. Sodium borohydride (SBH), a strong reducing agent has been selected for this work. Effect of SBH concentrations on optical behavior of AgNPs-G composite was also investigated. Resultant materials were characterized by various techniques including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), optical absorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM micrographs confirm wrapping of AgNPs into graphene whereas XRD analysis reveals their particle size variation between 47 nm to 69 nm. Optical studies throw a light on theirmore » strong absorption behavior towards solar radiation.« less

Intrinsic ferromagnetism in nanocrystalline Mn-doped ZnO depending on Mn concentration.

PubMed

Subramanian, Munisamy; Tanemura, Masaki; Hihara, Takehiko; Soga, Tetsuo; Jimbo, Takashi

2011-04-01

The physical properties of Zn(1-x)Mn(x)O nanoparticles synthesized by thermal decomposition are extensively investigated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman light scattering and Hysteresis measurements. XRD and XPS spectra reveal the absence of secondary phase in nanocrystalline ZnO doped with 5% or less Mn; and, later confirms that the valance state of Mn to be 2+ for all the samples. Raman spectra exhibit a peak at 660 cm(-1) which we attribute to the intrinsic lattice defects of ZnO with increasing Mn concentration. Overall, our results demonstrate that ferromagnetic properties can be realized while Mn-doped ZnO obtained in the nanocrystalline form.

Characterization of BN rich layer on ammonia treated Nextel{trademark}312 fibers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khasgiwale, N.R.; Butler, E.P.; Tsakalakos, L.

A BN rich layer grown on Nextel{trademark}312 fibers by appropriate ammonia treatments was evaluated using various complimentary techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM)/Parallel Electron Energy Loss Spectroscopy (PEELS in TEM). Three different ammonia treatments were studied. Ammonia treatment resulted in crystallization of the Nextel{trademark}312 fiber. The BN rich surface layer formed due to ammonia treatment was clearly detected in XPS and PEELS both before and after oxidation. The layer thickness was estimated to be between 5--10 nm. The layer was stable after oxidation treatment at 600 C formore » 100 hours. High resolution TEM observations of the fiber surface revealed a variable BN rich layer thickness. Patches of turbostratic BN were observed under certain conditions, however mostly the layer appeared to be amorphous.« less

Preparation and characterization of bismuth oxichloride (BiOCl) nanoparticles and nano zerovalent iron (nZVI)

NASA Astrophysics Data System (ADS)

Sarwan, Bhawna; Pare, Brijesh; Deep Acharya, Aman

2017-05-01

In this work, we have synthesized nano scale zerovalent iron (nZVI) particles by borohydride reduction method and bismuth oxichloride (BiOCl) by a hydrolysis method. X-ray powder diffraction (XRD) was used for the structural and chemical characterization, while scanning/transmission electron microscopy (SEM/TEM) were employed to determine the physical properties of the nanoparticles. The reactivity of synthesized nanoparticles was compared by decolorization of nile blue (NB) dye under visible irradiation.

Synthesis and characterization of some metal oxide nanocrystals by microwave irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rashad, M.; Gaber, A.; Abdelrahim, M. A.

2013-12-16

Copper oxide and cobalt oxide (CuO, Co3O4) nanocrystals (NCs) have been successfully prepared in a short time using microwave irradiation. The resulted powders of nanocrystals (NCs) were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Thermogravimetric analysis (TGA) measurements are also studied. Fourier-transform infrared (FT-IR) and UV–visible absorption spectroscopy of both kind of nanoparticels are illustrated. Optical absorption analysis indicated the direct band gap for both kinds of nanocrystals.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan Qingtao; Huang Kai; Ni Shibing

Well-crystalline flower- and rod-like NiS nanostructures have been synthesized by an organic-free hydrothermal process at a low temperature of 200 deg. C. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) were employed to characterize the as-synthesized NiS nanostructures. The effects of temperature and reaction time on the morphology have been also investigated. The two-step flake-cracking mechanism for the formation of flower- and rod-like NiS nanostructures was discussed. The products were also investigated by photoluminescence (PL) spectroscopy.

Novel Crystalline SiO2 Nanoparticles via Annelids Bioprocessing of Agro-Industrial Wastes

PubMed Central

2010-01-01

The synthesis of nanoparticles silica oxide from rice husk, sugar cane bagasse and coffee husk, by employing vermicompost with annelids (Eisenia foetida) is reported. The product (humus) is calcinated and extracted to recover the crystalline nanoparticles. X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and dynamic light scattering (DLS) show that the biotransformation allows creating specific crystalline phases, since equivalent particles synthesized without biotransformation are bigger and with different crystalline structure. PMID:20802789

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

NASA Astrophysics Data System (ADS)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

Combustion synthesis and characterization of blue long lasting phosphor CaAl2O4: Eu2+, Dy3+ and its novel application in latent fingerprint and lip mark detection

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vijay; Kumar, Vinay; Verma, Kartikey; Swart, H. C.

2018-04-01

This work investigates the structural, optical and photometric characterization of a Eu2+/Dy3+ doped calcium aluminates phosphor (CaAl2O4: Eu2+/Dy3+) for finger and lip print detections. Synthesis of CaAl2O4: Eu2+/Dy3+ (CAED) phosphors were carried out via a combustion synthesis method with urea as a fuel. Eu2+/Dy3+ doped CaAl2O4 phosphors have been studied with X-ray diffraction (XRD, Energy Dispersive X-Ray Spectroscopy Selected Area Diffraction (SAED) and High resolution Transmission Electron Microscope (HR-TEM). The XRD pattern shows that the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphor have a single monoclinic structure and show that the addition of the dopant/co-dopants didn't change the crystal structure. The formation of monoclinic phase was confirmed by the selected area diffraction pattern. The TEM micrograph displays the morphology of the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphors as spherical particles with an average particle size of 33 nm. The optical band gap was calculated using the diffuse reflectance for the synthesized nanophosphor powders. The photoluminescence emission spectra was recorded for the synthesized powder, with an excitation wavelength of 326 nm and the major bands was recorded at 447 nm corresponding to the blue color and two minor bands were recorded at 577 nm and 616 nm. To the best of our knowledge, this work is the first to show the use of CaAl2O4: Eu2+/Dy3+ nanophosphor in developing latent fingerprint and lip print effectively.

The effect of PVP on morphology, optical properties and electron paramagnetic resonance of Zn0.5Co0.5Fe2-xPrxO4 nanoparticles

NASA Astrophysics Data System (ADS)

Bitar, Z.; El-Said Bakeer, D.; Awad, R.

2017-07-01

Zinc Cobalt nano ferrite doped with Praseodymium, Zn0.5Co0.5Fe2-xPrxO4 (0 ≤ x ≤ 0.2), were prepared by co-precipitation method from an aqueous solution containing metal chlorides and two concentrations of poly(vinylpyrrolidone) (PVP) 0 and 30g/L as capping agent. The samples were characterized using X-ray powder diffraction (XRD), Transmission Electron Microscope (TEM), UV-visible optical spectroscopy, Fourier transform infrared (FTIR) and Electron Paramagnetic Resonance (EPR). XRD results display the formation of cubic spinel structure with space group Fd3m and the lattice parameter (a) is slightly decreased for PVP capping samples. The particle size that determined by TEM, decreases for PVP capping samples. The optical band energy Eg increases for PVP capping samples, confirming the variation of energy gap with the particle size. The FTIR results indicate that the metal oxide bands were shifted for the PVP capping samples. EPR data shows that the PVP addition increases the magnetic resonance field and hence decreases the g-factor.

Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

PubMed

Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

2018-01-01

Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

NASA Astrophysics Data System (ADS)

Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

2018-01-01

The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

Matrix Dissolution Techniques Applied to Extract and Quantify Precipitates from a Microalloyed Steel

NASA Astrophysics Data System (ADS)

Lu, Junfang; Wiskel, J. Barry; Omotoso, Oladipo; Henein, Hani; Ivey, Douglas G.

2011-07-01

Microalloyed steels possess good strength and toughness, as well as excellent weldability; these attributes are necessary for oil and gas pipelines in northern climates. These properties are attributed in part to the presence of nanosized carbide and carbonitride precipitates. To understand the strengthening mechanisms and to optimize the strengthening effects, it is necessary to quantify the size distribution, volume fraction, and chemical speciation of these precipitates. However, characterization techniques suitable for quantifying fine precipitates are limited because of their fine sizes, wide particle size distributions, and low volume fractions. In this article, two matrix dissolution techniques have been developed to extract precipitates from a Grade100 (yield strength of 690 MPa) microalloyed steel. Relatively large volumes of material can be analyzed, and statistically significant quantities of precipitates of different sizes are collected. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) are combined to analyze the chemical speciation of these precipitates. Rietveld refinement of XRD patterns is used to quantify fully the relative amounts of the precipitates. The size distribution of the nanosized precipitates is quantified using dark-field imaging in the TEM.

Sonochemical method for producing titanium metal powder.

PubMed

Halalay, Ion C; Balogh, Michael P

2008-07-01

We demonstrate a sonochemical method for producing titanium metal powder. The method uses low intensity ultrasound in a hydrocarbon solvent at near-ambient temperatures to first create a colloidal suspension of liquid sodium-potassium alloy in the solvent and then to reduce liquid titanium tetrachloride to titanium metal under cavitation conditions. XRD data collected for the reaction products after the solvent removal show only NaCl and KCl, with no diffraction peaks attributable to titanium metal or other titanium compounds, indicating either the formation of amorphous metal or extremely small crystallite size. TEM micrographs show that hollow spheres formed of halide salts and titanium metal, with diameters with diameters ranging from 100 to 500 nm and a shell thickness of 20 to 40 nm form during the synthesis, suggesting that the sonochemical reaction occurs inside the liquid shell surrounding the cavitation bubbles. Metal particle sizes are estimated to be significantly smaller than 40 nm from TEM data. XRD data of the powder after annealing and prior to removal of the alkali chloride salts provides direct evidence that titanium metal was formed during the sonochemical synthesis.

UV-visible spectroscopic estimation of photodegradation of rhodamine-B dye using tin(IV) oxide nanoparticles.

PubMed

Sangami, G; Dharmaraj, N

2012-11-01

Nanocrystalline, tin(IV) oxide (SnO(2)) particles has been prepared by thermal decomposition of tin oxalate precursor obtained from the reactions of tin(IV) chloride and sodium oxalate using eggshell membrane (ESM). The as-prepared SnO(2) nanoparticles were characterized by thermal studies, transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Raman, FT-IR and UV-visible studies and used as a photocatalyst for the degradation of rhodamine-B (Rh-B) dye. The size of the prepared nanoparticles was in the range of 5-12nm as identified from the TEM images. Powder XRD data revealed the presence of a tetragonal, rutile crystalline phase of the tin(IV) oxide nanoparticles. Thermal analysis showed that the decomposition of tin oxalate precursor to yield the titled tin(IV) oxide nanoparticles was completed below 500°C. The extent of degradation of Rh-B in the presence of SnO(2) monitored by absorption spectral measurements demonstrated that 94.48% of the selected dye was degraded upon irradiation with UV light for 60 min. Copyright © 2012 Elsevier B.V. All rights reserved.

Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

NASA Astrophysics Data System (ADS)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

2016-05-01

A novel and facile approach for synthesis of spinel nickel ferrites (NiFe2O4) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe2O4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe2O4 and TEM image showed spherical particles of sizes 2-10 nm. These NiFe2O4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

Facile Synthesis of Calcium Borate Nanoparticles and the Annealing Effect on Their Structure and Size

PubMed Central

Erfani, Maryam; Saion, Elias; Soltani, Nayereh; Hashim, Mansor; Wan Abdullah, Wan Saffiey B.; Navasery, Manizheh

2012-01-01

Calcium borate nanoparticles have been synthesized by a thermal treatment method via facile co-precipitation. Differences of annealing temperature and annealing time and their effects on crystal structure, particle size, size distribution and thermal stability of nanoparticles were investigated. The formation of calcium borate compound was characterized by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and Thermogravimetry (TGA). The XRD patterns revealed that the co-precipitated samples annealed at 700 °C for 3 h annealing time formed an amorphous structure and the transformation into a crystalline structure only occurred after 5 h annealing time. It was found that the samples annealed at 900 °C are mostly metaborate (CaB2O4) nanoparticles and tetraborate (CaB4O7) nanoparticles only observed at 970 °C, which was confirmed by FTIR. The TEM images indicated that with increasing the annealing time and temperature, the average particle size increases. TGA analysis confirmed the thermal stability of the annealed samples at higher temperatures. PMID:23203073

Cytotoxicity Evaluation and Magnetic Characteristics of Mechano-thermally Synthesized CuNi Nanoparticles for Hyperthermia

NASA Astrophysics Data System (ADS)

Amrollahi, P.; Ataie, A.; Nozari, A.; Seyedjafari, E.; Shafiee, A.

2015-03-01

CuNi alloys are very well known, both in academia and industry, based on their wide range of applications. In the present investigation, the previously synthesized Cu0.5Ni0.5 nanoparticles (NPs) by mechano-thermal method were studied more extensively. Phase composition and morphology of the samples were studied by employing x-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) techniques. The Curie temperature ( T c) was determined by differential scanning calorimetry (DSC). In vitro cytotoxicity was studied through methyl-thiazolyl-tetrazolium (MTT) assay. XRD and FESEM results indicated the formation of single-phase Cu0.5Ni0.5. TEM micrographs showed that the mean particle size of powders is 20 nm. DSC results revealed that T c of mechano-thermally synthesized Cu0.5Ni0.5 is 44 °C. The MTT assay results confirmed the viability and proliferation of human bone marrow stem cells in contact with Cu0.5Ni0.5 NPs. In summary, the fabricated particles were demonstrated to have potential in low concentrations for cancer treatment applications.

Green Synthesis, Characterization and Application of Proanthocyanidins-Functionalized Gold Nanoparticles

PubMed Central

Biao, Linhai; Tan, Shengnan; Meng, Qinghuan; Gao, Jing; Zhang, Xuewei; Liu, Zhiguo; Fu, Yujie

2018-01-01

Green synthesis of gold nanoparticles using plant extracts is one of the more promising approaches for obtaining environmentally friendly nanomaterials for biological applications and environmental remediation. In this study, proanthocyanidins-functionalized gold nanoparticles were synthesized via a hydrothermal method. The obtained gold nanoparticles were characterized by ultraviolet and visible spectrophotometry (UV-Vis), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and X-ray diffraction (XRD) measurements. UV-Vis and FTIR results indicated that the obtained products were mainly spherical in shape, and that the phenolic hydroxyl of proanthocyanidins had strong interactions with the gold surface. TEM and XRD determination revealed that the synthesized gold nanoparticles had a highly crystalline structure and good monodispersity. The application of proanthocyanidins-functionalized gold nanoparticles for the removal of dyes and heavy metal ions Ni2+, Cu2+, Cd2+ and Pb2+ in an aqueous solution was investigated. The primary results indicate that proanthocyanidins-functionalized gold nanoparticles had high removal rates for the heavy metal ions and dye, which implies that they have potential applications as a new kind of adsorbent for the removal of contaminants in aqueous solution. PMID:29361727

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods.

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55eV. BET measurements show a high specific surface area (SSA) of 118-133m(2)/g and pore diameter (10-25nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM. Copyright © 2015 Elsevier B.V. All rights reserved.

Kyllinga brevifolia mediated greener silver nanoparticles

NASA Astrophysics Data System (ADS)

Isa, Norain; Bakhari, Nor Aziyah; Sarijo, Siti Halimah; Aziz, Azizan; Lockman, Zainovia

2017-12-01

Kyllinga brevifolia extract (KBE) was studied in this research as capping as well as reducing agent for the synthesis of greener plant mediated silver nanoparticles. This research was conducted in order to identify the compounds in the KBE that probable to work as reductant for the synthesis of Kyllinga brevifolia-mediated silver nanoparticles (AgNPs). Screening test such as Thin Layer Chromatography (TLC), Fourier Transform Infra-Red (FTIR), Carlo Erba Elemental analysis and Gas Chromatography-Mass Spectroscopy (GCMS) were used in identifying the natural compounds in KBE. The as-prepared AgNPs were characterized by UV-vis spectroscopy (UV-vis), Transmission Electron Microscope (TEM) and X-ray Diffraction (XRD). The TEM images showed that the as-synthesized silver have quasi-spherical particles are distributed uniformly with a narrow distribution from 5 nm to 40 nm. The XRD results demonstrated that the obtained AgNPs were face centre-cubic (FCC) structure. The catalytic activity of AgNPs on reduction of methylene blue (MB) using sodium borohydride (SB) was analyzed using UV-vis spectroscopy. This study showed that the efficacy of mediated AgNPs in catalysing the reduction of MB.

Molten salt synthesis and luminescent properties of YVO4:Ln (Ln = Eu3+, Dy3+) nanophosphors.

PubMed

Liu, Chenglu; Wang, Fang; Jia, Peiyun; Lin, Jun; Zhou, Zhiqiang

2012-01-01

Eu3+ and Dy(3+)-doped YVO4 nanocrystallites were successfully prepared at 400 degrees C in equal moles of NaNO3 and KNO3 molten salts. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, transmission electronic microscopy (TEM), photoluminescence (PL) spectrum and lifetime were used to characterize the nanocrystallites. XRD results demonstrate that NaOH concentration and annealing temperature play important roles in phase purity and crystallinity of the nanocrystallites, the optimum NaOH concentration and annealing temperature being 6:40 and 400 degrees C respectively. TEM micrographs show the nanocrystallites are well crystallized with a cubic morphology in an average grain size of about 18 nm. Upon excitation of the vanadate group at 314 nm, YVO4:Eu3+ and YVO4:Dy3+ nanocrystallites exhibit the characteristic emission of Eu3+ and Dy3+, which indicates that there is an energy transfer from the vanadate group to the rare earth ions. Moreover, the structure and luminescent properties of the nanocrystallites were compared with their bulk counterparts with same composition in detail.

Non-Metal Doped Titania Photocatalysts for the Degradation of Neonicotinoid Insecticides Under Visible Light Irradiation.

PubMed

Joseph, Amala Infant Joice; Thiripuranthagan, Sivakumar

2018-05-01

Recombination of e-/h+ pair, the major issue of any titania based photocatalytic material, is addressed here by doping non-metals such as C, N, B, F into the lattice of nano TiO2. The as-synthesised catalysts were characterized by using various instrumental techniques such as X-ray diffraction (XRD), UV-Diffuse reflectance spectroscopy (UV-DRS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Nanosize of titania was confirmed by both XRD and TEM studies. Visible light inactivity of TiO2 is overcome by C, N, B, F doped titania catalysts in the degradation of neonicotinoid type insecticides namely imidacloprid (IMI) and thiamethoxam (TMX). The degradation efficiencies of the catalysts under different irradiations namely UV, visible and solar were compared. Among the catalysts, CNBF/TiO2 degraded IMI completely at 150, 240 and 330 min whereas TMX has been degraded completely at 210, 270 and 420 min under UV, solar and visible irradiations respectively. The recyclability test of CNBF/TiO2 confirmed its stability towards photocatalytic reaction.

Graphite to Graphene via Graphene Oxide: An Overview on Synthesis, Properties, and Applications

NASA Astrophysics Data System (ADS)

Hansora, D. P.; Shimpi, N. G.; Mishra, S.

2015-12-01

This work represents a state-of-the-art technique developed for the preparation of graphene from graphite-metal electrodes by the arc-discharge method carried out in a continuous flow of water. Because of continuous arcing of graphite-metal electrodes, the graphene sheets were observed in water with uniformity and little damage. These nanosheets were subjected to various purification steps such as acid treatment, oxidation, water washing, centrifugation, and drying. The pure graphene sheets were analyzed using Raman spectrophotometry, x-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), and tunneling electron microscopy (TEM). Peaks of Raman spectra were recorded at (1300-1400 cm-1) and (1500-1600 cm-1) for weak D-band and strong G-band, respectively. The XRD pattern showed 85.6% crystallinity of pure graphite, whereas pure graphene was 66.4% crystalline. TEM and FE-SEM micrographs revealed that graphene sheets were overlapped to each other and layer-by-layer formation was also observed. Beside this research work, we also reviewed recent developments of graphene and related nanomaterials along with their preparations, properties, functionalizations, and potential applications.

Comparison of In Situ Polymerization and Solution-Dispersion Techniques in the Preparation of Polyimide/Montmorillonite (MMT) Nanocomposites

PubMed Central

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd. Sapuan; Hussein, Mohd. Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3′,4,4′-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique. PMID:22016643

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

PubMed

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Boosted surface acidity in TiO2 and Al2O3-TiO2 nanotubes as catalytic supports

NASA Astrophysics Data System (ADS)

Camposeco, R.; Castillo, S.; Mejía-Centeno, Isidro; Navarrete, J.; Nava, N.

2015-11-01

In this study, titanate nanotubes (NT) and titanate nanotubes with alumina (NT-Al) were studied as solid acid catalytic supports to show the relationship between the kind of acidity and catalytic activity. The supports were characterized by XRD, TEM, FTIR, XPS, and tested in the SCR-NO with NH3. It was found that the amount of Brönsted acid sites was maintained and the Lewis acid sites were significantly affected by the addition of alumina (1, 3, 5 and 10 wt.%); such acidity was higher than that of the titanate nanotubes (NT) by two-fold. To confirm the formation of titanate nanotubes and titanate nanotubes with alumina, transmission electron microscopy (TEM) was used. X-ray diffraction (XRD) revealed the formation of the H2Ti4O9·H2O phase. All NT and NT-Al supports presented catalytic activity to remove NO with NH3 under lean conditions, confirming the presence of an important amount of Brönsted and Lewis acid sites in both NT and NT-Al supports.

Characterization of tetraethylene glycol passivated iron nanoparticles

NASA Astrophysics Data System (ADS)

Nunes, Eloiza da Silva; Viali, Wesley Renato; da Silva, Sebastião William; Coaquira, José Antonio Huamaní; Garg, Vijayendra Kumar; de Oliveira, Aderbal Carlos; Morais, Paulo César; Jafelicci Júnior, Miguel

2014-10-01

The present study describes the synthesis and characterization of iron@iron oxide nanoparticles produced by passivation of metallic iron in tetraethylene glycol media. Structural and chemical characterizations were performed using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mössbauer spectroscopy. Pomegranate-like core@shell nanoparticulate material in the size range of 90-120 nm was obtained. According to quantitative phase analysis using Rietveld structure refinement the synthesized iron oxide was identified as magnetite (Fe3O4) whereas the iron to magnetite mass fractions was found to be 47:53. These findings are in good agreement with the data obtained from Mössbauer and thermal gravimetric analysis (TGA). The XPS data revealed the presence of a surface organic layer with higher hydrocarbon content, possibly due to the tetraethylene glycol thermal degradation correlated with iron oxidation. The room-temperature (300 K) saturation magnetization measured for the as-synthesized iron and for the iron-iron oxide were 145 emu g-1 and 131 emu g-1, respectively. The measured saturation magnetizations are in good agreement with data obtained from TEM, XRD and Mössbauer spectroscopy.

A Mössbauer spectral study of degradation in La 0.58Sr 0.4Fe 0.5Co 0.5O 3–x after long-term operation in solid oxide electrolysis cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmoud, Abdelfattah; Daroukh, Mahmoud Al; Lipinska-Chwalek, Marta

Here, degradation processes of oxygen electrodes in solid oxide electrolysis cells (SOECs) were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Mössbauer spectroscopy. La 0.58Sr 0.4Fe 0.5Co 0.5O 3–x (LSCF) anodes (oxygen electrode) were analyzed after different long-term operations durations of 1774, 6100 and 9000 h. The results were compared with a cell in the initial state. Besides the LSCF anode, the SOECs were composed of a Ce 0.8Gd 0.2O 1.9 barrier layer between the anode and electrolyte, yttria-stabilized zirconia (YSZ) as electrolyte and Ni-YSZ as cathode (hydrogen electrode). Mössbauer spectra of the iron-containingmore » anode were acquired in order to determine the alteration of the iron oxidation state and its local environment during operation. Mössbauer spectroscopy yields indirect information about the degradation mechanism, especially in combination with SEM, TEM, and XRD. XRD and TEM revealed the appearance of Co 3O 4 during the SOEC operation and SEM analyses confirmed the formation of SrZrO 3 at the electrode/electrolyte interface. The spectral analysis confirmed the reduction of iron from Fe(IV) to Fe(III) in LSCF after long-term operation. The fraction of Fe(IV) in the electrode decreased with time and 18, 15, 13 and 11% were obtained for 0, 1774, 6100, and 9000 h of operation, respectively.« less

A Mössbauer spectral study of degradation in La 0.58Sr 0.4Fe 0.5Co 0.5O 3–x after long-term operation in solid oxide electrolysis cells

DOE PAGES

Mahmoud, Abdelfattah; Daroukh, Mahmoud Al; Lipinska-Chwalek, Marta; ...

2017-10-21

Here, degradation processes of oxygen electrodes in solid oxide electrolysis cells (SOECs) were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Mössbauer spectroscopy. La 0.58Sr 0.4Fe 0.5Co 0.5O 3–x (LSCF) anodes (oxygen electrode) were analyzed after different long-term operations durations of 1774, 6100 and 9000 h. The results were compared with a cell in the initial state. Besides the LSCF anode, the SOECs were composed of a Ce 0.8Gd 0.2O 1.9 barrier layer between the anode and electrolyte, yttria-stabilized zirconia (YSZ) as electrolyte and Ni-YSZ as cathode (hydrogen electrode). Mössbauer spectra of the iron-containingmore » anode were acquired in order to determine the alteration of the iron oxidation state and its local environment during operation. Mössbauer spectroscopy yields indirect information about the degradation mechanism, especially in combination with SEM, TEM, and XRD. XRD and TEM revealed the appearance of Co 3O 4 during the SOEC operation and SEM analyses confirmed the formation of SrZrO 3 at the electrode/electrolyte interface. The spectral analysis confirmed the reduction of iron from Fe(IV) to Fe(III) in LSCF after long-term operation. The fraction of Fe(IV) in the electrode decreased with time and 18, 15, 13 and 11% were obtained for 0, 1774, 6100, and 9000 h of operation, respectively.« less

Biological Oxidation of Fe(II) in Reduced Nontronite Coupled with Nitrate Reduction by Pseudogulbenkiania sp. Strain 2002

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Linduo; Dong, Hailiang; Kukkadapu, Ravi K.

Nitrate contamination in soils, sediments, and water bodies is a significant issue. Although much is known about nitrate degradation in these environments, especially via microbial pathways, a complete understanding of all degradation processes, especially in clay mineral-rich soils, is still lacking. The objective of this study was to study the potential of removing nitrate contaminant using structural Fe(II) in clay mineral nontronite. Specifically, the coupled processes of microbial oxidation of Fe(II) in microbially reduced nontronite (NAu-2) and nitrate reduction by Pseudogulbenkiania species strain 2002 was investigated. Bio-oxidation experiments were conducted in bicarbonate-buffered medium under both growth and nongrowth conditions. Themore » extents of Fe(II) oxidation and nitrate reduction were measured by wet chemical methods. X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and 57Fe-Mössbauer spectroscopy were used to observe mineralogical changes associated with Fe(III) reduction and Fe(II) oxidation in nontronite. The bio-oxidation extent under growth and nongrowth conditions reached 93% and 57%, respectively. Over the same time period, nitrate was completely reduced under both conditions to nitrogen gas (N2), via an intermediate product nitrite. Magnetite was a mineral product of nitrate-dependent Fe(II) oxidation, as evidenced by XRD data and TEM diffraction patterns. The results of this study highlight the importance of iron-bearing clay minerals in the global nitrogen cycle with potential applications in nitrate removal in soils.« less

Green synthesis, characterization and catalytic degradation studies of gold nanoparticles against congo red and methyl orange.

PubMed

Umamaheswari, C; Lakshmanan, A; Nagarajan, N S

2018-01-01

The present study reports, novel and greener method for synthesis of gold nanoparticles (AuNPs) using 5,7-dihydroxy-6-metoxy-3 ' ,4 ' methylenedioxyisoflavone (Dalspinin), isolated from the roots of Dalbergia coromandeliana was carried out for the first time. The synthesized gold nanoparticles were characterized by UV-Vis spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The observed surface plasmon resonance (SPR) at 532nm in the UV-Vis absorption spectrum indicates the formation of gold nanoparticles. The powder XRD and SAED pattern for synthesized gold nanoparticles confirms crystalline nature. The HR-TEM images showed that the AuNPs formed were small in size, highly monodispersed and spherical in shape. The average particle sizes of the AuNPs are found to be ~10.5nm. The prepared AuNPs were found to be stable for more than 5months without any aggregation. The catalytic degradation studies of the synthesized AuNPs towards degradation of congo red and methyl orange, showed good catalytic in the complete degradation of both the dyes. The reduction catalyzed by gold nanoparticles followed the pseudo-first order kinetics, with a rate constant of 4.5×10 -3 s -1 (R 2 =0.9959) and 1.7×10 -3 s -1 (R 2 =0.9918) for congo red (CR) and methyl orange (MO), respectively. Copyright © 2017. Published by Elsevier B.V.

High-energy ball milling technique for ZnO nanoparticles as antibacterial material

PubMed Central

Salah, Numan; Habib, Sami S; Khan, Zishan H; Memic, Adnan; Azam, Ameer; Alarfaj, Esam; Zahed, Nabeel; Al-Hamedi, Salim

2011-01-01

Nanoparticles of zinc oxide (ZnO) are increasingly recognized for their utility in biological applications. In this study, the high-energy ball milling (HEBM) technique was used to produce nanoparticles of ZnO from its microcrystalline powder. Four samples were ball milled for 2, 10, 20, and 50 hours, respectively. The structural and optical modifications induced in the ‘as synthesized’ nanomaterials were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and photoluminescence emission spectra (PL). SEM and TEM results show a gradual decrease in particle size from around 600 to ∼30 nm, with increased milling time. The initial microstructures had random shapes, while the final shape became quite spherical. XRD analysis showed ZnO in a hexagonal structure, broadening in the diffracted peaks and going from larger to smaller particles along with a relaxation in the lattice constant c. The value of c was found to increase from 5.204 to 5.217 Å with a decrease in particle size (600 to ∼30 nm). PL result showed a new band at around 365 nm, whose intensity is found to increase as the particles size decreases. These remarkable structural and optical modifications induced in ZnO nanoparticles might prove useful for various applications. The increase in c value is an important factor for increasing the antibacterial effects of ZnO, suggesting that the HEBM technique is quite suitable for producing these nanoparticles for this purpose. PMID:21720499

Measurement of fatigue accumulation in high-strength steels by microstructural examination

NASA Astrophysics Data System (ADS)

Nakagawa, Y. G.; Yoshizawa, H.; Lapides, M. E.

1990-07-01

Fatigue test bars fabricated from an SA508 class 3 low-carbon steel plate were cyclically deformed at 300 °C (constant low-cycle fatigue, total strain range Δɛ = 0.78 pct and 0.48 pct) to crack initiation (100 pct cumulative damage, CD) and to the factors 75, 50, and 25 pct CD. The test bars were cut perpendicular to the stress axis at the center of the gage length. The X-ray diffraction line-broadening (XRD) was performed on the cross sections created by the cuts. Thin foils (˜0.1-μm thick) were prepared from each cross section and used for the transmission electron microscope (TEM) and selected area diffraction (SAD) study. The half-value line breadth change measured by the XRD increased with the CD increase up to 50 pct, beyond which a significant reduction was observed for the 75 and 100 pct CD sample regardless of the incident X-ray beam angle. By the TEM, the undamaged material (0 pct CD) was characterized by high-angle boundaries, small carbide precipitates, and dislocation cell networks in grains. These characteristics did not show any appreciable changes in all of the samples with fatigue damage of the respective levels. Micro-orientation changes of the dislocation cells studied by the SAD of the foils and a statistical data analysis clearly demonstrated that the mean orientation difference in the cells and its standard deviation increased gradually as the CD increased.

Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

PubMed

Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

2010-04-01

Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

Green synthesis of BiVO4 nanorods via aqueous extracts of Callistemon viminalis

NASA Astrophysics Data System (ADS)

Mohamed, H. E. A.; Sone, B. T.; Fuku, X. G.; Dhlamini, M. S.; Maaza, M.

2018-05-01

Nowadays, the development of efficient green chemistry methods for synthesis of metal oxides nanoparticles has become a major focus of researchers. These methods are being investigated in order to find an eco-friendly technique for production of well-characterized nanoparticles. In this contribution we report for the first time, the synthesis and structural characterization of n-type Bismuth vanadate (BiVO4) nanoparticles using aqueous extracts of Callistemon viminalis as a chelating agent. To ascertain the formation of BiVO4, X-Ray diffraction analysis (XRD), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), Electron Dispersion X-ray Spectroscopy (EDS), Fourier Transform Infra-red Spectroscopy (FTIR), and Photoluminescence spectroscopy (PL) were carried out.

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

In vitro toxicity test of nano-sized magnesium oxide synthesized via solid-phase transformation

NASA Astrophysics Data System (ADS)

Zheng, Jun; Zhou, Wei

2018-04-01

Nano-sized magnesium oxide (MgO) has been a promising potential material for biomedical pharmaceuticals. In the present investigation, MgO nanoparticles synthesized through in-situ solid-phase transformation based on the previous work (nano-Mg(OH)2 prepared by precipitation technique) using magnesium nitrate and sodium hydroxide. The phase structure and morphology of the MgO nanoparticles are characterized by X-ray powder diffraction (XRD), selected area electronic diffraction (SAED) and transmission electron microscopy (TEM) respectively. In vitro hemolysis tests are adopted to evaluate the toxicity of the synthesized nano-MgO. The results evident that nano-MgO with lower concentration is slightly hemolytic, and with concentration increasing nano-MgO exhibit dose-responsive hemolysis.

Optical properties of ZnO/BaCO3 nanocomposites in UV and visible regions.

PubMed

Zak, Ali Khorsand; Hashim, Abdul Manaf; Darroudi, Majid

2014-01-01

Pure zinc oxide and zinc oxide/barium carbonate nanoparticles (ZnO-NPs and ZB-NPs) were synthesized by the sol-gel method. The prepared powders were characterized by X-ray diffraction (XRD), ultraviolet-visible (UV-Vis), Auger spectroscopy, and transmission electron microscopy (TEM). The XRD result showed that the ZnO and BaCO3 nanocrystals grow independently. The Auger spectroscopy proved the existence of carbon in the composites besides the Zn, Ba, and O elements. The UV-Vis spectroscopy results showed that the absorption edge of ZnO nanoparticles is redshifted by adding barium carbonate. In addition, the optical parameters including the refractive index and permittivity of the prepared samples were calculated using the UV-Vis spectra. 81.05.Dz; 78.40.Tv; 42.70.-a.

Fabrication of Worm-Like Nanorods and Ultrafine Nanospheres of Silver Via Solid-State Photochemical Decomposition

PubMed Central

2009-01-01

Worm-like nanorods and nanospheres of silver have been synthesized by photochemical decomposition of silver oxalate in water by UV irradiation in the presence of CTAB and PVP, respectively. No external seeds have been employed for the synthesis of Ag nanorods. The synthesized Ag colloids have been characterized by UV-visible spectra, powder XRD, HRTEM, and selected area electron diffraction (SAED). Ag nanospheres of average size around 2 nm have been obtained in the presence of PVP. XRD and TEM analyses revealed that top and basal planes of nanorods are bound with {111} facets. Williamson–Hall plot has revealed the presence of defects in the Ag nanospheres and nanorods. Formation of defective Ag nanocrystals is attributed to the heating effect of UV-visible irradiation. PMID:20596513

Preparation and optical characteristics of ZnSe nanocrystals doped glass by sol gel in situ crystallization method

NASA Astrophysics Data System (ADS)

Hao, Haiyan; Yao, Xi; Wang, Minqiang

2007-01-01

Homogeneous ZnSe nanocrystals doped SiO 2 glass was successfully prepared by sol-gel in situ crystallization method. The structure of the doped ZnSe nanocrystals was studied by X-ray diffraction (XRD). ZnSe nanocrystals in silica were about 4-10 nm analysed by transmission electron microscopy (TEM), which was consistent with the results of XRD estimated using Scherrer's formular. The quantum size effect in ZnSe nanocrystals was evidenced from the blue-shifts of the optical absorption edge, and the average size of ZnSe nanocrystals was estimated by the magnitude of blue shift according to the L.E. Brus' effective mass model. The size of ZnSe nanocrystals depending on annealing time and temperature was further discussed using XRF.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

NASA Astrophysics Data System (ADS)

Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

2012-09-01

Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

Development of regenerated cellulose/halloysites nanocomposites via ionic liquids.

PubMed

Hanid, Nurbaiti Abdul; Wahit, Mat Uzir; Guo, Qipeng; Mahmoodian, Shaya; Soheilmoghaddam, Mohammad

2014-01-01

In this study, regenerated cellulose/halloysites (RC/HNT) nanocomposites with different nanofillers loading were fabricated by dissolving the cellulose in 1-ethyl-3-methylimidazolium chloride (EMIMCl) ionic liquid. The films were prepared via solution casting method and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The mechanical properties were investigated by tensile testing. It clearly displayed a good enhancement of both tensile strength and Young's modulus with HNT loading up to 5 wt%. As the HNT loadings increased to 5 wt%, the thermal behaviour and water resistance rate was also increased. The TEM and SEM images also depicted even dispersion of the HNT and a good intertubular interaction between the HNT and the cellulose matrix. Copyright © 2013 Elsevier Ltd. All rights reserved.

An Atom Probe Tomographic Investigation of High-Strength, High-Toughness Precipitation Strengthened Steels for Naval Applications

NASA Astrophysics Data System (ADS)

Hunter, Allen H.

Novel high-strength high-toughness alloys strengthened by precipitation are investigated for use in naval applications. The mechanical properties of an experimental steel alloy, NUCu-140, are evaluated and are not suitable for the naval requirements due to poor impact toughness at -40°C. An investigation is conducted to determine optimum processing conditions to restore toughness. A detailed aging study is conducted at 450, 500, and 550°C to determine the evolution of the microstructure and mechanical properties. A combination of transmission electron microscopy (TEM), synchrotron X-ray Diffraction (XRD), and Local electrode atom probe (LEAP) tomography are used to measure the evolution of the Cu precipitates, austenite, NbC, and cementite phases during aging. The evolution of the Cu precipitates significantly affects the yield strength of the steel, but low temperature toughness is controlled by the cementite precipitates. Extended aging is effective at improving the impact toughness but the yield strength is also decreased due to coarsening of the Cu precipitates. To provide a foundation for successful welding of NUCu-140 steel, an investigation of the effects of gas metal arc welding (GMAW) are performed. The microstructures in the base metal (BM), heat affected zone (HAZ), and fusion zone (FZ) of a GMAW sample are analyzed to determine the effects of the welding thermal cycle. Weld simulation samples with known thermal histories are prepared and analyzed by XRD and LEAP tomography. A significant loss in microhardness is observed as a result of dissolution of the Cu precipitates after the weld thermal cycle. The cooling time is too rapid to allow significant precipitation of Cu. In addition to the NUCu-140 alloy, a production HSLA-115 steel alloy is investigated using TEM, XRD, and LEAP tomography. The strength of the HSLA-115 is found to be derived primarily from Cu precipitates. The volume fractions of cementite, austenite, and NbC are measured by XRD. Austenite precipitates are observed at martensite lath boundaries using TEM.

Electroless Nickel Deposition for Front Side Metallization of Silicon Solar Cells

PubMed Central

Hsieh, Shu Huei; Hsieh, Jhong Min; Chen, Wen Jauh; Chuang, Chia Chih

2017-01-01

In this work, nickel thin films were deposited on texture silicon by electroless plated deposition. The electroless-deposited Ni layers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectroscopy (EDS), X-ray diffraction analysis (XRD), and sheet resistance measurement. The results indicate that the dominant phase was Ni2Si and NiSi in samples annealed at 300–800 °C. Sheet resistance values were found to correlate well with the surface morphology obtained by SEM and the results of XRD diffraction. The Cu/Ni contact system was used to fabricate solar cells by using two different activating baths. The open circuit voltage (Voc) of the Cu/Ni samples, before and after annealing, was measured under air mass (AM) 1.5 conditions to determine solar cell properties. The results show that open circuit voltage of a solar cell can be enhanced when the activation solution incorporated hydrofluoric acid (HF). This is mainly attributed to the native silicon oxide layer that can be decreased and/or removed by HF with the corresponding reduction of series resistance. PMID:28805724

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Electrochemical and Morphological Investigations of Ga Addition to Pt Electrocatalyst Supported on Carbon

PubMed Central

Paganoto, Giordano T.; Santos, Deise M.; Guimarães, Marco C. C.; Carneiro, Maria Tereza W. D.

2017-01-01

This paper is consisted in the synthesis of platinum-based electrocatalysts supported on carbon (Vulcan XC-72) and investigation of the addition of gallium in their physicochemical and electrochemical properties toward ethanol oxidation reaction (EOR). PtGa/C electrocatalysts were prepared through thermal decomposition of polymeric precursor method at a temperature of 350°C. Six different compositions were homemade: Pt50Ga50/C, Pt60Ga40/C, Pt70Ga30/C, Pt80Ga20/C, Pt90Ga10/C, and Pt100/C. These electrocatalysts were electrochemically characterized by cyclic voltammetry (CV), chronoamperometry (CA), chronopotentiometry (CP), and electrochemical impedance spectroscopy (EIS) in the presence and absence of ethanol 1.0 mol L−1. Thermogravimetric analysis (TGA), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and transmission electron microscopy (TEM) were also carried out for a physicochemical characterization of those materials. XRD results showed the main peaks of face-centered cubic Pt. The particle sizes obtained from XRD and TEM analysis range from 7.2 nm to 12.9 nm. The CV results indicate behavior typical of Pt-based electrocatalysts in acid medium. The CV, EIS, and CA data reveal that the addition of up to 31% of gallium to the Pt highly improves catalytic activity on EOR response when compared to Pt100/C. PMID:28466065

The effect of Fe-Rh alloying on CO hydrogenation to C 2+ oxygenates

DOE PAGES

Palomino, Robert; Magee, Joseph W.; Llorca, Jordi; ...

2015-05-20

A combination of reactivity and structural studies using X-ray diffraction (XRD), pair distribution function (PDF), and transmission electron microscopy (TEM) was used to identify the active phases of Fe-modified Rh/TiO 2 catalysts for the synthesis of ethanol and other C 2+ oxygenates from CO hydrogenation. XRD and TEM confirm the existence of Fe–Rh alloys for catalyst with 1–7 wt% Fe and ~2 wt% Rh. Rietveld refinements show that FeRh alloy content increases with Fe loading up to ~4 wt%, beyond which segregation to metallic Fe becomes favored over alloy formation. Catalysts that contain Fe metal after reduction exhibit some carburizationmore » as evidenced by the formation of small amounts of Fe 3C during CO hydrogenation. Analysis of the total Fe content of the catalysts also suggests the presence of FeO x also increased under reaction conditions. Reactivity studies show that enhancement of ethanol selectivity with Fe loading is accompanied by a significant drop in CO conversion. Comparison of the XRD phase analyses with selectivity suggests that higher ethanol selectivity is correlated with the presence of Fe–Rh alloy phases. As a result, the interface between Fe and Rh serves to enhance the selectivity of ethanol, but suppresses the activity of the catalyst which is attributed to the blocking or modifying of Rh active sites.« less

Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

2018-05-01

This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-07-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-04-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Green synthesis of silver nanoparticles using marine algae Caulerpa racemosa and their antibacterial activity against some human pathogens

NASA Astrophysics Data System (ADS)

Kathiraven, T.; Sundaramanickam, A.; Shanmugam, N.; Balasubramanian, T.

2015-04-01

We present the synthesis and antibacterial activity of silver nanoparticles using Caulerpa racemosa, a marine algae. Fresh C. racemosa was collected from the Gulf of Mannar, Southeast coast of India. The seaweed extract was used for the synthesis of AgNO3 at room temperature. UV-visible spectrometry study revealed surface plasmon resonance at 413 nm. The characterization of silver nanoparticle was carried out using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and transmission electron microscope (TEM). FT-IR measurements revealed the possible functional groups responsible for reduction and stabilization of the nanoparticles. X-ray diffraction analysis showed that the particles were crystalline in nature with face-centered cubic geometry.TEM micrograph has shown the formation of silver nanoparticles with the size in the range of 5-25 nm. The synthesized AgNPs have shown the best antibacterial activity against human pathogens such as Staphylococcus aureus and Proteus mirabilis. The above eco-friendly synthesis procedure of AgNPs could be easily scaled up in future for the industrial and therapeutic needs.

Evaluation of local anesthetic effects of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles in Male Swiss mice.

PubMed

Jiang, Qiliang; Yu, Shashuang; Li, Xingwang; Ma, Chuangen; Li, Aixiang

2018-01-01

A simple approach for the synthesis of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles (IL-AgNPs) was reported in this work. The shape, size and surface morphology of the Lidocaine-Ibuprofen ionic liquid stabilized AgNPs were characterized by using spectroscopic and microscopic techniques such as Ultraviolet-visible spectroscopy (UV-Visible), X-ray diffraction (XRD) analysis, Selected area electron diffraction (SAED), Transmission electron microscopy (TEM). TEM analysis showed the formation of 20-30nm size of IL-AgNPs with very clear lattice fringes. SAED pattern confirmed the highly crystalline nature of fabricated IL stabilized AgNPs. EDS results confirmed the formation of nanosilver. The fabricated IL-AgNPs were studied for their local anesthetic effect in rats. The results of local anesthetic effect showed that the time for onset of action by IL-AgNPs is 10min, which is significantly higher than that for EMLA. Further, tactile test results confirmed the stronger and faster local anesthetic effect of IL-AgNPs when compared to that of EMLA. Copyright © 2017. Published by Elsevier B.V.

Structural, optical and enhanced power filtering application of PEG capped Zn1-xCoxS quantum dots

NASA Astrophysics Data System (ADS)

Vineeshkumar, T. V.; Prasanth, S.; Pragash, R.; Unnikrishnan, N. V.; Sudarsanakumar, C.

2018-04-01

Zn1-xCoxS (x= 0.05, 0.1, 0.15 and 0.2) quantum dots were synthesized successfully using co precipitation technique in polyethylene glycol (PEG) matrix. The PEG acted as a capping agent as well as a reducing agent. The structural and optical properties of the samples were studied by x-ray diffraction (XRD), TEM analysis and UV-Visible absorption. Nonlinear optical properties were measured using open aperture z-scan technique, employing frequency doubled (532 nm) pumping sources.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

NASA Astrophysics Data System (ADS)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.

Structural, morphological and optical properties of chromium oxide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Babukutty, Blessy; Parakkal, Fasalurahman; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com

2015-06-24

Chromium oxide nanoparticles are synthesized by reduction route from chloride precursors with surfactant, trioctylphosphine oxide (TOPO). Structural and morphological characterization are analyzed using X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). Transmission Electron micrographs show that the average grain size lies in the range 5nm to 10nm. Optical characterization has been done by UV-VIS spectrophotometer. Distinct optical absorptions of Cr{sup 3+} ions show hinting towards the presence of Cr{sub 2}O{sub 3}. Presence of oxygen is also confirmed from Electron Energy Loss Spectroscopy (EELS) studies.

Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

Synthesis and magnetic properties of nickel nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Jaiveer, E-mail: jaiveer24singh@gmail.com, E-mail: netramkaurav@yahoo.co.uk; Patel, Tarachand; Okram, Gunadhor S.

2016-05-23

Monodisperse nickel nanoparticles (Ni-NPs) were synthesized via a thermal decomposition process. The NPs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). They were spherical with mean diameter of 4 nm. Zero field cooled (ZFC) and field cooled (FC) magnetization versus temperature data displayed interesting magnetic interactions. ZFC showed a peak at 4.49 K, indicating the super paramagnetic behavior. Magnetic anisotropic constant was estimated to be 4.62×10{sup 5} erg/cm{sup 3} and coercive field was 168 Oe at 3 K.

The growth of ZnO nanostructures using Arginine

NASA Astrophysics Data System (ADS)

Singh, Baljinder; Moudgil, Lovika; Singh, Gurinder; Kaura, Aman

2018-05-01

The growth mechanism of Zinc oxide (ZnO) nanomaterial with amino acid (Arginine) is explained at different shapes. The present study of ZnO nanostructures (NSs) in the presence of Arginine has enabled us to not only determine the growth mechanism of ZnO NSs but also to determine the effect of Arginine at different temperature of reactants. The synthesized samples are characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Results reveal that Arginine is responsible for formation of NSs. Based on these results, a plausible mechanism is explained.

Morphology and crystallinity of sisal nanocellulose after sonication

NASA Astrophysics Data System (ADS)

Sosiati, H.; Wijayanti, D. A.; Triyana, K.; Kamiel, B.

2017-09-01

Different preparation methods on the natural fibers resulted in different morphology. However, the relationships between type of natural fibers, preparation methods and the morphology of produced nanocellulose could not be exactly defined. The sisal nanocellulose was presently prepared by alkalization and bleaching followed by sonication to verify changes in the morphology and crystallinity of nanocellulose related to the formation mechanism. The extracted microcellulose was subjected to scanning electron microscopy (SEM) and x-ray diffraction (XRD) analysis. The isolated cellulose nanospheres were examined with respect to morphology by SEM and transmission electron microscopy (TEM) and, to crystallinity by electron diffraction analysis. Bleaching after alkalization made the microfibrils clearly separated from each other to the individual fiber whose width of the single fiber was ranging from 6 to 13 µm. The XRD crystallinity index (CI) of microcellulose gradually increased after the chemical treatments; 83.12% for raw sisal fiber, 88.57% for alkali treated fiber and 94.03% for bleached fibers. The ultrasonic agitation after bleaching that was carried out at 750 Watt, 20 kHz and amplitude of 39% for 2 h produces homogeneous cellulose nanospheres less than 50 nm in diameter with relatively low crystallinity. The electron diffraction analysis confirmed that the low crystallinity of produced nnocellulose is related to the effect of chemical treatment done before sonication.

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

Residual glass and crystalline phases in a barium disilicate glass–ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Araujo, Marcel C.C.; Botta, Walter J.; Kaufmann, Michael J.

2015-12-15

Investigations about the presence of residual glass are scarce, despite its fundamental role in the crystallization kinetics and luminescent properties of barium disilicate glass–ceramics (BaO·2SiO{sub 2}–BS{sub 2}) with a quasi-stoichiometric composition. Non-isothermal (DTA/DSC) experiments have demonstrated that BS{sub 2} presents a polymorphic transformation, where the h-BS{sub 2} (monoclinic structure) phase is completely transformed in l-BS{sub 2} (orthorhombic structure) at temperatures higher than 1020 °C (10 °C/min). In this study, BS{sub 2} monolithic samples were heat-treated at 1000 °C (BS2-10) and 1100 °C (BS2-11) in a DSC furnace at a heating rate of 10 °C/min. In addition, the crystalline and amorphousmore » phases were characterized and quantified by Transmission Electron Microscopy (TEM) and X-ray Diffraction (XRD) experiments, respectively. Although the complete polymorphic transformation from h-BS2 to l-BS2 was achieved at 1100 °C, our results demonstrated that BS2-11 contains a minor, albeit not negligible, amount of residual glass. - Highlights: • The crystalline and amorphous phases in a barium disilicate glass were characterized and quantified by XRD and TEM. • The BS2-10 sample was constituted by two main crystalline phases, which consists of 2 polymorphic forms: h-BS2 and l-BS2. • The orthorhombic BS2 phase (l-BS2) was predominant at 1100 °C. • The complete polymorphic transformation from h-BS2 to l-BS2 was achieved at 1100 °C. • Nevertheless, our XRD and TEM results demonstrated that BS2-11 contains a minor amount of residual glass.« less

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Calcium copper-titanate thin film growth: tailoring of the operational conditions through nanocharacterization and substrate nature effects.

PubMed

Lo Nigro, Raffaella; Toro, Roberta G; Malandrino, Graziella; Fragalà, Ignazio L; Losurdo, Maria; Giangregorio, Michelaria M; Bruno, Giovanni; Raineri, Vito; Fiorenza, Patrick

2006-09-07

A novel approach based on a molten multicomponent precursor source has been applied for the MOCVD fabrication of high-quality CaCu(3)Ti(4)O(12) (CCTO) thin films on various substrates. The adopted in situ strategy involves a molten mixture consisting of Ca(hfa)(2).tetraglyme, Ti(tmhd)(2)(O-iPr)(2), and Cu(tmhd)(2) [Hhfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione; tetraglyme = 2,5,8,11,14-pentaoxapentadecane; Htmhd = 2,2,6,6-tetramethyl-3,5-heptandione; O-iPr = isopropoxide] precursors. Film structural and morphological characterizations have been carried out by several techniques [X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM)], and in particular the energy filtered TEM mapping and X-ray energy dispersive (EDX) analysis in TEM mode provided a suitable correlation between nanostructural properties of CCTO films and deposition conditions and/or the substrate nature. Correlation between the nanostructure and optical/dielectric properties has been investigated exploiting spectroscopic ellipsometry.

Structural and Magnetic Response in Bimetallic Core/Shell Magnetic Nanoparticles

PubMed Central

Nairan, Adeela; Khan, Usman; Iqbal, Munawar; Khan, Maaz; Javed, Khalid; Riaz, Saira; Naseem, Shahzad; Han, Xiufeng

2016-01-01

Bimagnetic monodisperse CoFe2O4/Fe3O4 core/shell nanoparticles have been prepared by solution evaporation route. To demonstrate preferential coating of iron oxide onto the surface of ferrite nanoparticles X-ray diffraction (XRD), High resolution transmission electron microscope (HR-TEM) and Raman spectroscopy have been performed. XRD analysis using Rietveld refinement technique confirms single phase nanoparticles with average seed size of about 18 nm and thickness of shell is 3 nm, which corroborates with transmission electron microscopy (TEM) analysis. Low temperature magnetic hysteresis loops showed interesting behavior. We have observed large coercivity 15.8 kOe at T = 5 K, whereas maximum saturation magnetization (125 emu/g) is attained at T = 100 K for CoFe2O4/Fe3O4 core/shell nanoparticles. Saturation magnetization decreases due to structural distortions at the surface of shell below 100 K. Zero field cooled (ZFC) and Field cooled (FC) plots show that synthesized nanoparticles are ferromagnetic till room temperature and it has been noticed that core/shell sample possess high blocking temperature than Cobalt Ferrite. Results indicate that presence of iron oxide shell significantly increases magnetic parameters as compared to the simple cobalt ferrite. PMID:28335200

Synthesis of SiO(x) powder using DC arc plasma.

PubMed

Jung, Chan-Ok; Park, Dong-Wha

2013-02-01

SiO(x) was prepared by DC arc plasma and applied to the anode material of lithium ion batteries. A pellet of a mixture of Si and SiO2 was used as the raw material. The ratios of the silicon and silicon dioxide (SiO2) mixtures were varied by controlling the Si-SiO2 molar ratio (Si-SiO2 = 1-4). Hydrogen gas was used as the reduction atmosphere in the chamber. The prepared SiO(x) was collected on the chamber wall. The obtained SiO(x) was characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). XRD and TEM showed that the phase composition of the prepared particles was composed of amorphous SiO(x) and crystalline Si. The prepared SiO(x) showed wire and spherical morphology. XPS indicated the bonding state and 'x' value of the prepared SiO(x), which was close to one. The result of prepared SiO(x) is discussed from thermodynamic equilibrium calculations. The electrochemical behavior of the silicon monoxide anode was investigated.

Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

NASA Astrophysics Data System (ADS)

Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

2017-11-01

A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

Synthesis and evaluation of optical and antimicrobial properties of Ag-SnO2 nanocomposites

NASA Astrophysics Data System (ADS)

Kumar Nair, Kishore; Kumar, Promod; Kumar, Vinod; Harris, R. A.; Kroon, R. E.; Viljoen, Bennie; Shumbula, P. M.; Mlambo, M.; Swart, H. C.

2018-04-01

We report on the sol-gel based room temperature synthesis of undoped SnO2 and Ag-SnO2 nanostructures. The synthesized nanostructures were characterized by Fourier transform infrared spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and UV-visible spectroscopy. The XRD pattern confirmed that the obtained nanostructures have a tetragonally rutile structure. No extra phase changes were observed after Ag doping. UV-visible spectroscopy measurements indicated that the band gap of 3.59 eV for pure SnO2 nanostructures, decreased to 3.39 eV after doping. TEM analysis showed that no regular shape morphology existed and some rod-shaped particles were also detected in the nanostructures. The antibacterial activity of the nanostructures against E. coli was evaluated and a continuous decrease of microbial count was observed. The microbial population decreased from 6 × 105 cfu/ml to 7 × 104 cfu/ml and 5 × 104 cfu/ml on SnO2 and Ag-SnO2 treatments, respectively. Thus, the nanostructures can be used for the biorational management of E. coli for waste water treatment before discharge.

Effect of Co doping on the magnetic and DC electrical properties of Mn-Zn nanoferrites

NASA Astrophysics Data System (ADS)

Khandan Fadafan, H.; Lotfi Orimi, R.; Nezhadeini, S.

2018-06-01

In this study, Cobalt-Manganese-Zinc nanoferrites with the formula CoxMn0.5-xZn0.5Fe2O4 with x = 0.0, 0.1, 0.3, and 0.5 prepared by chemical Co-precipitation method. Then the structure and morphology of the synthesized nanoparticles were characterized by X-ray diffraction (XRD) and transmitting electron microscopy (TEM), respectively. The XRD patterns indicated the formation of single-phased cubic structure of spinel ferrite in nanometer size with no minor phase. The TEM image showed the formation of nanoparticles with average size of about 40 nm and normal size distribution. The magnetic measurements of the nanoparticles were done at room temperature using a vibrating sample magnetometer (VSM). Results exhibited a super-paramagnetic like behavior for some of the samples. DC electrical resistivity measurements were carried out by two-probe technique from 25 to 250 °C and showed decreasing of the resistivity with temperature meanwhile passing a transition to form of a peak. The peaks values observed near the Curie temperatures of samples suggest that anomaly behavior can attributed to spin canting associated with the phase transition from para to ferromagnetic state at TC.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

NASA Astrophysics Data System (ADS)

Deshpande, Aniruddha S.; Khomane, Ramdas B.; Vaidya, Bhalchandra K.; Joshi, Renuka M.; Harle, Arti S.; Kulkarni, Bhaskar D.

2008-06-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+ malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 and n-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5 15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

A novel route for synthesis of nanocrystalline hydroxyapatite from eggshell waste.

PubMed

Siva Rama Krishna, D; Siddharthan, A; Seshadri, S K; Sampath Kumar, T S

2007-09-01

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.

Progression in structural, magnetic and electrical properties of La-doped group IV elements

NASA Astrophysics Data System (ADS)

Deepapriya, S.; Annie Vinosha, P.; Rodney, John D.; Jerome Das, S.

2018-04-01

Progression of group IV elements such as zinc ferrite (ZnFe2O4), cobalt ferrite (CoFe2O4) was synthesized by doping lanthanum (La), via adopting a facile co-precipitation method. Doping hefty rare earth ion in spinel structure can amend to the physical properties of the lattice, which can be used in the enhancement of magnetic and electrical properties of the as-synthesized nanomaterial, it is vital to metamorphose and optimize its micro structural and magnetic features. The structural properties of the samples was analysed by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), Transmission electron microscopy (TEM) and UV-visible spectral analysis (UV-vis) reveals the optical property and optical band gap. The magnetic properties were evaluated using a vibrating sample magnetometer (VSM), the presence of functional group was confirmed by FTIR. XRD analyses elucidates that the synthesized samples zinc and cobalt had a spinel structure. From TEM analyses the morphology and diameter of the particle was observed. The substituted rare earth ions in Zinc ferrite inhibit the grain growth of the materials in an efficient manner compared with that of the Cobalt ferrite.

Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hojamberdiev, Mirabbos, E-mail: mirabbos_uz@yahoo.com; Zhu, Gangqiang; Xu, Yunhua

ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealedmore » that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.« less

Fabrication and characterization of akaganeite/graphene oxide nanocomposite for arsenic removal from water

NASA Astrophysics Data System (ADS)

Trang, Nguyen Thi Thuy; Thy, Lu Thi Mong; Cuong, Pham Mai; Tu, Tran Hoang; Hieu, Nguyen Huu

2018-04-01

In this study, akageneite/graphene oxide (β-FeOOH/GO) nanocomposite was fabricated by in situ forced hydrolysis of iron (III) chloride. The structure and morphology of β-FeOOH/GO were characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer-Emmett- Teller (BET) specific surface area. XRD, FTIR, and TEM results indicated that β-FeOOH nanoparticles were successfully decorated on the surface of GO nanosheets. The BET specific surface area of β-FeOOH/GO was observed of 97.94 m2/g. The nanocomposite was used as an adsorbent for removal of arsenic (As5+) from water. Adsorption experiments were carried out to investigate contact time, pH values, and As5+ initial concentrations. The adsorption equilibrium time was reached within 180 minutes. The adsorption was well-fitted by a pseudo-second-order kinetic and Langmuir isotherm model. The maximum adsorption capacity of β-FeOOH/GO for As5+ ions of 94.34 mg/g that was calculated from the Langmuir model at pH 3. Accordingly, the nanocomposite β-FeOOH/GO could be considered as a highly efficient adsorbent for removing arsenic from water.

The preparation and characterization of novel Pt/C electrocatalysts with controlled porosity and cluster size

DOE PAGES

Coker, Eric N.; Steen, William A.; Miller, Jeffrey T.; ...

2007-05-23

Small platinum clusters have been prepared in zeolite hosts through ion exchange and controlled calcination/reduction processes. In order to enable electrochemical application, the pores of the Pt-zeolite were filled with electrically conductive carbon via infiltration with carbon precursors, polymerization, and pyrolysis. The zeolite host was then removed by acid washing, to leave a Pt/C electrocatalyst possessing quasi-zeolitic porosity and Pt clusters of well-controlled size. The electrocatalysts were characterized by TEM, XRD, EXAFS, nitrogen adsorption and electrochemical techniques. Depending on the synthesis conditions, average Pt cluster sizes in the Pt/C catalysts ranged from 1.3 to 2.0 nm. The presence of orderedmore » porosity/structure in the catalysts was evident in TEM images as lattice fringes, and in XRD as a low-angle diffraction peak with d-spacing similar to the parent zeolite. The catalysts possess micro- and meso-porosity, with pore size distributions that depend upon synthesis variables. Finally, electroactive surface areas as high as 112 m 2 g Pt -1 have been achieved in Pt/C electrocatalysts which show oxygen reduction performance comparable to standard industrial catalysts.« less

[Raman spectrum of nano-graphite synthesized by explosive detonation].

PubMed

Wen, Chao; Li, Xun; Sun, De-Yu; Guan, Jin-Qing; Liu, Xiao-Xin; Lin, Ying-Rui; Tang, Shi-Ying; Zhou, Gang; Lin, Jun-De; Jin, Zhi-Hao

2005-01-01

The nano-graphite powder synthesized by the detonation of explosives with negative oxygen balance is a new powder material with potential applications. In this work, the preparation of nano-graphite powder in steel chamber by pure TNT (trinitrotoluene) explosives has been introduced. In the synthesis process, the protective gases in the steel chamber are N2, CO2 and Ar, and the pressure is 0.25-2 atm. Raman spectrum of the nano-graphite was measured. The characteristic Raman band assigned to sp2 of graphite has been observed at about 1 585 cm(-1) with half-peak width of 22 cm(-1). The peak shifted to a higher frequency by 5 cm(-1) compared with that of bulk graphite. The authors explain this blue shift phenomenon by size effect. The average size of nanographite from Raman measurement is 2.97-3.97 nm. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to measure the structure and particle size of the nano-graphite. The crystallite size of nano-graphite estimated from XRD andTEM are 2.58 nm (acid untreated) and 1.86 nm (acid treated) respectively, which is in accord with the results of the measurement approximately.

Piper nigrum leaf and stem assisted green synthesis of silver nanoparticles and evaluation of its antibacterial activity against agricultural plant pathogens.

PubMed

Paulkumar, Kanniah; Gnanajobitha, Gnanadhas; Vanaja, Mahendran; Rajeshkumar, Shanmugam; Malarkodi, Chelladurai; Pandian, Kannaiyan; Annadurai, Gurusamy

2014-01-01

Utilization of biological materials in synthesis of nanoparticles is one of the hottest topics in modern nanoscience and nanotechnology. In the present investigation, the silver nanoparticles were synthesized by using the leaf and stem extract of Piper nigrum. The synthesized nanoparticle was characterized by UV-vis spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), energy dispersive X-ray analysis (EDAX), and Fourier Transform Infrared Spectroscopy (FTIR). The observation of the peak at 460 nm in the UV-vis spectra for leaf- and stem-synthesized silver nanoparticles reveals the reduction of silver metal ions into silver nanoparticles. Further, XRD analysis has been carried out to confirm the crystalline nature of the synthesized silver nanoparticles. The TEM images show that the leaf- and stem-synthesized silver nanoparticles were within the size of about 7-50 nm and 9-30 nm, respectively. The FTIR analysis was performed to identify the possible functional groups involved in the synthesis of silver nanoparticles. Further, the antibacterial activity of the green-synthesized silver nanoparticles was examined against agricultural plant pathogens. The antibacterial property of silver nanoparticles is a beneficial application in the field of agricultural nanotechnology.

Characterisation of Sol-Gel Synthesis of Phase Pure CaTiO3 Nano Powders after Drying

NASA Astrophysics Data System (ADS)

Mallik, P. K.; Biswal, G.; Patnaik, S. C.; Senapati, S. K.

2015-02-01

According to a few recent studies, calcium titanate (CT) is a material that is similar to hydroxyapatite in biological properties. However, calcium titanate is not currently being used in the biomedical applications as to hydroxyapatite. The objective is to prepare nano calcium titanate powders from the equimolar solution of calcium oxide, ethanol and Titanium (IV) isopropoxide via sol-gel synthesis. The phase analysis and morphology of powder particles were studied by X-ray diffraction (XRD), while the composition and size of powder particles were determined by Transmission electron microscope (TEM) attached with energy dispersive x-ray spectrometer (EDS). As results, XRD confirm the presence of phase pure crystalline CaTiO3 after drying at 100°C for 24 hours, while TEM analysis confirms about 13 nm sizes of CaTiO3 particles and some agglomerated particle of 20-30 nm. Moreover, EDS analysis indicates that the approximately stoichiometric Ca/Ti ratio 1:1 was obtained in the CaTiO3 powders. Finally, it can be concluded that described sol-gel synthesis could be novel method for the production of nano CaTiO3 particles at lower temperature compared to any other methods of production.

Stability of Catalyzed Magnesium Hydride Nanocrystalline During Hydrogen Cycling. Part II: Microstructure Evolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Chengshang; Fang, Zhigang Zak; Bowman, Robert C.

2015-10-01

In Part I, the cyclic stabilities of the kinetics of catalyzed MgH2 systems including MgH2–TiH2, MgH2–TiMn2, and MgH2–VTiCr were investigated, showing stable kinetics at 300 °C but deteriorations of the hydrogenation kinetics at temperatures below 150 °C. The present Part II describes the characterization of uncycled and cycled catalyzed MgH2 by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analysis. XRD analysis shows the crystallite sizes of the Mg and MgH2 significantly increased after the cycling. The mean crystallite sizes of the catalysts (TiH2 and VTiCr) increased moderately after the cycling. SEMmore » and TEM imaging were used to compare the microstructures of uncycled (as-milled) and cycled materials, revealing a drastic change of the microstructure after 100 cycles. In particular, results from energy-dispersive spectroscopy (EDS) mapping show that a change of distribution of the catalyst particles in the Mg and MgH2 phase occurred during the cycling.« less

Influence of Mg doping on ZnO nanoparticles decorated on graphene oxide (GO) crumpled paper like sheet and its high photo catalytic performance under sunlight

NASA Astrophysics Data System (ADS)

Labhane, P. K.; Sonawane, S. H.; Sonawane, G. H.; Patil, S. P.; Huse, V. R.

2018-03-01

Mg doped ZnO nanoparticles decorated on graphene oxide (GO) sheets were synthesized by a wet impregnation method. The effect of Mg doping on ZnO and ZnO-GO composite has been evaluated by using x-ray diffraction (XRD), Williamson-Hall Plot (Wsbnd H Plot), field emission scanning electron microscope (FESEM), transmission electron microscopy (TEM) and energy dispersive x-ray spectroscopy (EDX). The physical parameters of as-prepared samples were estimated by XRD data. FESEM and HR-TEM images showed the uniform distribution of nanoparticles on GO crumpled paper like sheet. Solar light photocatalytic activities of samples were evaluated spectrophotometrically by the degradation of p-nitrophenol (PNP) and indigo carmine (IC) solution. Mgsbnd ZnO decorated on GO sheets exhibit excellent catalytic efficiency compared to all other prepared samples under identical conditions, degrading PNP and IC nearly 99% within 60 min under sunlight. The effective degradation by Mgsbnd ZnO decorated on GO sheet would be due to extended solar light absorption, enhanced adsorptivity on the composite catalyst surface and efficient charge separation of photo-induced electrons. Finally, plausible mechanism was suggested with the help of scavengers study.

Properties of Gd{sub 2}O{sub 3} nanoparticles studied by hyperfine interactions and magnetization measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Correa, E. L., E-mail: eduardo.correa@usp.br; Bosch-Santos, B.; Cavalcante, F. H. M.

2016-05-15

The magnetic behavior of Gd{sub 2}O{sub 3} nanoparticles, produced by thermal decomposition method and subsequently annealed at different temperatures, was investigated by magnetization measurements and, at an atomic level, by perturbed γ − γ angular correlation (PAC) spectroscopy measuring hyperfine interactions at {sup 111}In({sup 111}Cd) probe nuclei. Nanoparticle structure, size and shape were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). Magnetization measurements were carried out to characterize the paramagnetic behavior of the samples. XRD results show that all samples crystallize in the cubic-C form of the bixbyite structure with space group Ia3. TEM images showed that particlesmore » annealed at 873 K present particles with highly homogeneous sizes in the range from 5 nm to 10 nm and those annealed at 1273 K show particles with quite different sizes from 5 nm to 100 nm, with a wide size distribution. PAC and magnetization results show that samples annealed at 873 and 1273 K are paramagnetic. Magnetization measurements show no indication of blocking temperatures for all samples down to 2 K and the presence of antiferromagnetic correlations.« less

Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

PubMed Central

Ajibade, Peter A.; Botha, Nandipha L.

2017-01-01

We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II) dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA) to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles. PMID:28336865

Room temperature ferromagnetism of nanocrystalline Nd1.90Ni0.10O3-δ

NASA Astrophysics Data System (ADS)

Sarkar, B. J.; Mandal, J.; Dalal, M.; Bandyopadhyay, A.; Chakrabarti, P. K.

2018-05-01

Nanocrystalline sample of Ni2+ doped neodymium oxide (Nd1.90Ni0.10O3-δ, NNO) is synthesized by co-precipitation method. Analysis of X-ray diffraction (XRD) pattern by Rietveld refinement method confirms the desired phase of NNO and complete substitution of Ni2+ ions in the Nd2O3 lattice. Analyses of transmission electron microscopy (TEM) and Raman spectroscopy of NNO recorded at room temperature (RT) also substantiate this fact. Besides, no traces of impurities are found in the analyses of XRD, TEM and Raman data. Room temperature hysteresis loop of NNO suggests the presence of weak ferromagnetism (FM) in low field region ( 600 mT), but in high field region paramagnetism of the host is more prominent. Magnetization vs. temperature ( M- T) curve in the entire temperature range (300-5 K) is analyzed successfully by a combined equation generated from three-dimensional (3D) spin wave model and Curie-Weiss law, which suggests the presence of mixed paramagnetic phase together with ferromagnetic phase in the doped sample. The onset of magnetic ordering is analyzed by oxygen vacancy mediated F-center exchange (FCE) coupling mechanism.

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

PubMed Central

2008-01-01

Sulfur nanoparticles were synthesized from hazardous H2S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe3+–malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 andn-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H2S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5–15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

USGS Publications Warehouse

Drits, Victor A.; Środoń, Jan; Eberl, D.D.

1997-01-01

The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good agreement with estimates of the mean thickness of fundamental particles obtained both from TEM measurements and from fixed cations content, up to a mean value of 20 layers. Correction for instrumental broadening under the conditions employed here is unnecessary for this range of thicknesses.

Biological and catalytic applications of green synthesized fluorescent N-doped carbon dots using Hylocereus undatus.

PubMed

Arul, Velusamy; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok; Sethuraman, Mathur Gopalakrishnan

2017-03-01

In this work, a simple hydrothermal route for the synthesis of fluorescent nitrogen doped carbon dots (N-CDs) is reported. The Hylocereus undatus (H. undatus) extract and aqueous ammonia are used as carbon and nitrogen source, respectively. The optical properties of synthesized N-CDs are analyzed using UV-Visible (UV-Vis) and fluorescence spectroscopy. The surface morphology, elemental composition, crystallinity and functional groups present in the N-CDs are examined using high resolution transmission electron microscopy (HR-TEM) with energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, respectively. The synthesized N-CDs emit strong blue fluorescence at 400nm under the excitation of 320nm. Further, the excitation dependent emission properties are also observed from the fluorescence of synthesized N-CDs. The HR-TEM results reveal that synthesized N-CDs are in spherical shape with average diameter of 2.5nm. The XRD pattern exhibits, the graphitic nature of synthesized N-CDs. The doping of nitrogen is confirmed from the EDS and FT-IR studies. The cytotoxicity and biocompatibility of N-CDs are evaluated through MTT assay on L-929 (Lymphoblastoid-929) and MCF-7 (Michigan Cancer Foundation-7) cells. The results indicate that the fluorescent N-CDs show less cytotoxicity and good biocompatibility on both L-929 and MCF-7 cells. Moreover, the N-CDs show excellent catalytic activity towards the reduction of methylene blue by sodium borohydride. Copyright © 2017 Elsevier B.V. All rights reserved.

Amorphization of Ta2O5 under swift heavy ion irradiation

NASA Astrophysics Data System (ADS)

Cusick, Alex B.; Lang, Maik; Zhang, Fuxiang; Sun, Kai; Li, Weixing; Kluth, Patrick; Trautmann, Christina; Ewing, Rodney C.

2017-09-01

Crystalline Ta2O5 powder is shown to amorphize under 2.2 GeV 197Au ion irradiation. Synchrotron X-ray diffraction (XRD), Raman spectroscopy, small-angle X-ray scattering (SAXS), and transmission electron microscopy (TEM) were used to characterize the structural transition from crystalline to fully-amorphous. Based on Rietveld refinement of XRD data, the initial structure is orthorhombic (P2mm) with a very large unit cell (a = 6.20, b = 40.29, c = 3.89 Å; V = 971.7 Å3), ideally containing 22 Ta and 55 O atoms. At a fluence of approximately 3 × 1011 ions/cm2, a diffuse amorphous background becomes evident, increasing in intensity relative to diffraction maxima until full amorphization is achieved at approximately 3 × 1012 ions/cm2. An anisotropic distortion of the orthorhombic structure occurred during the amorphization process, with an approximately constant unit cell volume. The amorphous phase fraction as a function of fluence was determined, yielding a trend that is consistent with a direct-impact model for amorphization. SAXS and TEM data indicate that ion tracks exhibit a core-shell morphology. Raman data show that the amorphous phase is comprised of TaO6 and TaO5 coordination-polyhedra in contrast to the TaO6 and TaO7 units that exist in crystalline Ta2O5. Analysis of Raman data shows that oxygen-deficiency increases with fluence, indicating a loss of oxygen that leads to an estimated final stoichiometry of Ta2O4.2 at a fluence of 1 × 1013 ions/cm2.

Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.

Effects of various polyoxyethylene sorbitan monooils (Tweens) and sodium dodecyl sulfate on reflux synthesis of copper nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang Xifeng; Yin Hengbo; Cheng Xiaonong

2006-11-09

Size-controlled synthesis of phase pure Cu nanoparticles was carried out by using copper sulfate pentahydrate as a precursor, ascorbic acid as a reductant, Tweens and sodium dodecyl sulfate (SDS) as modifiers in an aqueous solution at 80 deg. C. The as-prepared Cu nanoparticles were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and Fourier transform infrared (FT-IR). The stabilizing effects of SDS and Tweens on the Cu nanoparticles should be through the coordination between Cu nanoparticles and the respective sulfate group and oxygen-containing bond. The synergic effect of the composite SDS and Tweensmore » on Cu nanoparticles was different from those arising from the individuals.« less

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens

PubMed Central

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-01-01

Background: Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. Objective: This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. Materials and Methods: AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Results: The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375–480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3–6 nm, 3–22 nm, and 3–18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] <25 μg/mL) > garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Conclusion: Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. SUMMARY The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger and cayenne pepper were evaluatedThe AgNPs formed were characterized using UV-Vis spectroscopy, SEM and TEM microscopy, as well as EDX, XRD and FTIR spectroscopy AgNPs were well dispersed with spherical shapes and average sizes of 3-6nm, 3-22nm and 3-18 nm for garlic, ginger and cayenne pepper respectivelyAmine, protein, phenolic and alkyne groups were revealed as the capping agents for the nanoparticlesThe silver nanoparticles were confirmed to be crystalline with characteristic face centred cubic natureThe antibacterial and antioxidant activities of the AgNPs confirmed the therapeutic potential of the AgNPs. Abbreviations used: AgNPs: Silver nanoparticles; UV-Vis: ultraviolet-visible; SEM: Scanning electron microscopy; TEM: Transmission electron microscopy; EDX: Energy dispersive X-ray; XRD: X-ray diffraction; FTIR: Fourier transform infrared; GaNPs: Garlic nanoparticles; GiNPs: Ginger nanoparticles; C.PeNPs: Cayenne pepper nanoparticles; FCC: Face centred cubic; SPR: Surface Plasmon resonance; ABTS-2: 2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid); DPPH-1: 1-diphenyl-2-picrylhydrazyl. PMID:28808381

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens.

PubMed

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-07-01

Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375-480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3-6 nm, 3-22 nm, and 3-18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] <25 μg/mL) > garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger and cayenne pepper were evaluatedThe AgNPs formed were characterized using UV-Vis spectroscopy, SEM and TEM microscopy, as well as EDX, XRD and FTIR spectroscopy AgNPs were well dispersed with spherical shapes and average sizes of 3-6nm, 3-22nm and 3-18 nm for garlic, ginger and cayenne pepper respectivelyAmine, protein, phenolic and alkyne groups were revealed as the capping agents for the nanoparticlesThe silver nanoparticles were confirmed to be crystalline with characteristic face centred cubic natureThe antibacterial and antioxidant activities of the AgNPs confirmed the therapeutic potential of the AgNPs. Abbreviations used: AgNPs: Silver nanoparticles; UV-Vis: ultraviolet-visible; SEM: Scanning electron microscopy; TEM: Transmission electron microscopy; EDX: Energy dispersive X-ray; XRD: X-ray diffraction; FTIR: Fourier transform infrared; GaNPs: Garlic nanoparticles; GiNPs: Ginger nanoparticles; C.PeNPs: Cayenne pepper nanoparticles; FCC: Face centred cubic; SPR: Surface Plasmon resonance; ABTS-2: 2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid); DPPH-1: 1-diphenyl-2-picrylhydrazyl.

Synthesis and characterization of barium hexaferrite with manganese (Mn) doping material as anti-radar

NASA Astrophysics Data System (ADS)

Susilawati, Doyan, Aris; Khalilurrahman

2017-01-01

Have been successfully synthesized barium powder doping Manganese hexaferrite with the expected potential as anti-radar material. Synthesis was done by using the co-precipitation method, the variation of the variable x concentrations used were 0; 0.2; 0.4; and 0.6 and calcined at temperatures of 400, 600 and 800°C. Characterization powders of hexaferrite have used XRD (X-Ray Diffraction), SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), LCR (inductance, capacitance, and resistance) meter, and VSM (Vibrating Sample Magnetometer). The higher the concentration and temperature of calcinations given affect the color of the powder. The test results using XRD indicates that it has formed barium hexaferrite phase with a hexagonal crystal structure. Tests using SEM showed that all the constituent elements barium powder hexaferrite by doping Manganese powders have been spread evenly. XRD test results were confirmed by a test using a TEM showing the crystal structure and the powder was sized nano particles. The results from the LCR meter showed that the barium powder hexaferrite by doping Manganese that has been synthesized classified in semiconductor materials. The result from VSM showed that the value of coercivity magnetic powder doped barium hexaferrite Manganese is smaller when compared with barium hexaferrite without doping and belong to the soft magnetic. Based on the results of the synthesis and characterization, we can conclude that the barium powder heksaferrite by doping Manganese potential as a material anti-radar.

Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.

Physicochemical characterizations of nano-palm oil fuel ash

NASA Astrophysics Data System (ADS)

Rajak, Mohd Azrul Abdul; Majid, Zaiton Abdul; Ismail, Mohammad

2015-07-01

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m2/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.

Fabrication of mesoporous iron (Fe) doped copper sulfide (CuS) nanocomposite in the presence of a cationic surfactant via mild hydrothermal method for supercapacitors

NASA Astrophysics Data System (ADS)

Brown, J. William; Ramesh, P. S.; Geetha, D.

2018-02-01

We report fabrication of mesoporous Fe doped CuS nanocomposites with uniform mesoporous spherical structures via a mild hydrothermal method employing copper nitrate trihydrate (Cu (NO3).3H2O), Thiourea (Tu,Sc(NH2)2 and Iron tri nitrate (Fe(No3)3) as initial materials with cationic surfactant cetyltrimethylamoniame bromide (CTAB) as stabilizer/size controller and Ethylene glycol as solvent at 130 °C temperature. The products were characterized by XRD, SEM/EDX, TEM, FTIR and UV analysis. X-ray diffraction (XRD) spectra confirmed the Fe doped CuS nanocomposites which are crystalline in nature. EDX and XRD pattern confirmed that the product is hexagonal CuS phase. Fe doped spherical structure of CuS with grain size of 21 nm was confirmed by XRD pattern. Fe doping was identified by energy dispersive spectrometry (EDS). The Fourier-transform infrared (FTIR) spectroscopy results revealed the occurrence of active functional groups required for the reduction of copper ions. Studies showed that after a definite time relining on the chosen copper source, the obtained Fe-CuS nanocomposite shows a tendency towards self-assembly and creating mesoporous like nano and submicro structures by TEM/SAED. The achievable mechanism of producing this nanocomposite was primarily discussed. The electrochemical study confirms the pseudocapacitive nature of the CuS and Fe-CuS electrodes. The CuS and Fe-CuS electrode shows a specific capacitance of about 328.26 and 516.39 Fg-1 at a scan rate of 5 mVs-1. As the electrode in a supercapacitor, the mesoporous nanostructured Fe-CuS shows excellent capacitance characteristics.

Boehmite nanostructures preparation by hydrothermal method from anodic aluminium oxide membrane.

PubMed

Yang, X; Wang, J Y; Pan, H Y

2009-02-01

Boehmite nanostructures were successfully synthesized from porous anodic aluminium oxide (AAO) membrane by a simple and efficient hydro-thermal method. The experiment used high purity alumina as raw material, and the whole reaction process avoided superfluous impurities to be introduced. Thus, the purity of Boehmite products was ensured. The examinations of the morphology and structure were carried out by atomic force microscope (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Composition of the specimens was analyzed using energy dispersive X-ray spectroscope (EDX) and X-ray diffraction (XRD). Based on these observations the growth process was analyzed.

Sonochemical fabrication of 8-hydroxyquinoline aluminum (Alq3) nanoflowers with high electrogenerated chemiluminescence.

PubMed

Mao, Chang-Jie; Wang, Dan-Chen; Pan, Hong-Cheng; Zhu, Jun-Jie

2011-03-01

Well-defined Alq(3) nanoflowers were fabricated via a facile and fast sonochemical route. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and shape of the as-prepared product. The results showed that the resulting Alq(3) was composed of nanobelts with thickness about 50 nm, average widths of 200 nm, and length up to 10 μm. The Alq(3) nanoflowers exhibited good electrogenerated chemiluminescence behavior. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis and characterization of graphene quantum dots/cobalt ferrite nanocomposite

NASA Astrophysics Data System (ADS)

Ramachandran, Shilpa; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.

2018-02-01

A facile method has been developed for the synthesis of a graphene quantum dots/cobalt ferrite nanocomposite. Graphene quantum dots (GQDs) were synthesized by a simple bottom-up method using citric acid, followed by the co-precipitation of cobalt ferrite nanoparticles on the graphene quantum dots. The morphology, structural analysis, optical properties, magnetic properties were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectroscopy, fluorescence spectroscopy, vibrating sample magnetometry (VSM) measurements. The synthesized nanocomposite showed good fluorescence and superparamagnetic properties, which are important for biomedical applications.

The Morphology of Titanium Dioxide Aerogels

NASA Astrophysics Data System (ADS)

Zhu, Zhu

The morphology of titanium dioxide TiO _2 aerogels has been characterized by four major techniques. This work will discuss these complementary techniques such as nitrogen adsorption, X-ray powder diffraction (XRD), electron microscopies (EM- TEM, SEM), and small angle neutron scattering (SANS). The results of these characterizations have shown that the morphology of titanium dioxide TiO_2 aerogels can be characterized in terms of two length scales: 5 nm diameter, crystalline nanoparticles of anatase closely packed into mesoaggregates about 50 nm in size. The mesoaggregates are, in turn, packed into a loosely linked structure with an overall porosity of 80%.

Hydrothermal Synthesis and Biocompatibility Study of Highly Crystalline Carbonated Hydroxyapatite Nanorods

NASA Astrophysics Data System (ADS)

Xue, Caibao; Chen, Yingzhi; Huang, Yongzhuo; Zhu, Peizhi

2015-08-01

Highly crystalline carbonated hydroxyapatite (CHA) nanorods with different carbonate contents were synthesized by a novel hydrothermal method. The crystallinity and chemical structure of synthesized nanorods were studied by Fourier transform infrared spectroscopy (FTIR), X-ray photo-electronic spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM). The biocompatibility of synthesized CHA nanorods was evaluated by cell viability and alkaline phosphatase (ALP) activity of MG-63 cell line. The biocompatibility evaluation results show that these CHA nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopedic application.

Composition, speciation and distribution of iron minerals in Imperata cylindrica.

PubMed

Amils, Ricardo; de la Fuente, Vicenta; Rodríguez, Nuria; Zuluaga, Javier; Menéndez, Nieves; Tornero, Jesús

2007-05-01

A comparative study of the roots, rhizomes and leaves of an iron hyperaccumulator plant, Imperata cylindrica, isolated from the banks of an extreme acidic environment, using complementary techniques: Mösbauer spectroscopy (MS), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled to energy-dispersive X-ray microanalysis (EDAX) and transmission electron microscopy (TEM), has shown that two main biominerals, jarosite and ferrihydrate-ferritin, accumulate in the different tissues. Jarosite accumulates mainly in roots and rhizomes, while ferritin has been detected in all the structures. A model of iron management in I. cylindrica is presented.

Synthesis on structure and properties of zinc nanocrystal in high ordered 3D nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sathyaseelan, B., E-mail: bsseelan03@gmail.com; Manigandan, A.; Anbarasu, V.

2015-06-24

The wet impregnation method was employed to prepare ZnO encapsulated in mesoporous silica (ZnO/KIT-6). The prepared ZnO/KIT-6 samples have been studied by X-ray diffraction, transmission electron microscope, and nitrogen adsorption–desorption isotherm. The low angle powder XRD patterns of Calcined ZnO/KIT-6 materials showed a phase that can be indexed to cubic Ia3d. Tem images revealed well ordered cubic 3D nanoporous chennels. The ZnO encapsulated in KIT-6 can be used as light-emitting diodes and ultraviolet nanolasers.

Effects of the Tempering and High-Pressure Torsion Temperatures on Microstructure of Ferritic/Martensitic Steel Grade 91

PubMed Central

Ganeev, Artur; Nikitina, Marina; Sitdikov, Vil; Islamgaliev, Rinat; Hoffman, Andrew; Wen, Haiming

2018-01-01

Grade 91 (9Cr-1Mo) steel was subjected to various heat treatments and then to high-pressure torsion (HPT) at different temperatures. Its microstructure was studied using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Effects of the tempering temperature and the HPT temperature on the microstructural features and microhardness in the ultrafine-grained (UFG) Grade 91 steel were researched. The study of the UFG structure formation takes into account two different microstructures observed: before HPT in both samples containing martensite and in fully ferritic samples. PMID:29671761

Preparation, characterization and antibacterial applications of ZnO-nanoparticles coated polyethylene films for food packaging.

PubMed

Tankhiwale, Rasika; Bajpai, S K

2012-02-01

The present work describes the preparation of ZnO nanoparticles loaded starch-coated polyethylene film. The presence of ZnO nanoparticles was confirmed by surface plasmon resonance (SPR), X-ray diffraction (XRD) studies and transmission electron microscopy (TEM). The ZnO loaded film was tested for its biocidal action against model bacteria Escherichia coli using zone inhibition and killing kinetics of bacterial growth methods. This newly developed material bears potential to be used as food packaging material to prevent food stuff from bacterial contamination. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis of Silver Nanoparticles Using Bombyxmori Silk Fibroin and Their Antibacterial Activity

NASA Astrophysics Data System (ADS)

Shivananda, C. S.; Lakshmeesha Rao, B.; Pasha, Azmath; Sangappa, Y.

2016-09-01

Present work describes the synthesis of colloidal silver nanoparticles using Bombyx mori silk fibroin under white light environment at room temperature. The bio reduction of silver ions showed the unique surface plasmon resonance (SPR) band at 420 nm which was confirmed by UV-visible spectroscopy. Transmission electron microscopy (TEM) showed the synthesized AgNPs are spherical in shape with the average particle size of 35-40 nm. X-ray diffraction (XRD) pattren evidenced the crystalline nature of the AgNPs with FCC structure. The biosynthesized AgNPs showed effective antibacterial activity against bacterial stains Bacillus subtilis, and Salmonella typhi.

Analysis on nonlinear optical properties of Cd (Zn) Se quantum dots synthesized using three different stabilizing agents

NASA Astrophysics Data System (ADS)

J, Joy Sebastian Prakash; G, Vinitha; Ramachandran, Murugesan; Rajamanickam, Karunanithi

2017-10-01

Three different stabilizing agents, namely, L-cysteine, Thioglycolic acid and cysteamine hydrochloride were used to synthesize Cd(Zn)Se quantum dots (QDs). It was characterized using UV-vis spectroscopy, x-ray diffraction (XRD) and transmission electron microscopy (TEM). The non-linear optical properties (non-linear absorption and non-linear refraction) of synthesized Cd(Zn)Se quantum dots were studied with z-scan technique using diode pumped continuous wavelaser system at a wavelength of 532 nm. Our (organic) synthesized quantum dots showed optical properties similar to the inorganic materials reported elsewhere.

Preparation and drug release behavior of temperature-responsive mesoporous carbons

NASA Astrophysics Data System (ADS)

Wang, Xiufang; Liu, Ping; Tian, Yong

2011-06-01

A temperature-responsive composite based on poly (N-isopropylacrylamide) (PNIPAAm) and ordered mesoporous carbons (OMCs) has been successfully prepared by a simple wetness impregnation technique. The structures and properties of the composite were characterized by infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 sorption, thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). The results showed that the inclusion of PNIPAAm had not greatly changed the basic ordered pore structure of the OMCs. Ibuprofen (IBU) was selected as model drug, and in vitro test of IBU release exhibited a temperature-responsive controlled release delivery.

Effect of Synthesis Parameter on Crystal Structures and Magnetic Properties of Magnesium Nickel Ferrite (Mg0.5Ni0.5Fe2O4) Nanoparticles

NASA Astrophysics Data System (ADS)

Maulia, R.; Putra, R. A.; Suharyadi, E.

2017-05-01

Mg0.5Ni0.5Fe2O4 nanoparticles have been successfully synthesized by using co-precipitation method and varying the synthesis parameter, i.e. synthesis temperature and NaOH concentration. X-ray Diffraction (XRD) pattern showed that nanoparticles have cubic spinel structures with an additional phase of γ-Fe2O3 and particle size varies within the range of 4.3 - 6.7 nm. This variation is due to the effect of various synthesis parameters. Transmission Electron Microscopy (TEM) image showed that the nanoparticles exhibited agglomeration. The observed diffraction ring from selected area electron diffraction showed that the sample was polycrystalline and confirmed the peak appearing in XRD. The coercivities showed an increasing trend with an increase in particle size from 44.7 Oe to 49.6 Oe for variation of NaOH concentration, and a decreasing trend with an increase in particle size from 46.8 to 45.1 Oe for variation of synthesis temperature. The maximum magnetization showed an increasing trend with an increase in the ferrite phase from 3.7 emu/g to 5.4 emu/g possessed in the sample with variations on NaOH concentration. The maximum magnetization for the sample with variations on synthesis temperature varied from 4.4 emu/g to 5.7 emu/g due to its crystal structures.

Electrical analysis of inter-growth structured Bi4Ti3O12-Na0.5Bi4.5Ti4O15 ceramics

NASA Astrophysics Data System (ADS)

Jiang, Xiangping; Jiang, Yalin; Jiang, Xingan; Chen, Chao; Tu, Na; Chen, Yunjing

2017-06-01

Inter-growth bismuth layer-structured ferroelectrics (BLSFs), Bi4Ti3O12-Na0.5Bi4.5Ti4O15 (BIT-NBT), were successfully synthesized using the traditional solid-state reaction method. X-ray diffraction (XRD) Rietveld refinements were conducted using GSAS software. Good agreement and low residual are obtained. The XRD diffraction peaks can be well indexed into I2cm space group. The inter-growth structure was further observed in the high-resolution TEM image. Dielectric and impedance properties were measured and systematically analyzed. At the temperature range 763-923 K (below {T}{{c}}), doubly ionized oxygen vacancies (OVs) are localized and the short-range hopping leads to the relaxation processes with an activation energy of 0.79-1.01 eV. Above {T}{{c}}, the doubly charged OVs are delocalized and become free ones, which contribute to the long-range dc conduction. The reduction in relaxation species gives rise to a higher relaxation activation energy ˜1.6  eV. Project supported by the National Natural Science Foundation of China (Grant Nos. 51562014, 51262009, and 51602135).

Annealing effect on thermal conductivity and microhardness of carbon nanotube containing Se80Te16Cu4 glassy composites

NASA Astrophysics Data System (ADS)

Upadhyay, A. N.; Tiwari, R. S.; Singh, Kedar

2018-02-01

This study deals with the effect of thermal annealing on structural/microstructural, thermal and mechanical behavior of pristine Se80Te16Cu4 and carbon nanotubes (CNTs) containing Se80Te16Cu4 glassy composites. Pristine Se80Te16Cu4, 3 and 5 wt%CNTs-Se80Te16Cu4 glassy composites are annealed in the vicinity of glass transition temperature to onset crystallization temperature (340-380 K). X-ray diffraction (XRD) pattern revealed formation of polycrystalline phases of hexagonal CuSe and trigonal selenium. The indexed d-values in XRD patterns are in well conformity with the d-values obtained after the indexing of the ring pattern of selected area electron diffraction pattern of TEM images. The SEM investigation exhibited that the grain size of the CNTs containing Se80Te16Cu4 glassy composites increased with increasing annealing temperature and decreased at further higher annealing temperature. Thermal conductivity, microhardness exhibited a substantial increase with increasing annealing temperature of 340-360 K and slightly decreases for 380 K. The variation of thermal conductivity and microhardness can be explained by cross-linking formation and voids reduction.

Nanorods, nanospheres, nanocubes: Synthesis, characterization and catalytic activity of nanoferrites of Mn, Co, Ni, Part-89

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Supriya; Srivastava, Pratibha; Singh, Gurdip, E-mail: gsingh4us@yahoo.com

2013-02-15

Graphical abstract: Prepared nanoferrites were characterized by FE-SEM and bright field TEM micrographs. The catalytic effect of these nanoferrites was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG–DSC techniques. The kinetics of thermal decomposition of AP was evaluated using isothermal TG data by model fitting as well as isoconversional method. Display Omitted Highlights: ► Synthesis of ferrite nanostructures (∼20.0 nm) by wet-chemical method under different synthetic conditions. ► Characterization using XRD, FE-SEM, EDS, TEM, HRTEM and SAED pattern. ► Catalytic activity of ferrite nanostructures on AP thermal decomposition by thermal techniques. ► Burning rate measurements ofmore » CSPs with ferrite nanostructures. ► Kinetics of thermal decomposition of AP + nanoferrites. -- Abstract: In this paper, the nanoferrites of Mn, Co and Ni were synthesized by wet chemical method and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive, X-ray spectra (EDS), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HR-TEM). It is catalytic activity were investigated on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) using thermogravimetry (TG), TG coupled with differential scanning calorimetry (TG–DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + nanoferrites have also been investigated using isoconversional and model fitting approaches which have been applied to data for isothermal TG decomposition. The burning rate of CSPs was considerably enhanced by these nanoferrites. Addition of nanoferrites to AP led to shifting of the high temperature decomposition peak toward lower temperature. All these studies reveal that ferrite nanorods show the best catalytic activity superior to that of nanospheres and nanocubes.« less

Effective coating of titania nanoparticles with alumina via atomic layer deposition

NASA Astrophysics Data System (ADS)

Azizpour, H.; Talebi, M.; Tichelaar, F. D.; Sotudeh-Gharebagh, R.; Guo, J.; van Ommen, J. R.; Mostoufi, N.

2017-12-01

Alumina films were deposited on titania nanoparticles via atomic layer deposition (ALD) in a fluidized bed reactor at 180 °C and 1 bar. Online mass spectrometry was used for real time monitoring of effluent gases from the reactor during each reaction cycle in order to determine the optimal dosing time of precursors. Different oxygen sources were used to see which oxygen source, in combination with trimethyl aluminium (TMA), provides the highest alumina growth per cycle (GPC). Experiments were carried out in 4, 7 and 10 cycles using the optimal dosing time of precursors. Several characterization methods, such as high resolution transmission electron microscopy (HRTEM), Brunauer-Emmett-Teller (BET), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR), X-ray diffraction (XRD) and instrumental neutron activation analysis (INAA), were conducted on the products. Formation of the alumina film was confirmed by EDX mapping and EDX line profiling, FTIR and TEM. When using either water or deuterium oxide as the oxygen source, the thickness of the alumina film was greater than that of ozone. The average GPC measured by TEM for the ALD of TMA with water, deuterium oxide and ozone was about 0.16 nm, 0.15 nm and 0.11 nm, respectively. The average GPC calculated using the mass fraction of aluminum from INAA was close to those measured from TEM images. Excess amounts of precursors lead to a higher average growth of alumina film per cycle due to insufficient purging time. XRD analysis demonstrated that amorphous alumina was coated on titania nanoparticles. This amorphous layer was easily distinguished from the crystalline core in the TEM images. Decrease in the photocatalytic activity of titania nanoparticles after alumina coating was confirmed by measuring degradation of Rhodamine B by ultraviolet irradiation.

Fabrication of Mesoporous Silica/Alumina Hybrid Membrane Film Nanocomposites using Template Sol-Gel Synthesis of Amphiphilic Triphenylene

NASA Astrophysics Data System (ADS)

Lintang, H. O.; Jalani, M. A.; Yuliati, L.; Salleh, M. M.

2017-05-01

Herein we reported that by introducing a one-dimensional (1D) substrate with a porous structure such as anodic aluminum oxide (AAO) membrane, mesoporous silica/alumina hybrid nanocomposites were successfully fabricated by using amphiphilic triphenylene (TPC10TEG) as a template in sol-gel synthesis (TPC10TEG/silicahex). For the optical study of the nanocomposites, TPC10TEG/silicahex showed absorption peak at 264 nm due to the ordered and long-range π-π stacking of the disc-like aromatic triphenylene core. Moreover, the hexagonal arrangement of TPC10TEG/silicahex was proven based on their diffraction peaks of d 100 and d 200 at 2θ = 2.52° and 5.04° and images of transmission electron microscopy (TEM), respectively. For fabrication of mesoporous silica/alumina hybrid membrane, TPC10TEG/silicahex was drop-casted onto AAO membrane for penetration into the porous structure via gravity. X-ray diffraction (XRD) analysis on the resulted hybrid nanocomposites showed that the diffraction peaks of d 100 and d 200 of TPC10TEG/silicahex were still preserved, indicating that the hexagonal arrangements of mesoporous silica were maintained even on AAO substrate. The morphology study on the hybrid nanocomposites using TEM, scanning electron microscope (SEM) and field emission scanning electron microscope (FE-SEM) showed the successful filling of most AAO channels with the TPC10TEG/silicahex nanocomposites.

Twin density of aragonite in molluscan shells characterized using X-ray diffraction and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Checa, Antonio G.; Sasaki, Takenori; Nagasawa, Hiromichi

2014-07-01

{110} twin density in aragonites constituting various microstructures of molluscan shells has been characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM), to find the factors that determine the density in the shells. Several aragonite crystals of geological origin were also investigated for comparison. The twin density is strongly dependent on the microstructures and species of the shells. The nacreous structure has a very low twin density regardless of the shell classes. On the other hand, the twin density in the crossed-lamellar (CL) structure has large variation among classes or subclasses, which is mainly related to the crystallographic direction of the constituting aragonite fibers. TEM observation suggests two types of twin structures in aragonite crystals with dense {110} twins: rather regulated polysynthetic twins with parallel twin planes, and unregulated polycyclic ones with two or three directions for the twin planes. The former is probably characteristic in the CL structures of specific subclasses of Gastropoda. The latter type is probably related to the crystal boundaries dominated by (hk0) interfaces in the microstructures with preferred orientation of the c-axis, and the twin density is mainly correlated to the crystal size in the microstructures.

Microwave-assisted hydrothermal synthesis of biocompatible silver sulfide nanoworms

NASA Astrophysics Data System (ADS)

Xing, Ruimin; Liu, Shanhu; Tian, Shufang

2011-10-01

In this study, silver sulfide nanoworms were prepared via a rapid microwave-assisted hydrothermal method by reacting silver nitrate and thioacetamide in the aqueous solution of the Bovine Serum Albumin (BSA) protein. The morphology, composition, and crystallinity of the nanoworms were characterized by field emission scanning electron microscopy (FESEM), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray energy dispersive spectroscopy (EDS), and Fourier transform infrared (FTIR) spectroscopy. The results show that the nanoworms were assembled by multiple adjacent Ag2S nanoparticles and stabilized by a layer of BSA attached to their surface. The nanoworms have the sizes of about 50 nm in diameter and hundreds of nanometers in length. The analyses of high-resolution TEM and their correlative Fast Fourier Transform (FFT) indicate that the adjacent Ag2S nanoparticles grow by misoriented attachment at the connective interfaces to form the nanoworm structure. In vitro assays on the human cervical cancer cell line HeLa show that the nanoworms exhibit good biocompatibility due to the presence of BSA coating. This combination of features makes the nanoworms attractive and promising building blocks for advanced materials and devices.

Green synthesis of Silver and Gold Nanoparticles for Enhanced catalytic and bactericidal activity

NASA Astrophysics Data System (ADS)

Naraginti, S.; Tiwari, N.; Sivakumar, A.

2017-11-01

A rapid one step green synthetic method using kiwi fruit extract was employed for preparation of silver and gold nanoparticles. The synthesized nanoparticles were successfully used as green catalysts for the reduction of 4-nitrophenol (4-NP) and methylene blue (MB). They also exhibited excellent antimicrobial activity against clinically isolated Pseudomonas aeruginosa (P.aeruginosa) and Staphylococcus aureus (S.aureus). It was noticed that with increase in concentration of the aqueous silver and gold solutions, particle size of the Ag and Au NPS showed increase as evidenced from UV-Visible spectroscopy and TEM micrograph. The method employed for the synthesis required only a few minutes for more than 90% formation of nanoparticles when the temperature was raised to 80°C. It was also noticed that the catalytic activity of nanoparticles depends upon the size of the particles. These nanoparticles were observed to be crystalline from the clear lattice fringes in the transmission electron microscopic (TEM) images, bright circular spots in the selected area electron diffraction (SAED) pattern and peaks in the X-ray diffraction (XRD) pattern. The Fourier-transform infrared (FTIR) spectrum indicated the presence of different functional groups in the biomolecule capping the nanoparticles.

Zn(II)-PEG 300 globules as soft template for the synthesis of hexagonal ZnO micronuts by the hydrothermal reaction method.

PubMed

Shi, Xixi; Pan, Lingling; Chen, Shuoping; Xiao, Yong; Liu, Qiaoyun; Yuan, Liangjie; Sun, Jutang; Cai, Lintao

2009-05-19

Hexagonal ZnO micronuts (HZMNs) have been successfully synthesized with the assistance of poly(ethylene glycol) (PEG) 300 via a hydrothermal method. The structure and morphology of the HZMNs were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). An individual ZnO micronut is revealed as twinned crystals. Time-dependent investigation shows that the growth of HZMNs involves a dissolution-recrystallization process followed by Ostwald ripening, in which is the first formed solid ZnO particles dissolve and transform to HZMNs with hollow structure. PEG 300 has been found to play a crucial role in the growth of this unique hollow structure. TEM observations show that the PEG chains aggregate to globules in water, which then have interaction with the dissolved zinc species to form the globules in a coiled state under hydrothermal conditions. These Zn(II)-PEG 300 globules act as soft template for the growth of HZMNs, and the possible growth mechanism is proposed. The room-temperature photoluminescence (PL) spectrum shows red emission around 612 nm with a full width at half-maximum (fwhm) only about 13 nm.

Effect of aluminum and yttrium doping on zinc sulphide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Swati, E-mail: sharma.swati1507@gmail.com; Kashyap, Jyoti; Kapoor, A.

2016-05-06

In this work, pristine and doped Zinc Sulphide (ZnS) nanoparticles have been synthesized via chemical co-precipitation method. ZnS nanoparticles have been doped with Aluminium (Al) and Yttrium (Y) with doping concentration of 5wt% each. The structural and optical properties of the as prepared nanoparticles have been studied using X-Ray diffraction (XRD) technique and Photoluminescence spectroscopy. Average grain size of 2-3nm is observed through the XRD analysis. Effect of doping on stress, strain and lattice constant of the nanoparticles has also been analyzed. Photoluminescence spectra of the as prepared nanoparticles is enhanced due to Al doping and quenched due to Ymore » doping. EDAX studies confirm the relative doping percentage to be 3.47 % and 3.94% by wt. for Al and Y doped nanoparticles respectively. Morphology of the nanoparticles studied using TEM and SEM indicates uniform distribution of spherical nanoparticles.« less

A High Sensitivity Isopropanol Vapor Sensor Based on Cr₂O₃-SnO₂ Heterojunction Nanocomposites via Chemical Precipitation Route.

PubMed

Jawaher, K Rackesh; Indirajith, R; Krishnan, S; Robert, R; Pasha, S K Khadheer; Deshmukh, Kalim; Sastikumar, D; Das, S Jerome

2018-08-01

Cr2O3-SnO2 heterojunction nanocomposites were prepared via chemical precipitation method. The prepared samples were characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra and Field Emission Electron Microscopy (FESEM). The XRD spectrum confirms the presence of both tetragonal rutile SnO2 and rhombohedral corundum Cr2O3 structure. Further investigation into the gas sensing performances of the prepared Cr2O3-SnO2 nanocomposites exhibited an enhanced sensitivity towards VOPs such as isopropanol, acetone, ethanol and formaldehyde. Especially, isopropanol vapor sensor shows excellent sensitivity at an operating temperature of 100 °C. The highest sensitivity for Cr2O3-SnO2 heterojunction nanocomposites indicate that these materials can be a good candidate for the production of high-performance isopropanol sensors.

Extracellular biosynthesis of gold and silver nanoparticles using Krishna tulsi ( Ocimum sanctum) leaf

NASA Astrophysics Data System (ADS)

Philip, Daizy; Unni, C.

2011-05-01

Aqueous extract of Ocimum sanctum leaf is used as reducing agent for the environmentally friendly synthesis of gold and silver nanoparticles. The nanoparticles were characterized using UV-vis, transmission electron microscopy (TEM), X-ray diffraction (XRD) and FTIR analysis. These methods allow the synthesis of hexagonal gold nanoparticles having size ∼30 nm showing two surface plasmon resonance (SPR) bands by changing the relative concentration of HAuCl 4 and the extract. Broadening of SPR is observed at larger quantities of the extract possibly due to biosorption of gold ions. Silver nanoparticles with size in the range 10-20 nm having symmetric SPR band centered around 409 nm are obtained for the colloid synthesized at room temperature at a pH of 8. Crystallinity of the nanoparticles is confirmed from the XRD pattern. Biomolecules responsible for capping are different in gold and silver nanoparticles as evidenced by the FTIR spectra.

Synthesis, characterization, bioactivity and antibacterial studies of silver doped calcium borosilicate glass-ceramics

NASA Astrophysics Data System (ADS)

Kumar, Alesh; Mariappan, C. R.

2018-04-01

Bioactive glass-ceramics 45.8 mol% SiO- 45.8 CaO - 8.4 B2O3 doped with Ag2O were synthesized by sol-gel method. The glass-ceramic nature of samples was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis. Fourier transform infrared (FT-IR) spectra reveal the probable stretching and bending vibration modes of silicate and borate groups. UV-Visible spectra reveal the presence of Ag+ ions and metallic Ag in the glass matrix for Ag2O doped ceramic sample. Biocompatibility of the glass nature of samples was studied by soaking of samples in Dulbecco's Modified Eagle's Medium (DMEM) with subsequent XRD studies. It was found that bone-like apatite formation on the glasses after soaked in DMEM. Antibacterial studies of glass ceramics powder against gram positive and negative microorganisms were carried out.

Structural and magnetic properties of chromium doped zinc ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sebastian, Rintu Mary; Thankachan, Smitha; Xavier, Sheena

2014-01-28

Zinc chromium ferrites with chemical formula ZnCr{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by Sol - Gel technique. The structural as well as magnetic properties of the synthesized samples have been studied and reported here. The structural characterizations of the samples were analyzed by using X – Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The single phase spinel cubic structure of all the prepared samples was tested by XRD and FTIR. The particle size was observed to decrease from 18.636 nm to 6.125more » nm by chromium doping and induced a tensile strain in all the zinc chromium mixed ferrites. The magnetic properties of few samples (x = 0.0, 0.4, 1.0) were investigated using Vibrating Sample Magnetometer (VSM)« less

In situ synthesis of hydroxyapatite coating by laser cladding.

PubMed

Wang, D G; Chen, C Z; Ma, J; Zhang, G

2008-10-15

HA bioceramic coatings were synthesized on titanium substrate by laser cladding using cheap calcium carbonate and calcium hydrogen phosphate. The thermodynamic condition for synthesizing HA was calculated by software Matlab 5.0, the microstructure and phase analysis of laser clad HA bioceramic coatings were studied by electron probe microanalyser (EPMA), X-ray diffractometer (XRD) and transmission electron microscopy (TEM). The theoretical results show that the Gibbs free enthalpy for the synthesis of HA phase is satisfied, and the presence of HA phase in the clad coatings was then further verified by XRD and the selected area diffraction patterns. When the laser power is 600W and the scanning speed is 3.5mm/s, the compact HA bioceramic coatings were obtained, which have cellular dendritic structure and consist of the phases of HA, alpha-Ca(2)P(2)O(7), CaO and CaTiO(3).

One step electrochemical synthesis of bimetallic PdAu supported on nafion–graphene ribbon film for ethanol electrooxidation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shendage, Suresh S., E-mail: sureshsshendage@gmail.com; Singh, Abilash S.; Nagarkar, Jayashree M., E-mail: jm.nagarkar@ictmumbai.edu.in

2015-10-15

Highlights: • Electrochemical deposition of bimetallic PdAu NPs. • Highly loaded PdAu NPs are obtained. • Nafion–graphene supported PdAu NPs shows good activity for ethanol electrooxidation. - Abstract: A nafion–graphene ribbon (Nf–GR) supported bimetallic PdAu nanoparticles (PdAu/Nf–GR) catalyst was prepared by electrochemical codeposition of Pd and Au at constant potential. The prepared catalyst was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM) and X-ray diffraction analysis (XRD). The average particle size of PdAu nanoparticles (NPs) determined from XRD was 3.5 nm. The electrocatalytic activity of the PdAu/Nf–GR catalyst was examined by cyclic voltametry.more » It was observed that the as prepared catalyst showed efficient activity and good stability for ethanol electrooxidation in alkaline medium.« less

Synthesis of gold nanochains via photoactivation technique and their catalytic applications.

PubMed

Sinha, Arun Kumar; Basu, Mrinmoyee; Sarkar, Sougata; Pradhan, Mukul; Pal, Tarasankar

2013-05-15

The article reports a simple photoactivation technique for the synthesis of chain like assembly of spherical Au nanocrystals using a nontoxic biochemical, β-cyclodextrin under ~365 nm UV-light irradiation. Under UV irradiation, β-cyclodextrin acts as a reducing as well as capping agent and eventually becomes a stabilizing linker for Au nanoparticles. The UV-visible spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), and X-ray photoelectron spectroscopic techniques are employed to systematically characterize the Au nanochains. Additionally, it is shown that the Au nanocrystals act as an effective catalyst for the reduction in nitrobenzene to aniline and methylene blue to leuco methylene blue in presence of suitable reducing agent. The catalytic reduction reactions and kinetic parameters are evaluated from UV-visible spectroscopy. Copyright © 2013 Elsevier Inc. All rights reserved.

Characterisation of phases in nanostructured, multilayered titanium alloys by analytical and high-resolution electron microscopy.

PubMed

Czyrska-Filemonowicz, A; Buffat, P A

2009-01-01

Surface processing of a Ti-6Al-4V alloy led to a complex multilayered microstructure containing several phases of the Ni-Ti-P-Al-O system, which improves the mechanical and tribological surface properties. The microstructure, chemical and phase compositions of the hard layer formed on the surface were investigated by LM, XRD, SEM as well as analytical/high-resolution TEM, STEM, EDS, electron diffraction and FIB. Phase identification based on electron diffraction, HRTEM and EDS microanalysis revealed the presence of several binary and ternary phases in the system Ti-Ni-P, sometimes with partial substitution of Ti by Al. However some phases, mainly nanoparticles, still remain not identified satisfactorily. Electron microscopy techniques used for identification of phases present in surface multilayers and some practical limits to their routine application are reminded here.

Impedance spectroscopic and dielectric properties of nanosized Y2/3Cu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Sharma, Sunita; Yadav, Shiv Sundar; Singh, M. M.; Mandal, K. D.

2014-11-01

Yttrium Copper Titanate (Y2/3Cu3Ti4O12) nanoceramic is structurally analogous to CaCu3Ti4O12 (CCTO). X-ray diffraction (XRD) of Y2/3Cu3Ti4O12 (YCTO) shows the presence of all normal peaks of CCTO. SEM micrograph exhibits the presence of bimodal grains of size ranging from 1-2 μm. Bright field TEM image clearly displays nanocrystalline particle which is supported by presence of a few clear rings in the corresponding selected area electron diffraction (SAED) pattern. It exhibits a high value of dielectric constant (ɛ‧ = 8434) at room temperature and 100 Hz frequency with characteristic relaxation peaks. Impedance and modulus studies revealed the presence of temperature-dependent Maxwell-Wagner type of relaxation in the ceramic.

Green synthesis of gold nanoparticles using Citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) aqueous extract and its characterization.

PubMed

Sujitha, Mohanan V; Kannan, Soundarapandian

2013-02-01

This study reports the biological synthesis of gold nanoparticles by the reduction of HAuCl(4) by using citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) juice extract as the reducing and stabilizing agent. A various shape and size of gold nanoparticles were formed when the ratio of the reactants were altered with respect to 1.0mM chloroauric acid solution. The gold nanoparticles obtained were characterized by UV-visible spectra, transmission electron microscopy (TEM) and X-ray diffraction (XRD). TEM studies showed the particles to be of various shapes and sizes and particle size ranges from 15 to 80 nm. Selected-area electron diffraction (SAED) pattern confirmed fcc phase and crystallinity of the particles. The X-ray diffraction analysis revealed the distinctive facets (111, 200, 220 and 222 planes) of gold nanoparticles. Dynamic light scattering (DLS) studies revealed that the average size for colloid gp(3) of C. limon, C. reticulata and C. sinensis are 32.2 nm, 43.4 nm and 56.7 nm respectively. The DLS graph showed that the particles size was larger and more polydispersed compared to the one observed by TEM due to the fact that the measured size also includes the bio-organic compounds enveloping the core of the Au NPs. Zeta potential value for gold nanoparticles obtained from colloid gp(3) of C. limon, C. reticulata and C. sinensis are -45.9, -37.9 and -31.4 respectively indicating the stability of the synthesized nanoparticles. Herein we propose a novel, previously unexploited method for the biological syntheses of polymorphic gold nanoparticles with potent biological applications. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis of hollow ZnO microspheres by an integrated autoclave and pyrolysis process.

PubMed

Duan, Jinxia; Huang, Xintang; Wang, Enke; Ai, Hanhua

2006-03-28

Hollow zinc oxide microspheres have been synthesized from a micro ZnBr2·2H2O precursor obtained by an autoclave process in bromoform steam at 220 °C /2.5 MPa. Field-emission scanning electron microscropy (FE-SEM) and transmission electron microscopy (TEM) show that the products are about 1.0 µm single crystal spherical particles with hollow interiors, partly open surfaces and walls self-assembled by ZnO nanoparticles. X-ray diffraction (XRD) analysis shows that the as-prepared ZnO hollow spheres are of a hexagonal phase structure. A possible formation mechanism is suggested on the basis of the shape evolution of ZnO nanostructures observed by SEM and TEM. The room-temperature photoluminescence (PL) spectrum shows UV emission around 386 nm and weak green emission peaks indicating that there are few defects in the single crystal grains of the ZnO microspheres.

Synthesis of nano-crystalline hydroxyapatite and ammonium sulfate from phosphogypsum waste

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mousa, Sahar, E-mail: dollyriri@yahoo.com; King Abdulaziz University, Science and Art College, Chemistry Department, Rabigh Campus, P.O. Box:344, Postal code: 21911 Rabigh; Hanna, Adly

2013-02-15

Graphical abstract: TEM micrograph of dried HAP at 800 °C. -- Abstract: Phosphogypsum (PG) waste which is derived from phosphoric acid manufacture by using wet method was converted into hydroxyapatite (HAP) and ammonium sulfate. Very simple method was applied by reacting PG with phosphoric acid in alkaline medium with adjusting pH using ammonia solution. The obtained nano-HAP was dried at 80 °C and calcined at 600 °C and 900 °C for 2 h. Both of HAP and ammonium sulfate were characterized by X-ray diffraction (XRD) and infrared spectroscopy (IR) to study the structural evolution. The thermal behavior of nano-HAP wasmore » studied; the particle size and morphology were estimated by using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). All the results showed that HAP nano-crystalline and ammonium sulfate can successfully be produced from phosphogypsum waste.« less

Biocatalytic and antibacterial visualization of green synthesized silver nanoparticles using Hemidesmus indicus.

PubMed

Latha, M; Sumathi, M; Manikandan, R; Arumugam, A; Prabhu, N M

2015-05-01

In the present investigation, we described the green synthesis of silver nanoparticles using plant leaf extract of Hemidesmus indicus. The synthesized silver nanoparticles were characterized by UV-visible spectroscopy, fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX). TEM images proved that the synthesized silver nanoparticles were spherical in shape with an average particle size of 25.24 nm. To evaluate antibacterial efficacy, bacteria was isolated from poultry gut and subjected to 16S rRNA characterization and confirmed as Shigella sonnei. The in vitro antibacterial efficacy of synthesized silver nanoparticles was studied by agar bioassay, well diffusion and confocal laser scanning microscopy (CLSM) assay. The H. indicus mediated synthesis of silver nanoparticles shows rapid synthesis and higher inhibitory activity (34 ± 0.2 mm) against isolated bacteria S. sonnei at 40 μg/ml. Copyright © 2015 Elsevier Ltd. All rights reserved.

High-performance anode based on porous Co3O4 nanodiscs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Anqiang; Wang, Yaping; Xu, Wu

2014-06-01

In this article, two-dimensional, Co3O4 hexagonal nanodiscs are prepared using a hydrothermal method without surfactants. X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) have been employed to characterize the structural properties. As revealed by the SEM and TEM experiments, the thickness of our as-fabricated Co3O4 hexagonal nanodiscs is about 20 nm, and the pore diameters range from several nanometers to 30 nm. As an anode for lithium-ion batteries, porous Co3O4 nanodiscs exhibit an average discharge voltage of ~1 V (Vs. Li/Li+) and a high specific charge capacity of 1161 mAh g-1 after 100 cycles. They alsomore » demonstrate excellent rate performance and high Coloumbic efficiency at various rates. These results indicate that porous Co3O4 nanodiscs are good candidates as anode materials for lithium-ion batteries.« less

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fatimah, Is, E-mail: isfatimah@uii.ac.id; Yudha, Septian P.; Mutiara, Nur Afisa Lintang

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particlemore » sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.« less

Reusability Performance of Zinc Oxide Nanoparticles for Photocatalytic Degradation of POME

NASA Astrophysics Data System (ADS)

Zarifah Zainuri, Nur; Hanis Hayati Hairom, Nur; Abu Bakar Sidik, Dilaelyana; Misdan, Nurasyikin; Yusof, Norhaniza; Wahab Mohammad, Abdul

2018-03-01

Performance and reusability of different zinc oxide nanoparticles (ZnO-PVP and ZnO-PEG) for photocatalytic degradation of palm-mill oil effluent (POME) has been studied. The nanoparticles properties were characterised with fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The TEM results show that ZnO-PEG nanoparticles exhibit the smaller size than ZnO-PVP with less agglomeration. It was found that ZnO-PEG shows better effectiveness than ZnO-PVP in reducing turbidity, colour and increasing the dissolved oxygen (DO). By using two types of reusability methods: (a) oven drying (b) hot water rinsing, the oven drying method portrayed the most efficient route for POME treatment. This research would be a solution to the palm oil industry for photocatalyst recovering as well as reduction of the chemical usage in order to meet the development of advanced and greener technologies.

Hollow raspberry-like PdAg alloy nanospheres: High electrocatalytic activity for ethanol oxidation in alkaline media

NASA Astrophysics Data System (ADS)

Peng, Cheng; Hu, Yongli; Liu, Mingrui; Zheng, Yixiong

2015-03-01

Palladium-silver (PdAg) alloy nanospheres with unique structure were prepared using a one-pot procedure based on the galvanic replacement reaction. Their electrocatalytic activity for ethanol oxidation in alkaline media was evaluated. The morphology and crystal structure of the samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Electrochemical characterization techniques, including cyclic voltammetry (CV) and chronoamperometry (CA) measurements were used to analyze the electrochemical performance of the PdAg alloy nanospheres. The SEM and TEM images showed that the PdAg alloy nanospheres exhibit a hierarchical nanostructure with hollow interiors and porous walls. Compared to the commercial Pd/C catalyst, the as-prepared PdAg alloy nanospheres exhibit superior electrocatalytic activity and stability towards ethanol electro-oxidation in alkaline media, showing its potential as a new non-Pt electro-catalyst for direct alcohol fuel cells (DAFCs).

Formation of organoclays by a one step synthesis

NASA Astrophysics Data System (ADS)

Jaber, Maguy; Miéhé-Brendlé, Jocelyne; Delmotte, Luc; Le Dred, Ronan

2005-05-01

Different lamellar hybrid inorganic-organic materials having as inorganic parent 2:1 (T.O.T.) phyllosilicates such as talc, saponite, pyrophyllite, beidellite and montmorillonite were prepared by a one step synthesis. The solids were characterized by X-ray diffraction, solid state 29Si, 27Al, and 19F nuclear magnetic resonance and transmission electron microscopy. XRD patterns show that solids with inorganic parents having octahedral sheet based on aluminium exhibit a lamellar structure similar to MCM-50, whereas those with magnesium have an organophyllosilicate structure. In the first case, the absence of hexacoordinated aluminium was confirmed by 27Al NMR and an ordered stacking of the layers is observed on TEM micrographs. In opposite, a disorder is observed on the TEM images of organophyllosilicates. The formation of the 2:1 structure was found to be controlled mainly by the insertion of silicic species in the interlamellar space of brucite like layers.

Performance of carbon nanofiber supported Pd-Ni catalysts for electro-oxidation of ethanol in alkaline medium

NASA Astrophysics Data System (ADS)

Maiyalagan, T.; Scott, Keith

Carbon nanofibers (CNF) supported Pd-Ni nanoparticles have been prepared by chemical reduction with NaBH 4 as a reducing agent. The Pd-Ni/CNF catalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical voltammetry analysis. TEM showed that the Pd-Ni particles were quite uniformly distributed on the surface of the carbon nanofiber with an average particle size of 4.0 nm. The electro-catalytic activity of the Pd-Ni/CNF for oxidation of ethanol was examined by cyclic voltammetry (CV). The onset potential was 200 mV lower and the peak current density four times higher for ethanol oxidation for Pd-Ni/CNF compared to that for Pd/C. The effect of an increase in temperature from 20 to 60 °C had a great effect on increasing the ethanol oxidation activity.

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

NASA Astrophysics Data System (ADS)

Fatimah, Is; Yudha, Septian P.; Mutiara, Nur Afisa Lintang

2016-02-01

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particle sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.

The structure and transformation of the nanomineral schwertmannite: a synthetic analog representative of field samples

NASA Astrophysics Data System (ADS)

French, Rebecca A.; Monsegue, Niven; Murayama, Mitsuhiro; Hochella, Michael F.

2014-04-01

The phase transformation of schwertmannite, an iron oxyhydroxide sulfate nanomineral synthesized at room temperature and at 75 °C using H2O2 to drive the precipitation of schwertmannite from ferrous sulfate (Regenspurg et al. in Geochim Cosmochim Acta 68:1185-1197, 2004), was studied using high-resolution transmission electron microscopy. The results of this study suggest that schwertmannite synthesized using this method should not be described as a single phase with a repeating unit cell, but as a polyphasic nanomineral with crystalline areas spanning less than a few nanometers in diameter, within a characteristic `pin-cushion'-like amorphous matrix. The difference in synthesis temperature affected the density of the needles on the schwertmannite surface. The needles on the higher-temperature schwertmannite displayed a dendritic morphology, whereas the needles on the room-temperature schwertmannite were more closely packed. Visible lattice fringes in the schwertmannite samples are consistent with the powder X-ray diffraction (XRD) pattern taken on the bulk schwertmannite and also matched d-spacings for goethite, indicating a close structural relationship between schwertmannite and goethite. The incomplete transformation from schwertmannite to goethite over 24 h at 75 °C was tracked using XRD and TEM. TEM images suggest that the sample collected after 24 h consists of aggregates of goethite nanocrystals. Comparing the synthetic schwertmannite in this study to a study on schwertmannite produced at 85 °C, which used ferric sulfate, reveals that synthesis conditions can result in significant differences in needle crystal structure. The bulk powder XRD patterns for the schwertmannite produced using these two samples were indistinguishable from one another. Future studies using synthetic schwertmannite should account for these differences when determining schwertmannite's structure, reactivity, and capacity to take up elements like arsenic. The schwertmannite synthesized by the Regenspurg et al. method produces a mineral that is consistent with the structure and morphology of natural schwertmannite observed in our previous study using XRD and TEM, making this an ideal synthetic method for laboratory-based mineralogical and geochemical studies that intend to be environmentally relevant.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

NASA Astrophysics Data System (ADS)

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. Electronic supplementary information (ESI) available: Fig. S1, AFM image (5 μm × 5 μm) of graphene nanoplate-MnO2 composite obtained at 3 h; Fig. S2, nitrogen adsorption/desorption isotherm of graphene nanoplate-MnO2 composite obtained at 3 h. See DOI: 10.1039/c1nr10229j

Preparation and Characterization of Guar-Montmorillonite Nanocomposites

PubMed Central

Mansa, Rola; Detellier, Christian

2013-01-01

Polymer-clay nanocomposites are highly sought-after materials, mainly due to their applicability in a variety of avenues. From the standpoint of the preparation of these nanocomposites, however, organic compatibility with clay and adherence to “green chemistry” concepts and principles can be limiting factors. As such, the objective was to prepare a biopolymer-modified clay nanocomposite using a simple and environmentally friendly method of preparation, whereby pre-treatment of the clay for organic compatibility was bypassed. Novel montmorillonite nanocomposites were prepared using neutral guar gum and cationic guar gum. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the formation of intercalated structures. A monolayer configuration of cationic guar within the interlayer space was indicated by XRD results, while treatment with neutral guar gum resulted in the observance of both monolayer and bilayer configurations. Additionally, TEM results indicated partial exfoliation. Results attributed from 13C cross polarization/magic angle spinning nuclear magnetic resonance spectroscopy (CP/MAS NMR) of the nanocomposites indicated peaks corresponding to the guar constituent, confirming the adsorption of the biopolymer. Inductively coupled plasma emission spectrometry (ICP-ES) results indicated the exchange of cations present in neutral guar gum with the sodium cations of montmorillonite, in the case of the neutral guar nanocomposites. PMID:28788384

Preparation and properties of calcium oxide from eggshells via calcination

NASA Astrophysics Data System (ADS)

Tangboriboon, N.; Kunanuruksapong, R.; Sirivat, A.

2012-12-01

Duck eggs are one of the most versatile cooking ingredients in which residue eggshells are discarded. Raw duck eggshells were calcined at temperatures between 300 to 900 °C, for 1, 3, and 5 h. Both the raw and calcined duck eggshells were characterized by FTIR, STA, XRD, XRF, TEM, BET, a particle size analyzer, and an impedance analyzer. The proper calcination conditions are: 900 °C and 1 h, yielding calcium oxide with a purity of 99.06 % w/w. The calcium carbonate of the rhombohedral form (CaCO3) transforms completely into the calcium oxide or lime of the face centered cubic form (CaO) at 900 °C, as shown by XRD diffraction patterns. The transmission electron microscopy (TEM) images of the calcium oxide reveal a moderately good dispersion of nearly uniform particles. The calcium oxide has a white color, a spherical shape, high porosity, and narrow particles size distribution. The percentage of ceramic yield of the calcium oxide is 53.53, as measured by STA (TG-DTA-DTG). The calcium oxide has a N2 adsorption-desorption isotherm indicating the meso-porosity range. The dielectric constant and the electrical conductivity of the calcined calcium oxide are 35 and 1:0×10-6(Ω·m)-1, respectively, at the frequency of 500 Hz.

Ti-Nb thin films deposited by magnetron sputtering on stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gonzalez, E. David; Niemeyer, Terlize C.; Afonso, Conrado R. M.

2016-03-15

Thin films of Ti-Nb alloys were deposited on AISI 316L stainless steel substrate by magnetron sputtering, and the structure, composition, morphology, and microstructure of the films were analyzed by means of x-ray diffraction (XRD), (scanning) transmission electron microscopy (TEM) coupled with energy-dispersive x-ray spectroscopy, atomic force microscopy (AFM), and x-ray photoelectron spectroscopy (XPS). Thin films of four compositions were produced: Ti{sub 85}Nb{sub 15} (Ti-26 wt. % Nb), Ti{sub 80}Nb{sub 20} (Ti-33 wt. % Nb), Ti{sub 70}Nb{sub 30} (Ti-45 wt. % Nb), and Ti{sub 60}Nb{sub 40} (Ti-56 wt. % Nb). Structural characterization by XRD indicated that only the β phase was present in the thinmore » films and that the increase in the Nb content modified the alloy film texture. These changes in the film texture, also detected by TEM analysis, were attributed to different growth modes related to the Nb content in the alloy films. The mean grain sizes measured by AFM increased with the Nb amount (from 197 to 222 nm). XPS analysis showed a predominance of oxidized Ti and Nb on the film surfaces and an enrichment of Ti.« less

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Sung Phil; Choi, Myong Yong, E-mail: mychoi@gnu.ac.kr; Choi, Hyun Chul, E-mail: chc12@chonnam.ac.kr

2016-02-15

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by usingmore » the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.« less

Carbon-encapsulated cobalt nanoparticles: synthesis, properties, and magnetic particle hyperthermia efficiency

NASA Astrophysics Data System (ADS)

Kotoulas, A.; Dendrinou-Samara, C.; Sarafidis, C.; Kehagias, Th.; Arvanitidis, J.; Vourlias, G.; Angelakeris, M.; Kalogirou, Orestis

2017-12-01

A facile and low-cost method for structuring carbon-encapsulated cobalt nanoparticles (Co@C) is presented. Three samples were solvothermally prepared in one step at 220 °C and one in two steps at 200 °C. Three different polyols such as propylene glycol, triethylene glycol, and tetraethylene glycol were used as carbon sources, solvents, and reducing agents. The samples were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Concerning the crystal structure of the particles, a mixture of hcp/ fcc Co phases was obtained in three of the samples, independently of the polyol used. The coexistence of cubic and hexagonal phases was revealed both from XRD and high-resolution TEM (HRTEM). The formation of the cubic fcc structure, despite the relatively low reaction temperature, is attributed to the role of the interface between carbon coating and metallic core. The presence of carbon coating was demonstrated by Raman spectrometry, exhibiting the characteristic D and G graphitic bands, and by HRTEM observations. All samples showed ferromagnetic behavior with saturation magnetization up to 158 emu/g and coercivity up to 206 Oe. From the magnetic particle hyperthermia measurements recorded at a frequency of 765 kHz, a maximum SLP value of 241 W/g was obtained.

Flux Growth of Highly Crystalline Photocatalytic BaTiO3 Particle Layers on Porous Titanium Sponge Substrate and Insights into the Formation Mechanism

NASA Astrophysics Data System (ADS)

Wang, Q.; Li, B.

2017-09-01

A unique architecture of idiomorphic and highly crystalline BaTiO3 particle layers directly grown on a porous titanium sponge substrate was successfully achieved for the first time using a facile molten salt method at a relatively low temperature of 700 °C. Specifically, the low-melting KCl-NaCl eutectic salts and barium hydroxide octahydrate were employed as the reaction medium and barium source, respectively. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and UV-vis diffuse reflectance spectrophotometry were used to characterize the structure, morphology and optical property of the obtained samples. The results revealed that the flux-grown tetragonal BaTiO3 products had well-defined and uniform morphology with an average size of 300 nm and a band gap of ∼3.16 eV. Based on XRD, EDS, SEM, and TEM, the possible formation mechanism responsible for the well-developed architecture of BaTiO3 particle layers was proposed and discussed. Furthermore, the photocatalytic activity of the flux-grown BaTiO3 products for organic pollutant degradation under simulated sunlight irradiation was also investigated.

Preparation of C60(O)n-ZnO nanocomposite under electric furnace and photocatalytic degradation of organic dyes.

PubMed

Cho, Bum Hwi; Oh, Youn Jun; Mun, Sang Mi; Ko, Weon Bae

2012-07-01

Zinc oxide (ZnO) nanoparticles were synthesized sonochemically by applying ultrasonic irradiation to a mixed aqueous-alcoholic solution of zinc nitrate with sodium hydroxide at room temperature. The morphology and optical properties of the ZnO nanoparticles were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-vis spectroscopy. The C60(O)n nanoparticles were synthesized by heating a mixture of C60 and 3-chloroperoxybenzoic acid in a benzene solvent under the reflux system. The heated C60(O)n-ZnO nanocomposite was synthesized in an electric furnace at 700 degrees C for two hours. The heated C60(O)n-ZnO nanocomposite was characterized by XRD, SEM, and TEM, and examined as a catalyst in the photocatalytic degradation of organic dyes by UV-vis spectroscopy. The photocatalytic effect of the heated C60(O)n-ZnO nanocomposite was evaluated by a comparison with that of unheated C60(O)n nanoparticles, heated C60(O)n nanoparticles, and unheated C60(O)n-ZnO in organic dyes, such as methylene blue (MB), methyl orange (MO), and rhodamine B (RhB) under ultraviolet light at 365 nm.

Green way genesis of silver nanoparticles using multiple fruit peels waste and its antimicrobial, anti-oxidant and anti-tumor cell line studies

NASA Astrophysics Data System (ADS)

Naganathan, Kiruthika; Thirunavukkarasu, Somanathan

2017-04-01

Green synthesis of silver nanoparticles (SNP) opens a new path to kill and prevent various infectious diseases and also tumor. In this study, we have synthesized silver nanoparticles using multiple fruit peel waste (pomegranate, orange, banana and apple (POBA)). The primarily nanoparticles formation has been confirmed by the color change. The synthesized SNP were analyzed by various physicochemical techniques such as UV- Visible spectroscopy, x-ray diffraction (XRD), fourier transform infra red (FT-IR) spectroscopy and transmission electron microscope (TEM). The formation of SNP was confirmed by its absorbance peak observed at 430 nm in UV-Visible spectrum. Further, the obtained SNP were identified by XRD and TEM, respectively to know the crystalline nature and size and shape of the particles. The activities of SNP were checked with human pathogens (Salmonella, E.coli and Pseudomonas), plant pathogen (Fusarium) and marine pathogen (Aeromonas hydrophila) and also studied the scavenging effect and anticancer properties against MCF-7 cell lines. This studies proves that the SNP prepared from fruit waste peel extract approach appears extremely fast, cost efficient, eco-friendly and alternative for conventional methods of SNP synthesis to promote the usage of these nanoparticles in medicinal application.

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

Piper nigrum Leaf and Stem Assisted Green Synthesis of Silver Nanoparticles and Evaluation of Its Antibacterial Activity Against Agricultural Plant Pathogens

PubMed Central

Paulkumar, Kanniah; Gnanajobitha, Gnanadhas; Vanaja, Mahendran; Rajeshkumar, Shanmugam; Malarkodi, Chelladurai; Pandian, Kannaiyan; Annadurai, Gurusamy

2014-01-01

Utilization of biological materials in synthesis of nanoparticles is one of the hottest topics in modern nanoscience and nanotechnology. In the present investigation, the silver nanoparticles were synthesized by using the leaf and stem extract of Piper nigrum. The synthesized nanoparticle was characterized by UV-vis spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), energy dispersive X-ray analysis (EDAX), and Fourier Transform Infrared Spectroscopy (FTIR). The observation of the peak at 460 nm in the UV-vis spectra for leaf- and stem-synthesized silver nanoparticles reveals the reduction of silver metal ions into silver nanoparticles. Further, XRD analysis has been carried out to confirm the crystalline nature of the synthesized silver nanoparticles. The TEM images show that the leaf- and stem-synthesized silver nanoparticles were within the size of about 7–50 nm and 9–30 nm, respectively. The FTIR analysis was performed to identify the possible functional groups involved in the synthesis of silver nanoparticles. Further, the antibacterial activity of the green-synthesized silver nanoparticles was examined against agricultural plant pathogens. The antibacterial property of silver nanoparticles is a beneficial application in the field of agricultural nanotechnology. PMID:24558336

Green synthesis and characterization of ANbO3 (A = Na, K) nanopowders fabricated using a biopolymer

NASA Astrophysics Data System (ADS)

Khorrami, Gh. H.; Mousavi, M.; Khayatian, S. A.; Kompany, A.; Khorsand Zak, A.

2017-10-01

Lead-free sodium niobate (NaNbO3, NN) and potassium niobate (KNbO3, KN) nanopowders were successfully synthesized by a simple and green synthesis process in gelatin media. Gelatin, which is a biopolymer, was used as stabilizer. In order to determine the lowest calcination temperature needed to obtain pure NN and KN nanopowders, the produced gels were analyzed by thermogravometric analyzer (TGA). The produced gels were calcined at 500∘C and 600∘C. The structural and optical properties of the prepared powders were examined using X-ray diffraction (XRD) technique, transmission electron microscopy (TEM), and UV-Vis spectroscopy. The XRD results revealed that pure phase NN and KN nanopowders were formed at low temperature calcination of 500∘C and 600∘C, respectively. The Scherrer formula and size-strain plot (SSP) method were employed to estimate crystallite size and lattice strain of the samples. The TEM images show that the NN and KN samples calcined at 600∘C have cubic shape with an average particle size of 60.95 and 39.29 nm, respectively. The optical bandgap energy of the samples was calculated using UV-Vis diffused reflectance spectra of the samples and Kubelka-Munck relation.

Fungus-mediated synthesis of gold nanoparticles and standardization of parameters for its biosynthesis.

PubMed

Tidke, Pritish R; Gupta, Indarchand; Gade, Aniket K; Rai, Mahendra

2014-12-01

We report the extracellular biosynthesis of gold nanoparticles (AuNPs) using a fungus Fusarium acuminatum. Mycosynthesis of Au-NPs was carried out by challenging the fungal cells filtrate with HAuCl 4 solution (1 mM), as nanoparticles synthesizing enzyme secrete extracellularly by the fungi. The AuNPs were characterized with the help of UV-Visible spectrophotometer, Fourier Transform Infrared spectroscopy, Zeta Potential, X-ray diffraction (XRD) and Transmission electron microscopy (TEM). We observed absorbance peak in between 520 nm-550 nm corresponding to the surface plasmon absorbance of the gold nanoparticles. The nanoparticles synthesized in the present investigation were found to be capped by proteins. XRD results showed that the distinctive formation of crystalline gold nanoparticles in the solution. The spherical and polydispersed AuNPs in the range 8 to 28 nm with average size of 17 nm were observed by TEM analysis. We also standardized the parameters like the effect of pH, temperature and salt concentration on the biosynthesis of gold nanoparticles. It was found that acidic pH, 1 mM salt concentration and 37 (°)C temperature were found to be optimum for the synthesis of Au-NPs. Therefore, the present study introduces the easy, better and cheaper method for biosynthesis of AuNPs.

Cellulase assisted synthesis of nano-silver and gold: Application as immobilization matrix for biocatalysis.

PubMed

Mishra, Abhijeet; Sardar, Meryam

2015-01-01

In the present study, we report in vitro synthesis of silver and gold nanoparticles (NPs) using cellulase enzyme in a single step reaction. Synthesized nanoparticles were characterized by UV-VIS spectroscopy, Dynamic Light Spectroscopy (DLS), Transmission Electron Microscopy (TEM), Energy-dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), Circular Dichroism (CD) and Fourier Transform Infrared Spectroscopy (FTIR). UV-visible studies shows absorption band at 415nm and 520nm for silver and gold NPs respectively due to surface plasmon resonance. Sizes of NPs as shown by TEM are 5-25nm for silver and 5-20nm for gold. XRD peaks confirmed about phase purity and crystallinity of silver and gold NPs. FTIR data shows presence of amide I peak on both the NPs. The cellulase assisted synthesized NPs were further exploited as immobilization matrix for cellulase enzyme. Thermal stability analysis reveals that the immobilized cellulase on synthesized NPs retained 77-80% activity as compared to free enzyme. While reusability data suggests immobilized cellulase can be efficiently used up to sixth cycles with minimum loss of enzyme activity. The secondary structural analysis of cellulase enzyme during the synthesis of NPs and also after immobilization of cellulase on these NPs was carried out by CD spectroscopy. Copyright © 2015 Elsevier B.V. All rights reserved.

Platinum nanocatalysts prepared with different surfactants for C1-C3 alcohol oxidations and their surface morphologies by AFM

NASA Astrophysics Data System (ADS)

Ertan, Salih; Şen, Fatih; Şen, Selda; Gökağaç, Gülsün

2012-06-01

In this study, platinum nanoparticle catalysts have been prepared using PtCl4 as a starting material and 1-octanethiol, 1-decanethiol, 1-dodecanethiol, and 1-hexadecanethiol as surfactants for methanol, ethanol, and 2-propanol oxidation reactions. The structure, particle sizes, and surface morphologies of the catalysts were characterized by X-ray diffraction (XRD), atomic force microscopy and transmission electron microscopy (TEM). XRD and TEM results indicate that all prepared catalysts have a face-centered cubic structure and are homogeneously dispersed on the carbon support with a narrow size distribution (2.0-1.3 nm). X-ray photoelectron spectra of the catalysts were examined and it is found that platinum has two different oxidation states, Pt (0) and Pt(IV), oxygen and sulfur compounds are H2Oads and OHads, bound and unbound thiols. The electrochemical and electrocatalytic properties of these catalysts were investigated with respect to C1-C3 alcohol oxidations by cyclic voltammetry and chronoamperometry. The highest electrocatalytic activity was obtained from catalyst I which was prepared with 1-octanethiol. This may be attributed to a decrease in the ratio of bound to unbound thiol species increase in Pt (0)/Pt(IV), H2Oads/OHads ratios, electrochemical surface area, CO tolerance and percent platinum utility.

PdRu/C catalysts for ethanol oxidation in anion-exchange membrane direct ethanol fuel cells

NASA Astrophysics Data System (ADS)

Ma, Liang; He, Hui; Hsu, Andrew; Chen, Rongrong

2013-11-01

Carbon supported PdRu catalysts with various Pd:Ru atomic ratios were synthesized by impregnation method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), electrochemical half-cell tests, and the anion-exchange membrane direct ethanol fuel cell (AEM-DEFC) tests. XRD results suggest that the PdRu metal exists on carbon support in an alloy form. TEM study shows that the bimetallic PdRu/C catalysts have slightly smaller average particle size than the single metal Pd/C catalyst. Lower onset potential and peak potential and much higher steady state current for ethanol oxidation in alkaline media were observed on the bimetallic catalysts (PdxRuy/C) than on the Pd/C, while the activity for ethanol oxidation on the pure Ru/C was not noticeable. By using Pd/C anode catalysts and MnO2 cathode catalysts, AEM-DEFCs free from the expensive Pt catalyst were assembled. The AEM DEFC using the bimetallic Pd3Ru/C anode catalyst showed a peak power density as high as 176 mW cm-2 at 80 °C, about 1.8 times higher than that using the single metal Pd/C catalyst. The role of Ru for enhancing the EOR activity of Pd/C catalysts is discussed.

Preparation and Characterization of Polyhydroxybutyrate/Polycaprolactone Nanocomposites

PubMed Central

Liau, Cha Ping; Bin Ahmad, Mansor; Shameli, Kamyar; Yunus, Wan Md Zin Wan

2014-01-01

Polyhydroxybutyrate (PHB)/polycaprolactone (PCL)/stearate Mg-Al layered double hydroxide (LDH) nanocomposites were prepared via solution casting intercalation method. Coprecipitation method was used to prepare the anionic clay Mg-Al LDH from nitrate salt solution. Modification of nitrate anions by stearate anions between the LDH layers via ion exchange reaction. FTIR spectra showed the presence of carboxylic acid (COOH) group which indicates that stearate anions were successfully intercalated into the Mg-Al LDH. The formation of nanocomposites only involves physical interaction as there are no new functional groups or new bonding formed. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the mixtures of nanocomposites are intercalated and exfoliated types. XRD results showed increasing of basal spacing from 8.66 to 32.97 Å in modified stearate Mg-Al LDH, and TEM results revealed that the stearate Mg-Al LDH layers are homogeneously distributed in the PHB/PCL polymer blends matrix. Enhancement in 300% elongation at break and 66% tensile strength in the presence of 1.0 wt % of the stearate Mg-Al LDH as compare with PHB/PCL blends. Scanning electron microscopy (SEM) proved that clay improves compatibility between polymer matrix and the best ratio 80PHB/20PCL/1stearate Mg-Al LDH surface is well dispersed and stretched before it breaks. PMID:24600329

Steam-assisted crystallization of TPA{sup +}-exchanged MCM-41 type mesoporous materials with thick pore walls

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Hong Li; Zhang, Kun; Wang, Yi Meng, E-mail: ymwang@chem.ecnu.edu.cn

2012-07-15

Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, {sup 1}H–{sup 13}C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show thatmore » the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.« less

Isolation and characterization of nanocrystalline cellulose from roselle-derived microcrystalline cellulose.

PubMed

Kian, Lau Kia; Jawaid, Mohammad; Ariffin, Hidayah; Karim, Zoheb

2018-07-15

Roselle fiber is a renewable and sustainable agricultural waste enriched with cellulose polysaccharides. The isolation of Nanocrystalline cellulose (NCC) from roselle-derived microcrystalline cellulose (MCC) is an alternative approach to recover the agricultural roselle plant residue. In the present study, acid hydrolysis with different reaction time was carried out to degrade the roselle-derived MCC to form NCC. The characterizations of isolated NCC were conducted through Fourier Transform Infrared Ray (FTIR), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), Energy Dispersive Spectroscopy (EDS), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). As evaluated from the performed morphological investigations, the needle-like shape NCC nanostructures were observed under TEM and AFM microscopy studies, while irregular rod-like shape of NCC was observed under FESEM analysis. With 60min hydrolysis time, XRD analysis demonstrated the highest NCC crystallinity degree with 79.5%. In thermal analysis by TGA and DSC, the shorter hydrolysis time tended to produce NCC with higher thermal stability. Thus, the isolated NCC from roselle-derived MCC has high potential to be used in application of pharmaceutical and biomedical fields for nanocomposite fabrication. Copyright © 2018 Elsevier B.V. All rights reserved.

Green Synthesis of Zinc Oxide Nanoparticles for Enhanced Adsorption of Lead Ions from Aqueous Solutions: Equilibrium, Kinetic and Thermodynamic Studies.

PubMed

Azizi, Susan; Mahdavi Shahri, Mahnaz; Mohamad, Rosfarizan

2017-06-08

In the present study, ZnO nanoparticles (NPs) were synthesized in zerumbone solution by a green approach and appraised for their ability to absorb Pb(II) ions from aqueous solution. The formation of as-synthesized NPs was established by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), and UV-visible studies. The XRD and TEM analyses revealed high purity and wurtzite hexagonal structure of ZnO NPs with a mean size of 10.01 ± 2.6 nm. Batch experiments were performed to investigate the impact of process parameters viz. Pb(II) concentration, pH of solution, adsorbent mass, solution temperature, and contact time variations on the removal efficiency of Pb(II). The adsorption isotherm data provided that the adsorption process was mainly monolayer on ZnO NPs. The adsorption process follows pseudo-second-order reaction kinetic. The maximum removal efficiencies were 93% at pH 5. Thermodynamic parameters such as enthalpy change (ΔH⁰), free energy change (ΔG⁰), and entropy change (ΔS⁰) were calculated; the adsorption process was spontaneous and endothermic. The good efficiency of the as-synthesized NPs makes them attractive for applications in water treatment, for removal of heavy metals from aqueous system.

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

Structure and properties of electrodeposited nanocrystalline Ni and Ni-Fe alloy continuous foils

NASA Astrophysics Data System (ADS)

Giallonardo, Jason Derek

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or "growth faults", which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young's modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young's modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in intercrystal defects or interfaces in the solid.

Physicochemical characterizations of nano-palm oil fuel ash

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rajak, Mohd Azrul Abdul, E-mail: azrulrajak88@gmail.com; Preparatory Centre of Science and Technology, Universiti Malaysia Sabah, Jalan UMS, 88400, Kota Kinabalu, Sabah; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my

2015-07-22

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM)more » and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m{sup 2}/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.« less

Nanocrystalline p-hydroxyacetanilide (paracetamol) and gold core-shell structure as a model drug deliverable organic-inorganic hybrid nanostructure

NASA Astrophysics Data System (ADS)

Das, Subhojit; Paul, Anumita; Chattopadhyay, Arun

2013-09-01

We report on the generation of core-shell nanoparticles (NPs) having an organic nanocrystal (NC) core coated with an inorganic metallic shell, being dispersed in aqueous medium. First, NCs of p-hydroxyacetanilide (pHA)--known also as paracetamol--were generated in an aqueous medium. Transmission electron microscopy (TEM) and powder X-ray diffraction (XRD) evidenced the formation of pHA NCs and of their crystalline nature. The NCs were then coated with Au to form pHA@Au core-shell NPs, where the thickness of the Au shell was on the order of nanometers. The formation of Au nanoshell--surrounding pHA NC--was confirmed from its surface plasmon resonance (SPR) band in the UV/Vis spectrum and by TEM measurements. Further, on treatment of the core-shell particles with a solution comprising NaCl and HCl (pH < 3), the Au shell could be dissolved, subsequently releasing pHA molecules. The dissolution of Au shell was marked by a gradual diminishing of its SPR band, while the release of pHA molecules in the solution was confirmed from TEM and FTIR studies. The findings suggest that the core-shell NP could be hypothesized to be a model for encapsulating drug molecules, in their crystalline forms, for slow as well as targeted release.We report on the generation of core-shell nanoparticles (NPs) having an organic nanocrystal (NC) core coated with an inorganic metallic shell, being dispersed in aqueous medium. First, NCs of p-hydroxyacetanilide (pHA)--known also as paracetamol--were generated in an aqueous medium. Transmission electron microscopy (TEM) and powder X-ray diffraction (XRD) evidenced the formation of pHA NCs and of their crystalline nature. The NCs were then coated with Au to form pHA@Au core-shell NPs, where the thickness of the Au shell was on the order of nanometers. The formation of Au nanoshell--surrounding pHA NC--was confirmed from its surface plasmon resonance (SPR) band in the UV/Vis spectrum and by TEM measurements. Further, on treatment of the core-shell particles with a solution comprising NaCl and HCl (pH < 3), the Au shell could be dissolved, subsequently releasing pHA molecules. The dissolution of Au shell was marked by a gradual diminishing of its SPR band, while the release of pHA molecules in the solution was confirmed from TEM and FTIR studies. The findings suggest that the core-shell NP could be hypothesized to be a model for encapsulating drug molecules, in their crystalline forms, for slow as well as targeted release. Electronic supplementary information (ESI) available: See DOI: 10.1039/c3nr03566b

Synthesis of gold nanoparticles using silk fibroin and their characterization

NASA Astrophysics Data System (ADS)

Gowda, Mahadeva; Harisha, K. S.; Ranjana, T.; Harish, K. V.; Narayana, B.; Byrappa, K.; Sangappa, Y.

2018-05-01

The synthesis of metal nanoparticales by environmentally friendly processes is an important aspect of nanotechnology today. One such approach that shows immense potential is based on the in situ synthesis of gold nanoparticles (AuNPs) using naturally available materials such as aqueous silk fibroin (SF) obtained from Bombyx mori silk. The UV-visible absorption study revealed the formation of AuNPs by showing characteristic surface plasmon resonance (SPR) band at 525 nm. The X-ray diffraction (XRD) analysis study suggests the synthesized gold nanoparticles are FCC crystal structure. The transmission electron microscopy (TEM) images showed that the formed AuNPs are spherical in shape with smooth edges.

Monetite formed in mixed solvents of water and ethylene glycol and its transformation to hydroxyapatite.

PubMed

Ma, Ming-Guo; Zhu, Ying-Jie; Chang, Jiang

2006-07-27

Agglomerated nanorods of hydroxyapatite have been synthesized using monetite as a precursor in a NaOH solution. Monetite consisting of nanosheets has been successfully synthesized by a one-step microwave-assisted method using CaCl(2).2.5H(2)O, NaH(2)PO(4), and sodium dodecyl sulfate (SDS) in water/ethylene glycol (EG) mixed solvents. The effects of the molar ratio of water to EG and the reaction time on the products were investigated. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectrometry (FTIR).

Structure comparison of PMN-PT and PMN-PZT nanocrystals prepared by gel-combustion method at optimized temperatures

NASA Astrophysics Data System (ADS)

Ghasemifard, M.; Hosseini, S. M.; Bagheri-Mohagheghi, M. M.; Shahtahmasbi, N.

2009-09-01

We have synthesized and were performed a comparison of structures and optical properties between relaxor ferroelectric PMN-PT and PMN-PZT nanopowders. A gel-combustion method has been used to synthesize PMN-PT and PMN-PZT nanocrystalline with the perovskite structure. The precursors employed in the gel-combustion process were lead nitrate, magnesium acetate, niobium ammonium oxalate and zirconium nitrate. The nanopowders were characterized using the X-ray diffraction (XRD) and transmission electron microscopy (TEM) observation. Fourier transform infrared (FTIR) spectroscopy was employed to monitor the transformation of precursor solutions during the thermal reactions leading to the formation of perovskite phase.

Polyol-mediated thermolysis process for the synthesis of MgO nanoparticles and nanowires

NASA Astrophysics Data System (ADS)

Subramania, A.; Vijaya Kumar, G.; Sathiya Priya, A. R.; Vasudevan, T.

2007-06-01

The main aim of this work is to prepare MgO nanoparticles and nanowires by a novel polyol-mediated thermolysis (PMT) process. The influence of different mole concentration of magnesium acetate, polyvinyl pyrrolidone (PVP; capping agent) and ethylene glycol (EG; solvent as well as reducing agent) on the formation of nanoparticles and nanowires and the effect of calcination on the crystalline size of the samples were also examined. The resultant oxide structure, thermal behaviour, size and shape have been studied using x-ray diffraction (XRD) studies, thermal (TG/DTA) analysis and scanning electron microscopy (SEM)/transmission electron microscopy (TEM) respectively.

Influence of Ag substitution on structural and dielectric properties of TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ahmed, Ateeq; Siddique, M. Naseem; Aftab, Tabish; Tripathi, P.

2018-04-01

In this paper, we report the structural, electrical and dielectric properties of Ag-substituted TiO2 nanoparticles synthesized by sol-gel method. The X-ray diffraction (XRD) spectra revealed that the synthesized nanoparticles are pure and crystalline in nature and showing tetragonal anatase phase of TiO2. TEM micrograph shows that shapes of the nanoparticles are non-spherical. We have also studied the dielectric properties and in relation to it the dielectric constants, dielectric loss and A.C. conductivity have been studied as the function of frequency and composition of iron. The above theory may be explained by `Maxwell Wagner Model'.

Synthesis and characterization of magnetic semiconducting Cu{sub 2}CoSnS{sub 4} nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gupta, Aman; Mokurala, Krishnaiah; Kamble, Anvita

2015-06-24

Multifunctional wurtzite Cu{sub 2}CoSnS{sub 4} (CCoTS) nanoparticles were successfully synthesized by facile hot-injection method using elemental sulfur as sulfur source. As-synthesized CCoTS nanoparticles were characterized using X-ray diffraction (XRD) for phase identification. Morphology of as-prepared nanoparticles was examined using FEG-SEM and FEG-TEM. Resistivity of film was measured using four probe method and it’s value (0.8 Ωcm) lies in the range of semiconductors. Magnetization curve of Cu{sub 2}CoSnS{sub 4} nanoparticles (at room temperature) indicates weak ferromagnetic behavior.

Enhancement of durability of NIR emission of Ag2S@ZnS QDs in water

NASA Astrophysics Data System (ADS)

Karimipour, M.; Bagheri, M.; Molaei, M.

2017-11-01

Stability of Ag2S@ZnS QDs in water is a crucial concern for their application in biology. In this work, both physical sustainability and emission stability of Ag2S QDs were enhanced using parameter optimization of a pulsed microwave irradiation (MI) method up to 105 days after their preparation. UV-Vis and photoluminescence spectroscopies depicted an absorption and emission about 817 nm and 878 nm, respectively. X-ray diffraction (XRD) analysis showed a growth of Ag2S acanthite phase. Transmission Electron Microscopy (TEM) images revealed a clear formation of Ag2S@ZnS core-shell structure.

Frabicating hydroxyapatite nanorods using a biomacromolecule template

NASA Astrophysics Data System (ADS)

Zhu, Aiping; Lu, Yan; Si, Yunfeng; Dai, Sheng

2011-02-01

Rod-like hydroxyapatite (HAp) nanoparticles with various aspect ratios are synthesized by means of low-temperature hydrothermal method in the presence of a N-[(2-hydroxy-3-trimethylammonium) propyl]chitosan chloride (HTCC) template. The synthesized HAps were examined by X-ray diffraction (XRD), Fourier transform infrared spectrophotometer (FTIR) and transmission electron microscopy (TEM) techniques. The results reveal that HAps are rod-like monocrystals, where the size and morphology can be tailored by varying synthesis conditions, such as pH, hydrothermal synthesis temperature and the ratio of PO43- to the quaternary ammonium in HTCC. The mechanism of HTCC template on HAp nanorod preparation is analyzed.

Study on industrial wastewater treatment using superconducting magnetic separation

NASA Astrophysics Data System (ADS)

Zhang, Hao; Zhao, Zhengquan; Xu, Xiangdong; Li, Laifeng

2011-06-01

The mechanism of industrial wastewater treatment using superconducting magnetic separation is investigated. Fe 3O 4 nanoparticles were prepared by liquid precipitation and characterized by X-ray diffraction (XRD). Polyacrylic acid (PAA) film was coated on the magnetic particles using plasma coating technique. Transmission electron microscope (TEM) observation and infrared spectrum measurement indicate that the particle surface is well coated with PAA, and the film thickness is around 1 nm. Practical paper factory wastewater treatment using the modified magnetic seeds in a superconducting magnet (SCM) was carried out. The results show that the maximum removal rate of chemical oxygen demand (COD) by SCM method can reach 76%.

New polyurethane nanocomposites based on soya oil.

PubMed

Mohammed, Issam Ahmed; Abd Khadir, Nurul Khizrien; Jaffar Al-Mulla, Emad Abbas

2014-01-01

New polyurethane (PU) nanocomposites were prepared from a dispersion of 0 - 5% montmorillonite (MMT) clay with isocyanate and soya oil polyol that was synthesized via transesterification of triglycerides to reduce petroleum dependence. FT-IR spectra indicate the presence of hydrogen bonding between nanoclay and the polymer matrix, whereas the exfoliated structure of clay layers was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Optical microscopy, mechanical and thermal analyses were done to investigate significant improvement of the nanocomposites. The results showed PU-3% nanoclay (NC) showed optimum results in mechanical properties such as tensile and flexural strength but the lowest in impact strength.

Effect of deep cryogenic treatment on the formation of nano-sized carbides and the wear behavior of D2 tool steel

NASA Astrophysics Data System (ADS)

Amini, Kamran; Akhbarizadeh, Amin; Javadpour, Sirus

2012-09-01

The effect of deep cryogenic treatment on the microstructure, hardness, and wear behavior of D2 tool steel was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), hardness test, pin-on-disk wear test, and the reciprocating pin-on-flat wear test. The results show that deep cryogenic treatment eliminates retained austenite, makes a better carbide distribution, and increases the carbide content. Furthermore, some new nano-sized carbides form during the deep cryogenic treatment, thereby increasing the hardness and improving the wear behavior of the samples.

Formation of crystalline Zn-Al layered double hydroxide precipitates on γ-alumina: the role of mineral dissolution.

PubMed

Li, Wei; Livi, Kenneth J T; Xu, Wenqian; Siebecker, Matthew G; Wang, Yujun; Phillips, Brian L; Sparks, Donald L

2012-11-06

To better understand the sequestration of toxic metals such as nickel (Ni), zinc (Zn), and cobalt (Co) as layered double hydroxide (LDH) phases in soils, we systematically examined the presence of Al and the role of mineral dissolution during Zn sorption/precipitation on γ-Al(2)O(3) (γ-alumina) at pH 7.5 using extended X-ray absorption fine structure spectroscopy (EXAFS), high-resolution transmission electron microscopy (HR-TEM), synchrotron-radiation powder X-ray diffraction (SR-XRD), and (27)Al solid-state NMR. The EXAFS analysis indicates the formation of Zn-Al LDH precipitates at Zn concentration ≥0.4 mM, and both HR-TEM and SR-XRD reveal that these precipitates are crystalline. These precipitates yield a small shoulder at δ(Al-27) = +12.5 ppm in the (27)Al solid-state NMR spectra, consistent with the mixed octahedral Al/Zn chemical environment in typical Zn-Al LDHs. The NMR analysis provides direct evidence for the existence of Al in the precipitates and the migration from the dissolution of γ-alumina substrate. To further address this issue, we compared the Zn sorption mechanism on a series of Al (hydr)oxides with similar chemical composition but differing dissolubility using EXAFS and TEM. These results suggest that, under the same experimental conditions, Zn-Al LDH precipitates formed on γ-alumina and corundum but not on less soluble minerals such as bayerite, boehmite, and gibbsite, which point outs that substrate mineral surface dissolution plays an important role in the formation of Zn-Al LDH precipitates.

Evaluation of poly (vinyl alcohol) based cryogel-zinc oxide nanocomposites for possible applications as wound dressing materials.

PubMed

Chaturvedi, Archana; Bajpai, Anil K; Bajpai, Jaya; K Singh, Sunil

2016-08-01

In this investigation cryogels composed of poly (vinyl alcohol) (PVA) were prepared by repeated freeze thaw method followed by in situ precipitation of zinc oxide nanoparticles within the cryogel networks. Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX) were used to characterize the nanocomposites. The morphologies of native PVA cryogels and PVA cryogel-ZnO nanocomposites were observed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well-defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated zinc oxide nanoparticles with diameter<100nm. XRD results showed all relevant Bragg's reflections for crystal structure of zinc oxide nanoparticles. Thermo gravimetric-differential thermal analysis (TG-DTA) was conducted to evaluate thermal stability of the nanocomposites. Mechanical properties of nanocomposites were determined in terms of tensile strength and percent elongation. Biocompatible nature was ascertained by anti-haemolytic activity, bovine serum albumin (blood protein) adsorption and in vitro cytotoxicity tests. The prepared nanocomposites were also investigated for swelling and deswelling behaviours. The results revealed that both the swelling and deswelling process depend on the chemical composition of the nanocomposites, number of freeze-thaw cycles, pH and temperature of the swelling medium. The developed biocompatible PVA cryogel-ZnO nanocomposites were also tested for antibacterial activities against both Gram-negative and Gram-positive bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

Thermal annealing dynamics of carbon-coated LiFePO{sub 4} nanoparticles studied by in-situ analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krumeich, Frank, E-mail: krumeich@inorg.chem.ethz.ch; Waser, Oliver; Pratsinis, Sotiris E.

The thermal behavior of core-shell carbon-coated lithium iron phosphate (LiFePO{sub 4}-C) nanoparticles made by flame spray pyrolysis (FSP) during annealing was investigated by in-situ transmission electron microscopy (TEM), in-situ X-ray powder diffraction (XRD) as well as ex-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Crystallization of the initially glassy LiFePO{sub 4}-C nanoparticles starts at quite low temperatures (T=400 °C), forming single crystals inside the confinement of the carbon shell. Upon increasing the temperature to T≥700 °C, LiFePO{sub 4} starts to diffuse through the carbon shell resulting in cavities inside the mostly intact carbon shell. By increasing the temperature further tomore » T≥800 °C, the initial core-shell morphology converts into open carbon shells (flakes and cenospheres) and bulky LiFePO{sub 4} particles (diameter in the range 300–400 nm), in agreement with ex-situ experiments. - Graphical abstract: TEM images of a typical sample area recorded at room temperature and after heating in-situ heating reveal the growth of particles and the formation of empty carbon cages. - Highlights: • LiFePO{sub 4} coated by a carbon shell is produced by flame spray pyrolysis. • The amorphous LiFePO{sub 4} starts to crystallize at 400 °C as revealed by in-situ XRD. • Crystal growth was visualized by TEM heating experiments. • The formation of empty carbon cages starts at 700 °C.« less

Using nuclear magnetic resonance and transient electromagnetics to characterise water distribution beneath an ice covered volcanic crater: the case of Sherman Crater Mt. Baker Washington.

USGS Publications Warehouse

Irons, Trevor P.; Martin, Kathryn; Finn, Carol A.; Bloss, Benjamin; Horton, Robert J.

2014-01-01

Surface and laboratory Nuclear Magnetic Resonance (NMR) measurements combined with transient electromagnetic (TEM) data are powerful tools for subsurface water detection. Surface NMR (sNMR) and TEM soundings, laboratory NMR, complex resistivity, and X-Ray Diffraction (XRD) analysis were all conducted to characterise the distribution of water within Sherman Crater on Mt. Baker, WA. Clay rich rocks, particularly if water saturated, can weaken volcanoes, thereby increasing the potential for catastrophic sector collapses that can lead to far-travelled, destructive debris flows. Detecting the presence and volume of shallow groundwater is critical for evaluating these landslide hazards. The TEM data identified a low resistivity layer (<10 ohm-m), under 60 m of glacial ice related to water saturated clays. The TEM struggles to resolve the presence or absence of a plausible thin layer of bulk liquid water on top of the clay. The sNMR measurements did not produce any observable signal, indicating the lack of substantial accumulated bulk water below the ice. Laboratory analysis on a sample from the crater wall that likely represented the clays beneath the ice confirmed that the controlling factor for the lack of sNMR signal was the fine-grained nature of the media. The laboratory measurements further indicated that small pores in clays detected by the XRD contain as much as 50% water, establishing an upper bound on the water content in the clay layer. Forward modelling of geologic scenarios revealed that bulk water layers as thin as ½ m between the ice and clay layer would have been detectable using sNMR. The instrumentation conditions which would allow for sNMR detection of the clay layer are investigated. Using current instrumentation the combined analysis of the TEM and sNMR data allow for valuable characterisation of the groundwater system in the crater. The sNMR is able to reduce the uncertainty of the TEM in regards to the presence of a bulk water layer, a valuable piece of information in hazard assessment.

Pronounced pre-martensitic anomaly in the magnetization on Ni2MnGa thin films

NASA Astrophysics Data System (ADS)

Neckel, I. T.; Müller, C.; Nobrega, K. Z.; Dartora, C. A.; Schreiner, W. H.; Mosca, D. H.

2018-05-01

We have prepared [110]-textured Ni2MnGa thin films exhibiting an unusual pre-martensitic transition accompanied by an extremely large magnetization change. The thin films were grown by molecular beam epitaxy directly on epi-ready GaAs(111)B. Crystalline structure was investigated in situ by reflection high-energy electron diffraction (RHEED) and ex situ by x-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the film exhibits cubic crystalline structure (L2 1) at room temperature with lattice parameter a = 5.88 Å which undergoes martensitic transition. Magnetic characterization shows ferromagnetic behavior at room temperature with Curie temperature higher than room temperature. Martensitic transformation occurs at TM ∼ 185 K. A phenomenological model based on Landau theory of phase transformation was developed to explain the anomalous pre-martensitic transition at ∼285 K.

Synthesis, Characterization and Antibacterial Activity of BiVO4 Microstructure

NASA Astrophysics Data System (ADS)

Ekthammathat, Nuengruethai; Phuruangrat, Anukorn; Thongtem, Somchai; Thongtem, Titipun

2018-05-01

Hyperbranched BiVO4 microstructure were successfully synthesized by a hydrothermal method. Upon characterization the products by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, selected area electron diffraction (SAED) and photoluminescence (PL) spectroscopy, pure monoclinic hyperbranched BiVO4 with dominant vibration peak at 810 cm-1 and strong photoemission peak at 360 nm was synthesized in the solution with pH 1. In the solution with pH 2, tetragonal BiVO4 phase was also detected. In this research, antibacterial activity against S. aureus and E. coli was investigated by counting the colony forming unit (CFU). At 37°C within 24 h, the monoclinic BiVO4 phase can play the role in inhibiting S. aureus growth (350 CFU/mL remaining bacteria) better than that against E. coli (a large number of remaining bacteria).

Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

Visible-light-assisted SLCs template synthesis of sea anemone-like Pd/PANI nanocomposites with high electrocatalytic activity for methane oxidation in acidic medium

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

Sea anemone-like palladium (Pd)/polyaniline (PANI) nanocomposites were synthesized via visible-light-assisted swollen liquid crystals (SLCs) template method. The resulting samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV–vis) absorption spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, respectively. The electrocatalytic properties of Pd/PANI nanocomposites modified glass carbon electrode (GCE) for methane oxidation were investigated by cycle voltammetry (CV) and chronoamperometry. Those dispersed sea anemone-like Pd/PANI nanocomposites had an average diameter of 320 nm. The obtained Pd nanoparticles with an average diameter of about 45 nm were uniformly distributed in PANI matrix. Sea anemone-like Pd/PANI nanocomposites exhibited excellent electrocatalytic activity and stability for oxidation of methane (CH4).

New frontiers in water purification: highly stable amphopolycarboxyglycinate-stabilized Ag-AgCl nanocomposite and its newly discovered potential

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Zherebin, Pavel M.; Kudrinskiy, Alexey A.; Zubavichus, Yan V.; Presniakov, Mikhail Yu; Yapryntsev, Alexey D.; Karabtseva, Anastasia V.; Mikhaylov, Dmitry M.; Lisichkin, Georgii V.

2016-09-01

A simple synthetic procedure for high-stable dispersions of porous composite Ag/AgCl nanoparticles stabilized with amphoteric surfactant sodium tallow amphopolycarboxyglycinate has been proposed for the first time. The prepared samples were characterized by UV-vis spectroscopy, x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy, small area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electron probe micro-analysis. In addition, measurements (carried out at the Kurchatov synchrotron radiation source stations) of the Ag K-edge extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) spectra and XRD of the prepared nanoparticles have been performed. The obtained results suggest that small-sized Ag clusters are homogeneously distributed in the mass of the AgCl nanoparticle (~80 nm) formed during the synthesis. The Ag/AgCl dispersion demonstrates photocatalytic activity (with respect to methyl orange) and high bactericidal activity against E. coli. This activity is superior to the activity of both Ag and AgCl nanoparticles stabilized by the same surfactant. Thus, porous composite Ag/AgCl nanoparticles can be used as a multifunctional agent that is able to remove both pollutants and bacterium from water.

Synthesis and structure of a stuffed derivative of α-quartz, Mg 0.5AlSiO 4

DOE PAGES

Xu, Hongwu; Heaney, Peter J.; Yu, Ping; ...

2015-10-01

A structural derivative of quartz with the composition Mg 0.5AlSiO 4 has been grown from glass and characterized using synchrotron X-ray diffraction (XRD), transmission electron microscopy (TEM), and 29Si nuclear magnetic resonance (NMR) spectroscopy. Rietveld analysis of the XRD data indicates that the framework of Mg 0.5AlSiO 4 is isostructural with α-quartz, rather than β-quartz, as is consistent with previous theoretical modeling (Sternitzke and Müller 1991). Al and Si exhibit long-range disorder over the framework tetrahedral sites, indicated by the absence of the superlattice reflections corresponding to the doubling of c relative to that of quartz. Nevertheless, 29Si NMR measurementsmore » show that Al and Si exhibit partial short-range order with an ordering degree of 56%. Electron diffraction reveals superlattice reflections indicative of doubled periodicities along the a-axes. In conclusion, Fourier electron density maps show that Mg occupies channel sites that each are bonded to six O atoms, in contrast to the tetrahedral coordination of Li in the β-quartz-type framework for β-eucryptite, LiAlSiO 4. Furthermore, the concentrations of Mg in adjacent channels are different, resulting in framework distortions that generate the superstructures along a.« less

Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less

ZnS, CdS and HgS nanoparticles via alkyl-phenyl dithiocarbamate complexes as single source precursors.

PubMed

Onwudiwe, Damian C; Ajibade, Peter A

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively.

ZnS, CdS and HgS Nanoparticles via Alkyl-Phenyl Dithiocarbamate Complexes as Single Source Precursors

PubMed Central

Onwudiwe, Damian C.; Ajibade, Peter A.

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively. PMID:22016607

A novel green synthesis of Fe3O4-Ag core shell recyclable nanoparticles using Vitis vinifera stem extract and its enhanced antibacterial performance

NASA Astrophysics Data System (ADS)

Venkateswarlu, Sada; Natesh Kumar, B.; Prathima, B.; Anitha, K.; Jyothi, N. V. V.

2015-01-01

We described a novel and eco-friendly method for preparing Fe3O4-Ag core shell nanoparticles (CSNPs) with high magnetism and potent antibacterial activity. The Fe3O4-Ag CSNPs were obtained using waste material of Vitis vinifera (grape) stem extract as the green solvent, reducing and capping agent. The result recorded from X-ray powder diffraction (XRD), UV-vis spectrum, energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) supports the biosynthesis and characterization of Fe3O4-Ag CSNPs. From transmission electron microscopy (TEM) the size of the Fe3O4-Ag nanoparticles was measured below 50 nm; high-resolution TEM (HRTEM) indicates the core shell structure; and selected area electron diffraction (SAED) has revealed polycrystalline nature. Vibrating sample magnetometer (VSM) shows the ferromagnetic nature of Fe3O4-Ag CSNPs at room temperature with saturation magnetization of 15.74 emu/g. Further, these biogenic nanoparticles were highly hazardous to microorganisms. The antibacterial activity of biogenic Fe3O4-Ag CSNPs showed potent inhibitory activity against both Gram-positive and Gram-negative pathogens. These nanoparticles may also be reusable because of its excellent ferromagnetic property.

Growth of high quality AlN films on CVD diamond by RF reactive magnetron sputtering

NASA Astrophysics Data System (ADS)

Chen, Liang-xian; Liu, Hao; Liu, Sheng; Li, Cheng-ming; Wang, Yi-chao; An, Kang; Hua, Chen-yi; Liu, Jin-long; Wei, Jun-jun; Hei, Li-fu; Lv, Fan-xiu

2018-02-01

A highly oriented AlN layer has been successfully grown along the c-axis on a polycrystalline chemical vapor deposited (CVD) diamond by RF reactive magnetron sputtering. Structural, morphological and mechanical properties of the heterostructure were investigated by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Transmission Electron Microscopy (TEM), X-ray diffraction (XRD), Nano-indentation and Four-probe meter. A compact AlN film was demonstrated on the diamond layer, showing columnar grains and a low surface roughness of 1.4 nm. TEM results revealed a sharp AlN/diamond interface, which was characterized by the presence of a distinct 10 nm thick buffer layer resulting from the initial AlN growth stage. The FWHM of AlN (002) diffraction peak and its rocking curve are as low as 0.41° and 3.35° respectively, indicating a highly preferred orientation along the c-axis. AlN sputtered films deposited on glass substrates show a higher bulk resistivity (up to 3 × 1012 Ω cm), compared to AlN films deposited on diamond (∼1010 Ω cm). Finally, the film hardness and Young's modulus of AlN films on diamond are 25.8 GPa and 489.5 GPa, respectively.

Influence of nickel substitution on crystal structure and magnetic properties of strontium ferrite preparation via sol-gel auto-combustion route

NASA Astrophysics Data System (ADS)

Roohani, Ebrahim; Arabi, Hadi; Sarhaddi, Reza

2018-01-01

In this research, SrFe12-xNixO19 (x = 0 - 1) hexagonal ferrites were prepared by sol-gel auto-combustion method. Effect of Ni substitution on structural, morphological and magnetic properties of nanoparticles was investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM), respectively. The XRD results confirmed that all samples with x ≤ 0.5 have single phase M-type strontium ferrite structure, whereas for the SrFe12-xNixO19 samples with x > 0.5, the spinel NiFe2O4 phase has also appeared. The lattice parameters and crystallite sizes of the powders were concluded from the XRD data and Williamson-Hall method. Magnetic analyses showed that the coercivity of powders decreased from 5672 Oe to 639 Oe while the saturation magnetization increased from 74 emu/g to 81 emu/g with nickel substitution. The results of this study suggest that the strontium hexaferrites doped with Ni are suitable for applications in high density magnetic recording media as well as microwave devices because of their promising magnetic properties.

Preparation and physicochemical characterization of cellulose nanocrystals from industrial waste cotton

NASA Astrophysics Data System (ADS)

Thambiraj, S.; Ravi Shankaran, D.

2017-08-01

We aimed to develop a simple and low-cost method for the production of high-performance cellulose nanomaterials from renewable and sustainable resources. Here, cellulose microcrystals (CMCs) were prepared by controlled acidic and basic hydrolysis of cotton from textile industry wastes. The resulted CMCs were further converted into cellulose nanocrystals (CNCs) with high crystallinity by acidic hydrolysis. The physicochemical characteristics and morphological feature of CMCs and CNCs were studied by various analytical techniques such as UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Fluorescence spectroscopy, Atomic force microscopy (AFM), High-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The isolated CNCs possess a needle-like morphological structure with the longitudinal and lateral dimensions of 180 ± 60 nm, 10 ± 1 nm, respectively. The AFM result reveals that the CNCs have a high aspect ratio of 40 ± 14 nm and the average thickness of 6.5 nm. The XRD and TEM analysis indicate that the synthesized CNCs possess face-centered cubic crystal structure. Preliminary experiments were carried out to fabricate CNCs incorporated poly (vinyl alcohol) (PVA) film. The results suggest that the concept of waste to wealth could be well executed from the prepared CNCs, which have great potential for various applications including bio-sensors, food packaging and drug delivery applications.

Physical-chemical properties of nanocomposites based on poly(3-hydroxybutyrate-co-3-hydroxyvalerate) and titanium dioxide nanoparticles

NASA Astrophysics Data System (ADS)

Braga, Natália F.; da Silva, Ana Paula; Moraes Arantes, Tatiane; Lemes, Ana Paula; Cristovan, Fernando Henrique

2018-01-01

Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) was reinforced with titanium dioxide (TiO2) in concentrations of 1.0%, 2.5% and 5.0% (m/m) to produce nanocomposites by the solvent casting technique. TiO2 was synthesized by a hydrothermal treatment to produce nanoparticles. The nanostructure of the nanoparticles was studied by x-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The XRD confirmed TiO2 crystalline nanoparticles, with a mixture of anatase and rutile phases. Through TEM analysis, the formation of TiO2 nanorod agglomerates with an average diameter and length of 40 and 12 nm, respectively, was observed. The thermal and mechanical properties of the pure PHBV and nanocomposite films were characterized by differential scanning calorimetry (DSC) and dynamic mechanical analysis. The DSC analysis showed that the glass transition temperature decreased with the inclusion of TiO2 in the PHBV matrix in relation to pure PHBV. The results of biodegradation assays for the PHBV and nanocomposites in an aqueous medium and in soil showed morphological and structural changes for all samples, indicating a high biodegradation rate for this material. The most important conclusion is that the biodegradation of the PHBV was not affected by the addition of nanoparticles, thus enabling the use of nanocomposites in applications requiring biodegradable materials.

Preparation of N-doped ZnO-loaded halloysite nanotubes catalysts with high solar-light photocatalytic activity.

PubMed

Cheng, Zhi-Lin; Sun, Wei

2015-01-01

N-doped ZnO nanoparticles were successfully assembled into hollow halloysite nanotubes (HNTs) by using the impregnation method. The catalysts based on N-doped ZnO-loaded HNTs nanocomposites (N-doped ZnO/HNTs) were characterized by X-ray diffraction (XRD), transmission electron microscopy-energy dispersive X-ray (TEM-EDX), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), UV-vis and Fourier transform infrared spectroscopy (FT-IR) techniques. The XRD pattern showed ZnO nanoparticles with hexagonal structure loaded on HNTs. The TEM-EDX analysis indicated ZnO particles with the crystal size of ca.10 nm scattered in hollow structure of HNTs, and furthermore the concentration of N atom in nanocomposites was up to 2.31%. The SEM-EDX verified most of N-ZnO nanoparticles existing in hollow nanotubes of HNTs. Besides containing an obvious ultraviolet absorbance band, the UV-vis spectra of the N-doped ZnO/HNTs catalysts showed an available visible absorbance band by comparing to HNTs and non-doped ZnO/HNTs. The photocatalytic activity of the N-doped ZnO/HNTs catalysts was evaluated by the degradation of methyl orange (MO) solution with the concentration of 20 mg/L under the simulated solar-light irradiation. The result showed that the N-doped ZnO/HNTs catalyst exhibited a desirable solar-light photocatalytic activity.

A facile biomimetic preparation of highly stabilized silver nanoparticles derived from seed extract of Vigna radiata and evaluation of their antibacterial activity

NASA Astrophysics Data System (ADS)

Choudhary, Manoj Kumar; Kataria, Jyoti; Cameotra, Swaranjit Singh; Singh, Jagdish

2016-01-01

The significant antibacterial activity of silver nanoparticles draws the major attention toward the present nanobiotechnology. Also, the use of plant material for the synthesis of metal nanoparticles is considered as a green technology. In this context, a non-toxic, eco-friendly, and cost-effective method has been developed for the synthesis of silver nanoparticles using seed extract of mung beans ( Vigna radiata). The synthesized nanoparticles have been characterized by UV-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), atomic absorption spectroscopy (AAS), and X-ray diffraction (XRD). The UV-visible spectrum showed an absorption peak at around 440 nm. The different types of phytochemicals present in the seed extract synergistically reduce the Ag metal ions, as each phytochemical is unique in terms of its structure and antioxidant function. The colloidal silver nanoparticles were observed to be highly stable, even after 5 months. XRD analysis showed that the silver nanoparticles are crystalline in nature with face-centered cubic geometry and the TEM micrographs showed spherical particles with an average size of 18 nm. Further, the antibacterial activity of silver nanoparticles was evaluated by well-diffusion method and it was observed that the biogenic silver nanoparticles have an effective antibacterial activity against Escherichia coli and Staphylococcus aureus. The outcome of this study could be useful for nanotechnology-based biomedical applications.

A study on hydrogen-storage behaviors of nickel-loaded mesoporous MCM-41.

PubMed

Park, Soo-Jin; Lee, Seul-Yi

2010-06-01

The objective of the present work was to investigate the possibility of improving the hydrogen-storage capacity of mesoporous MCM-41 containing nickel (Ni) oxides (Ni/MCM-41). The MCM-41 and Ni/MCM-41 were prepared using a hydrothermal process as a function of Ni content (2, 5, and 10 wt.% in the MCM-41). The surface functional groups of the Ni/MCM-41 were identified by Fourier transform infrared spectroscopy (FTIR). The structure and morphology of the Ni/MCM-41 were characterized by X-ray diffraction (XRD) and field emission transmission electron microscopy (FE-TEM). XRD results showed a well-ordered hexagonal pore structure; FE-TEM also revealed, as a complementary technique, the structure and pore size. The textural properties of the Ni/MCM-41 were analyzed using N(2) adsorption isotherms at 77 K. The hydrogen-storage capacity of the Ni/MCM-41 was evaluated at 298 K/100 bar. It was found that the presence of Ni on mesoporous MCM-41 created hydrogen-favorable sites that enhanced the hydrogen-storage capacity by a spillover effect. Furthermore, it was concluded that the hydrogen-storage capacity was greatly influenced by the amount of nickel oxide, resulting in a chemical reaction between Ni/MCM-41 and hydrogen molecules. Crown Copyright © 2010. Published by Elsevier Inc. All rights reserved.

Fabrication of nano structural biphasic materials from phosphogypsum waste and their in vitro applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohamed, Khaled R., E-mail: Kh_rezk966@yahoo.com; Mousa, Sahar M.; Inorganic Chemistry Department, National Research Centre, Dokki, P.O. Box 12622, 11787 Cairo

2014-02-01

Graphical abstract: (a) Schema of the process, (b) TEM of nano particles of biphasic materials and (c) SEM of post-immersion. - Highlights: • Ratio of HA and β-TCP phases were controlled by thermal treatment. • HA partially decomposed into β-TCP with other bioactive phases. • Calcined HA at 900 °C is the best for the bioactivity behavior. - Abstract: In this study, a novel process of preparing biphasic calcium phosphate (BCP) is proposed. Also its bioactivity for the utilization of the prepared BCP as a biomaterial is studied. A mixture of calcium hydroxyapatite (HAP) and tricalcium phosphate (β-TCP) could bemore » obtained by thermal treatment of HAP which was previously prepared from phosphogypsum (PG) waste. The chemical and phase composition, morphology and particle size of prepared samples was characterized by X-ray diffraction (XRD), Infrared spectroscopy (IR), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The bioactivity was investigated by soaking of the calcined samples in simulated body fluid (SBF). Results confirmed that the calcination temperatures played an important role in the formation of calcium phosphate (CP) materials. XRD results indicated that HAP was partially decomposed into β-TCP. The in vitro data confirmed that the calcined HAP forming BCP besides other phases such as pyrophosphate and silica are bioactive materials. Therefore, BCP will be used as good biomaterials for medical applications.« less

Green synthesis of gold nanoparticles using a cheap Sphaeranthus indicus extract: Impact on plant cells and the aquatic crustacean Artemia nauplii.

PubMed

Balalakshmi, Chinnasamy; Gopinath, Kasi; Govindarajan, Marimuthu; Lokesh, Ravi; Arumugam, Ayyakannu; Alharbi, Naiyf S; Kadaikunnan, Shine; Khaled, Jamal M; Benelli, Giovanni

2017-08-01

The impact of green-fabricated gold nanoparticles on plant cells and non-target aquatic species is scarcely studied. In this research, we reported an environment friendly technique for the synthesis of gold nanoparticles (Au NPs) using the Sphaeranthus indicus leaf extract. The formation of the metal NPs was characterized by UV-Visible and FT-IR spectroscopy, XRD, SEM and TEM analyses. The UV-Visible spectra of Au NPs showed a surface plasmon resonance peak at 531nm. FT-IR analysis indicated functional bio-molecules associated with Au NPs formation. The crystalline nature of Au nanoparticles was confirmed by their XRD diffraction pattern. TEM revealed the spherical shape with a mean particle size of 25nm. Au NPs was tested at 0, 1, 3, 5, 7 and 10% doses in mitotic cell division assays, pollen germination experiments, and in vivo toxicity trials against the aquatic crustacean Artemia nauplii. Au NPs did not show any toxic effects on plant cells and aquatic invertebrates. Notably, Au NPs promoted mitotic cell division in Allium cepa root tip cells and germination of Gloriosa superba pollen grains. Au NPs showed no mortality on A. nauplii, all the tested animals showed 100% survivability. Therefore, these Au NPs have potential applications in the development of pollen germination media and plant tissue culture. Copyright © 2017 Elsevier B.V. All rights reserved.

Green synthesis, characterization and antibacterial efficacy of palladium nanoparticles synthesized using Filicium decipiens leaf extract

NASA Astrophysics Data System (ADS)

Sharmila, G.; Farzana Fathima, M.; Haries, S.; Geetha, S.; Manoj Kumar, N.; Muthukumaran, C.

2017-06-01

Synthesis of metal nanoparticles through green chemistry route is an emerging eco-friendly approach in the present days. An eco-friendly, biogenic synthesis of palladium nanoparticles (PdNPs) using Filicium decipiens leaf extract was reported in the present study. The synthesized PdNPs were characterized by UV-visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The PdNPs formation was confirmed by UV-visible spectrophotometer and spherical shaped PdNPs with size range of 2-22 nm was observed in TEM analysis. Energy dispersive X-ray spectroscopy (EDS) analysis confirmed the presence of palladium in the synthesized nanoparticles. The crystalline nature of PdNPs was confirmed by XRD pattern and compared with the standard. The phytochemicals and proteins were identified by their functional groups in FT-IR spectrum and revealed the amide, amine groups present in F. decipiens may have involved in the bio-reduction reaction for PdNPs synthesis. Prepared PdNPs showed potential antibacterial activity against both Gram-positive and Gram-negative bacteria. F. decipiens leaf extract based PdNPs showed high bactericidal activity against Escherichia coli, Pseudomonas aeruginosa as compared to Staphylococcus aureus and Bacillus subtilis Results showed that phytochemicals rich F. decipiens leaf extract may be utilized as an effective non-toxic reducing agent for PdNPs synthesis and prepared PdNPs may useful in biomedical applications.

Designing of luminescent GdPO4:Eu@LaPO4@SiO2 core/shell nanorods: Synthesis, structural and luminescence properties

NASA Astrophysics Data System (ADS)

Ansari, Anees A.; Labis, Joselito P.; Aslam Manthrammel, M.

2017-09-01

GdPO4:Eu3+ (core) and GdPO4:Eu@LaPO4 (core/shell) nanorods (NRs) were successfully prepared by urea based co-precipitation process at ambient conditions which was followed by coating with amorphous silica shell via the sol-gel chemical route. The role of surface coating on the crystal structure, crystallinity, morphology, solubility, surface chemistry and luminescence properties were well investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, Fourier Transform Infrared (FTIR), UV-Vis, and photoluminescence spectroscopy. XRD pattern revealed highly purified, well-crystalline, single phase-hexagonal-rhabdophane structure of GdPO4 crystal. The TEM micrographs exhibited highly crystalline and narrow size distributed rod-shaped GdPO4:Eu3+ nanostructures with average width 14-16 nm and typical length 190-220 nm. FTIR spectra revealed characteristic infrared absorption bands of amorphous silica. High absorbance in a visible region of silica modified core/shell/Si NRs in aqueous environment suggests the high solubility along with colloidal stability. The photoluminescence properties were remarkably enhanced after growth of undoped LaPO4 layers due to the reduction of nonradiative transition rate. The advantages of presented high emission intensity and high solubility of core/shell and core/shell/Si NRs indicated the potential applications in monitoring biological events.

Structural, optical and morphological characterization of Cu-doped α-Fe2O3 nanoparticles synthesized through co-precipitation technique

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-11-01

Pure and copper (Cu concentration varying from 2 to 8%) doped hematite (α-Fe2O3) nanocrystals were synthesized through co-precipitation method using simple equipment. X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA) and Ultraviolet-Visible (UV-Vis) techniques were used to characterize the synthesized samples. XRD measurements confirm that all the prepared nanocrystals consist only in nanocrystalline hematite phase. These results along with TEM and SEM show that the size of the nanoparticles decreases with Cu-doping down to 21 nm. FT-IR confirm the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we synthesized pure and Cu-doped hematite but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The UV-Vis absorption measurements confirm that the decrease of particle size is accompanied by a decrease in the band gap value from 2.12 eV for pure α-Fe2O3 down to 1.91 eV for 8% Cu-doped α-Fe2O3. 8% Cu-doped hematite had the smallest size, the best crystallinity and the lowest band gap.

Green synthesis of gold nanoparticles using Citrus maxima peel extract and their catalytic/antibacterial activities.

PubMed

Yuan, Chun-Gang; Huo, Can; Gui, Bing; Cao, Wei-Ping

2017-08-01

The peel of Citrus maxima ( C. maxima ) is the primary byproducts during the process of fruit or juice in food industries, and it was always considered as biomass waste for further treatments. In this study, the authors reported a simple and eco-friendly method to synthesise gold nanoparticles (AuNPs) using C. maxima peel extract as reducing and capping agents. The synthesised AuNPs were characterised by UV-visible spectrum, X-ray diffraction (XRD), transmission electron microscope (TEM) and Fourier-transform infrared spectroscopy (FTIR). The UV-visible spectrum of the AuNPs colloid showed a characteristic peak at 540 nm. The peaks of XRD analysis at (2 θ ) 38.30°, 44.28°, 64.62°, 77.57° and 81.75° were assigned to (111), (200), (220), (311) and (222) planes of the face-centered cubic (fcc) lattice of gold. The TEM images showed that AuNPs were nearly spherical in shape with the size of 8-25 nm. The FTIR spectrum revealed that some bioactive compounds capped the surface of synthesised AuNPs. The biosynthesised AuNPs performed strong catalytic activity in degradation of 4-nitrophenol to 4-aminophenol and good antibacterial activity against both gram negative ( Escherichia coli ) and gram positive ( Staphylococcus aureus ) bacterium. The synthesis procedure was proved simple, cost effective and environment friendly.

Evaluation of AlGaN/GaN high electron mobility transistors grown on ZrTi buffer layers with sapphire substrates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ren, Fan; Pearton, Stephen J.; Ahn, Shihyun

Here, AlGaN/GaN high electron mobility transistors (HEMTs) have been grown on sapphire substrates, using ZrTi buffer layers to provide in-plane lattice-matching to hexagonal GaN. X-ray diffraction (XRD) as well as cross-section transmission electron microscopy (TEM) were used to assess the quality of the HEMT structure. The XRD 2θ scans showed full-width-at-half-maximum values of 0.16°, 0.07°, and 0.08° for ZrTi alloy, GaN buffer layer, and the entire HEMT structure, respectively. TEM studies of the GaN buffer layer and the AlN/ZrTi/AlN stack showed the importance of growing thin AlN buffer layers on the ZrTi layer prior to growth of the GaN buffermore » layer. The density of threading dislocations in the GaN channel layer of the HEMT structure was estimated to be in the 10 8 cm –2 range. The HEMT device exhibited a saturation drain current density of 820 mA/mm, and the channel of the fabricated HEMTs could be well modulated. A cutoff frequency (f T) of 8.9 GHz and a maximum frequency of oscillation (f max) of 17.3 GHz were achieved for HEMTs with gate dimensions of 1 × 200 μm.« less

Evaluation of AlGaN/GaN high electron mobility transistors grown on ZrTi buffer layers with sapphire substrates

DOE PAGES

Ren, Fan; Pearton, Stephen J.; Ahn, Shihyun; ...

2016-09-21

Here, AlGaN/GaN high electron mobility transistors (HEMTs) have been grown on sapphire substrates, using ZrTi buffer layers to provide in-plane lattice-matching to hexagonal GaN. X-ray diffraction (XRD) as well as cross-section transmission electron microscopy (TEM) were used to assess the quality of the HEMT structure. The XRD 2θ scans showed full-width-at-half-maximum values of 0.16°, 0.07°, and 0.08° for ZrTi alloy, GaN buffer layer, and the entire HEMT structure, respectively. TEM studies of the GaN buffer layer and the AlN/ZrTi/AlN stack showed the importance of growing thin AlN buffer layers on the ZrTi layer prior to growth of the GaN buffermore » layer. The density of threading dislocations in the GaN channel layer of the HEMT structure was estimated to be in the 10 8 cm –2 range. The HEMT device exhibited a saturation drain current density of 820 mA/mm, and the channel of the fabricated HEMTs could be well modulated. A cutoff frequency (f T) of 8.9 GHz and a maximum frequency of oscillation (f max) of 17.3 GHz were achieved for HEMTs with gate dimensions of 1 × 200 μm.« less

Luminescent properties of Eu{sup 2+}-doped BaGdF{sub 5} glass ceramics a potential blue phosphor for ultra-violet light-emitting diode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Weihuan; Zhang, Yuepin, E-mail: zhangyuepin@nbu.edu.cn; Ouyang, Shaoye

2015-01-14

Eu{sup 2+} doped transparent oxyfluoride glass ceramics containing BaGdF{sub 5} nanocrystals were successfully fabricated by melt-quenching technique under a reductive atmosphere. The structure of the glass and glass ceramics were investigated by differential scanning calorimetry, X-ray diffraction (XRD), and transmission electron microscopy (TEM). The luminescent properties were investigated by transmission, excitation, and emission spectra. The decay time of the Gd{sup 3+} ions at 312 nm excited with 275 nm were also investigated. The results of XRD and TEM indicated the existence of BaGdF5 nanocrystals in the transparent glass ceramics. The excitation spectra of Eu{sup 2+} doped glass ceramics showed an excellent overlapmore » with the main emission region of an ultraviolet light-emitting diode (UV-LED). Compared with the as-made glass, the emission of glass ceramics is much stronger by a factor of increasing energy transfer efficiency from Gd{sup 3+} to Eu{sup 2+} ions, the energy transfer efficiency from Gd{sup 3+} to Eu{sup 2+} ions was discussed. In addition, the chromaticity coordinates of glass and glass ceramics specimens were also discussed, which indicated that the Eu{sup 2+} doped BaGdF{sub 5} glass ceramics may be used as a potential blue-emitting phosphor for UV-LED.« less

Chemical interaction of glycero-phosphate dimethacrylate (GPDM) with hydroxyapatite and dentin.

PubMed

Yoshihara, Kumiko; Nagaoka, Noriyuki; Hayakawa, Satoshi; Okihara, Takumi; Yoshida, Yasuhiro; Van Meerbeek, Bart

2018-04-28

Although the functional monomer glycero-phosphate dimethacrylate (GPDM) has since long been used in several dental adhesives and more recently in self-adhesive composite cements and restoratives, its mechanism of chemical adhesion to hydroxyapatite (HAp) is still unknown. We therefore investigated the chemical interaction of GPDM with HAp using diverse chemical analyzers and ultra-structurally characterized the interface of a GPDM-based primer formulation with dentin. HAp particles were added to a GPDM solution for various periods, upon which they were thoroughly washed with ethanol and water prior to being air-dried. As control, 10-methacryloyloxydecyl dihydrogen phosphate (MDP) was used. The molecular interaction of GPDM with HAp was analyzed using X-ray diffraction (XRD) and solid-state nuclear magnetic resonance (NMR) spectroscopy. Crystal formation upon application of GPDM onto dentin was analyzed using thin-film XRD (TF-XRD). Its hydrophobicity was measured using contact-angle measurement. The interaction of GPDM with dentin was characterized using transmission electron microscopy (TEM). XRD revealed the deposition of dicalcium phosphate dihydrate (DCPD: CaHPO 4 ·2H 2 O) on HAp after 24h. NMR confirmed the adsorption of GPDM onto HAp. However, GPDM was easily removed after washing with water, unlike MDP that remained adhered to HAp. Dentin treated with GPDM appeared more hydrophilic compared to dentin treated with MDP. TEM disclosed exposed collagen in the hybrid layer produced by the GPDM-based primer formulation. Although GPDM adsorbed to HAp, it did not form a stable calcium salt. The bond between GPDM and HAp was weak, unlike the strong bond formed by MDP to HAp. Due to its high hydrophilicity, GPDM might be an adequate monomer for an etch-and-rinse adhesive, but appears less appropriate for a 'mild' self-etch adhesive that besides micro-retention ionically interacts with HAp, or for a self-adhesive restorative material. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Local symmetry breaking in SnO2 nanocrystals with cobalt doping and its effect on optical properties.

PubMed

Roy, S; Joshi, Amish G; Chatterjee, S; Ghosh, Anup K

2018-06-07

X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to study the structural and morphological characteristics of cobalt doped tin(iv) oxide (Sn1-xCoxO2; 0 ≤ x ≤ 0.04) nanocrystals synthesized by a chemical co-precipitation technique. Electronic structure analysis using X-ray photoemission spectroscopy (XPS) shows the formation of tin interstitials (Sni) and reduction of oxygen vacancies (VO) in the host lattice on Co doping and that the doped Co exists in mixed valence states of +2 and +3. Using XRD, the preferential position of the Sni and doped Co in the unit cell of the nanocrystals have been estimated. Rietveld refinement of XRD data shows that samples are of single phase and variation of lattice constants follows Vegard's law. XRD and TEM measurements show that the crystallite size of the nanocrystals decrease with increase in Co doping concentration. SAED patterns confirm the monocrystalline nature of the samples. The study of the lattice dynamics using Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy shows the existence of many disorder activated forbidden optical phonon modes, along with the corresponding classical modes, signifying Co induced local symmetry breaking in the nanocrystals. UV-Vis spectroscopy shows that the optical band gap has red shifted with increase in doping concentration. The study of Urbach energy confirms the increase in disorder in the nanocrystals with Co doping. Local symmetry breaking induced UV emission along with violet, blue and green luminescence has been observed from the PL study. The spectral contribution of UV emission decreases and green luminescence increases with increase in doping. Using PL, in conjunction with Raman spectroscopy, the type of oxygen vacancy induced in the nanocrystals on Co doping has been confirmed and the position of the defect levels in the forbidden zone (w.r.t. the optical band gap) has been studied.

The effect of ultrasonic irradiation on the structure, morphology and photocatalytic performance of ZnO nanoparticles by sol-gel method.

PubMed

Mahdavi, Reza; Ashraf Talesh, S Siamak

2017-11-01

In this research, the effect of ultrasonic irradiation power (0, 75, 150 and 200W) and time (0, 5, 15 and 20min) on the structure, morphology and photocatalytic activity of zinc oxide nanoparticles synthesized by sol-gel method was investigated. Crystallographic structures and the morphologies of the resultant powders were determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns showed that ZnO samples were crystallized in their pure phase. The purity of samples was increased by increasing the ultrasonic irradiation power and time. Not only did ultrasonic irradiation unify both the structure and the morphology, but also it reduced the size and prohibited particles from aggregation. The optical behavior of the samples was studied by UV-vis spectroscopy. Photocatalytic activity of particles was measured by degradation of methyl orange under radiation of ultraviolet light. Ultrasound nanoparticles represented higher degradation compared to non-ultrasound ones. Copyright © 2017 Elsevier B.V. All rights reserved.

Improvement of crystalline quality of N-polar AlN layers on c-plane sapphire by low-pressure flow-modulated MOCVD

NASA Astrophysics Data System (ADS)

Takeuchi, M.; Shimizu, H.; Kajitani, R.; Kawasaki, K.; Kumagai, Y.; Koukitu, A.; Aoyagi, Y.

2007-01-01

The growth of N-polar AlN layers on c-plane sapphire is reported. Low-temperature AlN (LT-AlN) layers were used as seeding buffer layers with pre-nitridation for sapphire. To avoid strong vapor-phase reaction between trimethylaluminum (TMA) and ammonia (NH 3) and to improve the crystalline quality, low-pressure flow-modulated (FM) metal-organic chemical vapor deposition (MOCVD) technique was introduced with careful optimization of the FM sequence. The surface morphologies and the crystalline quality defined by the X-ray diffraction (XRD) (0 0 2) and (1 0 0) rocking curve measurements strongly depended on the LT-AlN thickness and on the TMA coverage per cycle of the FM growth. The sample showing the best XRD data with a good morphology was almost completely etched in aqueous KOH solution owing to N-polarity. From the plan-view transmission electron microscopy (TEM) observation, the dislocation density was counted to be about 3×10 10 cm -2.

A green approach to prepare silver nanoparticles loaded gum acacia/poly(acrylate) hydrogels.

PubMed

Bajpai, S K; Kumari, Mamta

2015-09-01

In this work, gum acacia (GA)/poly(sodium acrylate) semi-interpenetrating polymer networks (Semi-IPN) have been fabricated via free radical initiated aqueous polymerization of monomer sodium acrylate (SA) in the presence of dissolved Gum acacia (GA), using N,N'-methylenebisacrylamide (MB) as cross-linker and potassium persulphate (KPS) as initiator. The semi-IPNs, synthesized, were characterized by various techniques such as X-ray diffraction (XRD), thermo gravimetric analysis (TGA) and Fourier transform infrared (FTIR) spectroscopy. The dynamic water uptake behavior of semi-IPNs was investigated and the data were interpreted by various kinetic models. The equilibrium swelling data were used to evaluate various network parameters. The semi-IPNs were used as template for the in situ preparation of silver nanoparticles using extract of Syzygium aromaticum (clove). The formation of silver nanoparticles was confirmed by surface plasmon resonance (SPR), XRD and transmission electron microscopy (TEM). Finally, the antibacterial activity of GA/poly(SA)/silver nanocomposites was tested against E. coli. Copyright © 2015 Elsevier B.V. All rights reserved.

Controllable self-assembly of mesoporous hydroxyapatite.

PubMed

Chen, Jingdi; Wang, Zihao; Wen, Zhenliang; Yang, Shen; Wang, Jianhua; Zhang, Qiqing

2015-03-01

In this paper, mesoporous hydroxyapatite (HAp) of controllable pore size was tailored with the template of a biodegradable mono-alkyl phosphate (MAP) via a simple route by hydrothermal treatment. A serial study of the various experimental parameters on pore size of HAp was investigated. The additive amount of MAP and hydrothermal temperature were important factors for the pore structure and pore size. Powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption-desorption (BET, BJH) were used to characterize the structure and composition of the HAp samples. Both XRD and BJH results indicated that regular mesoporous HAp nanoparticles (with a mean pore size of 3.5nm) were successfully produced. As shown in transmission electron microscopy (TEM), orderly uniform pore structure appeared in the HAp particles. Because of the special structure of the MAP and the interaction between ionized MAP and other ions in solution, the product presents uniform mesoporous structure with well-defined pore size. Copyright © 2015 Elsevier B.V. All rights reserved.

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

An electrochemical sensor based on nitrogen doped carbon material prepared from nitrogen-containing precursors

NASA Astrophysics Data System (ADS)

Cui, G. Y.; Wang, C. Y.; Xiang, G. Q.; Zhou, B.

2018-01-01

In this work, a nitrogen doped carbon material (NDC) was prepared by using a copper adenine complex as precursor and applied to electrochemical sensing of Vitamin B2 (VB2). The experimental results show that the nitrogen doped carbon material is obtained after calcination at 650 °C under argon atmosphere, afterwards, which were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), fourier transform infrared (FT-IR), and electrochemical method. According to the XRD data, the product was a carbon material, and infrared data demonstrates that there are two kinds of carbonyl nitrogen combination, respectively, C-N and C = N combination of ways. Importantly, we used NDC to construct electrochemical biosensor to detect VB2 by differential pulse voltammetry (DPV). The linear range was 6 × 10-6 - 3.5 × 10-4 M (R=0.9962), the minimum detection limit was 5.4 × 10-6 M, and the sensitivity is better. Consequently, it has better sensing performance.

Photocatalytic degradation of methyl orange and bromophenol blue dyes in water using sol-gel synthesized TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Dhanalakshmi, J.; Pathinettam Padiyan, D.

2017-09-01

TiO2 nanoparticles were prepared by a sol-gel method using titanium tetra isopropoxide as a precursor. The structural, optical, morphological and electrical properties were studied by x-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), a high resolution scanning electron microscope (HR-SEM), a transmission electron microscope (TEM), Raman analysis, Photoluminescence (PL) and impedance spectroscopy. The XRD and Raman spectra revealed that the synthesized samples are in pure anatase phase with an average crystallite size of 18 nm. Photocatalytic activity of the TiO2 nanoparticles was investigated for the degradation of 10 ppm methyl orange (MO) and bromophenol blue (BPB) dye using 10 mg of catalyst. Anatase TiO2 exhibited the removal of 67.12% and 85.51% of MO and BPB, respectively, within 240 min. The photocatalytic degradation process is explained using pseudo second order kinetics and fits well with the higher correlation coefficient.

Evaluation of electrical properties of Cr/CrN nano-multilayers for electronic applications.

PubMed

Marulanda, D M; Olaya, J J; Patiño, E J

2011-06-01

The electrical properties of Cr/CrN nano-multilayers produced by Unbalanced Magnetron Sputtering have been studied as a function of bilayer period and total thickness. Two groups of multilayers were produced: in the first group the bilayer period varied between 20 nm, 100 nm and 200 nm with total thickness of 1 microm, and in the second group the bilayer period varied between 25 nm, 50 nm and 100 nm and a total thickness of 100 nm. X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) were used in order to investigate the microstructure characteristics of the multilayers, and the Four Point Probe (FPP) method was used to evaluate in-plane and transverse electrical resistivity. XRD results show (111) and (200) orientations for all the CrN coatings and the presence of a multilayer structure was confirmed through SEM studies. Transverse electrical resistivity results show that this property is strongly dependent on the bilayer period.

The preparation and cathodoluminescence of ZnS nanowires grown by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Huang, Meng-Wen; Cheng, Yin-Wei; Pan, Ko-Ying; Chang, Chen-Chuan; Shieu, F. S.; Shih, Han C.

2012-11-01

Single crystal ZnS nanowires were successfully synthesized in large quantities on Si (1 0 0) substrates by simple thermal chemical vapor deposition without using any catalyst. The morphology, composition, and crystal structure were characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and cathodoluminescence (CL) spectroscopy. SEM observations show that the nanowires have diameters about 20-50 nm and lengths up to several tens of micrometers. XRD and TEM results confirmed that the nanowires exhibited both wurtzite and zinc blende structures with growth directions aligned along [0 0 0 2] and [1 1 1], respectively. The CL spectrum revealed emission bands in the UV and blue regions. The blue emissions at 449 and ˜581 nm were attributed to surface states and impurity-related defects of the nanowires, respectively. The perfect crystal structure of the nanowires indicates their potential applications in nanotechnology and in the fabrication of nanodevices.

Synthesis and characterization of CdS/PVA nanocomposite films

NASA Astrophysics Data System (ADS)

Wang, Hongmei; Fang, Pengfei; Chen, Zhe; Wang, Shaojie

2007-08-01

A series CdS/PVA nanocomposite films with different amount of Cd salt have been prepared by means of the in situ synthesis method via the reaction of Cd 2+-dispersed poly vinyl-alcohol (PVA) with H 2S. The as-prepared films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectra, Fourier transform infrared spectroscope (FTIR) and thermogravimetric analysis (TGA). The XRD results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The primary FTIR spectra of CdS/PVA nanocomposite in different processing stages have been discussed. The vibrational absorption peak of Cd sbnd S bond at 405 cm -1 was observed, which further testified the generation of CdS nanoparticles. The TGA results showed incorporation of CdS nanoparticles significantly altered the thermal properties of PVA matrix. The photoluminescence and UV-vis spectroscopy revealed that the CdS/PVA films showed quantum confinement effect.

Highly Sensitive NiO Nanoparticle based Chlorine Gas Sensor

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Singh, Arun

2018-03-01

We have synthesized a chemiresistive sensor for chlorine (Cl2) gas in the range of 2-200 ppm based on nickel oxide (NiO) nanoparticles obtained by wet chemical synthesis. The nanoparticles were characterized by x-ray diffraction (XRD) analysis, field-emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), transmission electron microscopy (TEM), Fourier-transform infrared (FTIR) spectroscopy, Raman spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, and photoluminescence (PL) spectroscopy. XRD spectra of the sensing layer revealed the cubic phase of NiO nanoparticles. The NiO nanoparticle size was calculated to be ˜ 21 nm using a Williamson-Hall plot. The bandgap of the NiO nanoparticles was found to be 3.13 eV using Tauc plots of the absorbance curve. Fast response time (12 s) and optimum recovery time (˜ 27 s) were observed for 10 ppm Cl2 gas at moderate temperature of 200°C. These results demonstrate the potential application of NiO nanoparticles for fabrication of highly sensitive and selective sensors for Cl2 gas.

A novel method for the functionalization of aminoacids L-glycine, L-glutamic acid and L-arginine on maghemite/magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Bruno, A. J.; Correa, J. R.; Peláez-Abellán, E.; Urones-Garrote, E.

2018-06-01

Nanoparticles of maghemite/magnetite functionalized with L-glycine, L-glutamic acid and L-arginine were synthesized by a novel method. The novel procedure consists in an alternative of that reported by Massart for the precipitation of magnetite in which the aminoacid is added in the carboxylate form. The amounts of aminoacid in the initial molar concentrations were 35%, 45% and 65% with respect to the ferrophase. The obtained nanoparticles were characterized by several techniques: X-ray diffraction (XRD), Fourier transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), Electron energy-loss spectroscopy (EELS) and magnetometry. The IR spectroscopy confirmed that the selected aminoacids were functionalized on the surface of iron oxide. XRD and EELS confirm that iron oxide consists of a maghemite-magnetite intermediate phase with an average particle size about 6 nm, which was measured by transmission electron microscopy. The superparamagnetic character of the nanoparticles was evaluated by magnetometry.

Production of new cellulose nanomaterial from red algae marine biomass Gelidium elegans.

PubMed

Chen, You Wei; Lee, Hwei Voon; Juan, Joon Ching; Phang, Siew-Moi

2016-10-20

Nanocellulose was successfully isolated from Gelidium elegans red algae marine biomass. The red algae fiber was treated in three stages namely alkalization, bleaching treatment and acid hydrolysis treatment. Morphological analysis was performed by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). TEM results revealed that the isolated nanocellulose had the average diameter and length of 21.8±11.1nm and of 547.3±23.7nm, respectively. Fourier transform infrared (FTIR) spectroscopy proved that the non-cellulosic polysaccharides components were progressively removed during the chemically treatment, and the final derived materials composed of cellulose parent molecular structure. X-ray diffraction (XRD) study showed that the crystallinity of yielded product had been improved after each successive treatments subjected to the treated fiber. The prepared nano-dimensional cellulose demonstrated a network-like structure with higher crystallinity (73%) than that of untreated fiber (33%), and possessed of good thermal stability which is suitable for nanocomposite material. Copyright © 2016 Elsevier Ltd. All rights reserved.

Visible cathodoluminescence of Er ions in β-Ga(2)O(3) nanowires and microwires.

PubMed

Nogales, E; Méndez, B; Piqueras, J

2008-01-23

Erbium doped β-Ga(2)O(3) nanowires and microwires have been obtained by a vapour-solid process from an initial mixture of Ga(2)O(3) and Er(2)O(3) powders. X-ray diffraction (XRD) analysis reveals the presence of erbium gallium garnet as well as β-Ga(2)O(3) phases in the microwires. Scanning electron microscopy (SEM) images show that the larger microwires have a nearly rectangular cross-section. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) analysis show good crystal quality of the β-Ga(2)O(3) nanowires. The nanostructures have been studied by means of the cathodoluminescence technique in the scanning electron microscope. Er intraionic blue, green and red emission lines are observed in luminescence spectra even at room temperature, which confirms the optical activity of the rare earth ions in the grown structures. Mapping of the main 555 nm emission intensity shows a non-homogeneous distribution of Er ions in the microstructures.

Deformation Behavior and Microstructure of Ti6Al4V Manufactured by SLM

NASA Astrophysics Data System (ADS)

Krakhmalev, P.; Fredriksson, G.; Yadroitsava, I.; Kazantseva, N.; Plessis, A. du; Yadroitsev, I.

Mechanical properties, porosity, and microstructure of Ti6Al4V (ELI) material produced by Selective Laser Melting (SLM) under controlled oxygen content were analyzed. Fully martensitic α'structure with high dislocation density and stacking faults was observed in both as-built and stress relieved samples by means of XRD and TEM. Tensile {101 ̅2} twinning was identified by TEM and electron diffraction. Accommodation of thermal stresses during manufacturing was suggested as a possible reason for twinning. Computed tomography of pores was carried out. Pores in the specimens were evenly distributed and mostly had an elongated shape. Defect analysis by micro CT scans in pre-strained samples confirmed that the pore coalescence was the main crack formation mechanism in the final fracture with typical cup-and-cone fracture morphology. Additionally, typical dimples and quasi-cleavage were revealed. Mechanical properties of the samples after stress relieving heat treatment at 650°C for 3 h are complied with the international standard for Ti alloys for biomedical applications.

Synthesis and Luminescence Properties of Core/Shell ZnS:Mn/ZnO Nanoparticles.

PubMed

Jiang, Daixun; Cao, Lixin; Liu, Wei; Su, Ge; Qu, Hua; Sun, Yuanguang; Dong, Bohua

2009-01-01

In this paper the influence of ZnO shell thickness on the luminescence properties of Mn-doped ZnS nanoparticles is studied. Transmission electron microscopy (TEM) images showed that the average diameter of ZnS:Mn nanoparticles is around 14 nm. The formation of ZnO shells on the surface of ZnS:Mn nanoparticles was confirmed by X-ray diffraction (XRD) patterns, high-resolution TEM (HRTEM) images, and X-ray photoelectron spectroscopy (XPS) measurements. A strong increase followed by a gradual decline was observed in the room temperature photoluminescence (PL) spectra with the thickening of the ZnO shell. The photoluminescence excitation (PLE) spectra exhibited a blue shift in ZnO-coated ZnS:Mn nanoparticles compared with the uncoated ones. It is shown that the PL enhancement and the blue shift of optimum excitation wavelength are led by the ZnO-induced surface passivation and compressive stress on the ZnS:Mn cores.

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

NASA Astrophysics Data System (ADS)

Nirmala, R.; Sheikh, Faheem A.; Kanjwal, Muzafar A.; Lee, John Hwa; Park, Soo-Jin; Navamathavan, R.; Kim, Hak Yong

2011-05-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N, N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA-Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA-Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus ( S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli ( E. coli) by the disc diffusion susceptibility test. The HA-Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

Fabrication, characterization and application of pectin degrading Fe3O4-SiO2 nanobiocatalyst.

PubMed

Seenuvasan, Muthulingam; Malar, Carlin Geor; Preethi, Sridhar; Balaji, Nagarajan; Iyyappan, Jeyaraj; Kumar, Madhava Anil; Kumar, Kannaiyan Sathish

2013-05-01

The covalent binding of pectinase onto amino functionalized silica-coated magnetic nanoparticles (CSMNPs) through glutaraldehyde activation was investigated for nanobiocatalyst fabrication. The average particle size and morphology of the nanoparticles were characterized using transmission electron microscopy (TEM). The statistical analysis for TEM image suggests that the coating and binding process did not cause any significant change in size of MNPs. The morphological and phase change of the magnetic nanoparticles (MNPs) after various coatings and immobilization were characterized by X-ray diffraction (XRD) studies. The various surface modifications and pectinase binding onto nanoparticles were confirmed by Fourier transform infrared (FT-IR) spectroscopy. The maximum activity of immobilized pectinase was obtained at its weight ratio of 19.0×10(-3) mg bound pectinase/mg CSMNPs. The pH, temperature, reusability, storage ability and kinetic studies were established to monitor their improved stability and activity of the fabricated nanobiocatalyst. Furthermore, the application was extended in the clarification of Malus domestica juice. Copyright © 2013 Elsevier B.V. All rights reserved.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

Novel synthesis and structural analysis of zinc oxide nanoparticles for the non enzymatic glucose biosensor.

PubMed

Dayakar, T; Venkateswara Rao, K; Bikshalu, K; Rajendar, V; Park, Si-Hyun

2017-06-01

A non-enzymatic glucose biosensor was developed by utilizing the zinc oxide nanoparticles (ZnO NPs) synthesized by a novel green method using the leaf extract of Ocimum tenuiflorum. The structural, optical and morphological properties of ZnO NPs characterized by means of X-ray diffraction (XRD), ultraviolet-visible (UV-vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray (EDAX) spectroscopy, and transmission electron microscopy (TEM). The XRD analysis revealed that the ZnO NPs were crystalline and had a hexagonal wurtzite structure. The crystallite size measured by XRD was the same as that measured using SEM and TEM. The UV-vis absorption spectrum estimates the band gap of ZnO NPs present in the range of 2.82 to 3.45eV. The reduction and formation of ZnO NPs mainly due to the involvement of leaf extract bio-molecular compounds analyzed from the FTIR spectra. The SEM result confirms the morphology of the NPs responsible from the various concentration of leaf extract in the synthesis process. HRTEM analysis depicts the spherical structure of ZnO NPs. The synthesized NPs have the average size ranges from 10 to 20nm. The fabricated GCE/ZnO glucose sensor represents superior electro catalytic activity that has been observed for ZnO NPs with a reproducible sensitivity of 631.30μAmM -1 cm -2 , correlation coefficient of R=0.998, linear dynamic range from 1-8.6mM, low detection limit of 0.043μM (S/N=3) and response time<4s. Copyright © 2017 Elsevier B.V. All rights reserved.

Low toxic maghemite nanoparticles for theranostic applications.

PubMed

Kuchma, Elena A; Zolotukhin, Peter V; Belanova, Anna A; Soldatov, Mikhail A; Lastovina, Tatiana A; Kubrin, Stanislav P; Nikolsky, Anatoliy V; Mirmikova, Lidia I; Soldatov, Alexander V

2017-01-01

Iron oxide nanoparticles have numerous and versatile biological properties, ranging from direct and immediate biochemical effects to prolonged influences on tissues. Most applications have strict requirements with respect to the chemical and physical properties of such agents. Therefore, developing rational design methods of synthesis of iron oxide nanoparticles remains of vital importance in nanobiomedicine. Low toxic superparamagnetic iron oxide nanoparticles (SPIONs) for theranostic applications in oncology having spherical shape and maghemite structure were produced using the fast microwave synthesis technique and were fully characterized by several complementary methods (transmission electron microscopy [TEM], X-ray diffraction [XRD], dynamic light scattering [DLS], X-ray photoelectron spectroscopy [XPS], X-ray absorption near edge structure [XANES], Mossbauer spectroscopy, and HeLa cells toxicity testing). TEM showed that the majority of the obtained nanoparticles were almost spherical and did not exceed 20 nm in diameter. The averaged DLS hydrodynamic size was found to be ~33 nm, while that of nanocrystallites estimated by XRD waŝ16 nm. Both XRD and XPS studies evidenced the maghemite (γ-Fe 2 O 3 ) atomic and electronic structure of the synthesized nanoparticles. The XANES data analysis demonstrated the structure of the nanoparticles being similar to that of macroscopic maghemite. The Mossbauer spectroscopy revealed the γ-Fe 2 O 3 phase of the nanoparticles and vibration magnetometry study showed that reactive oxygen species in HeLa cells are generated both in the cytoplasm and the nucleus. Quasispherical Fe 3+ SPIONs having the maghemite structure with the average size of 16 nm obtained by using the fast microwave synthesis technique are expected to be of great value for theranostic applications in oncology and multimodal anticancer therapy.

Low toxic maghemite nanoparticles for theranostic applications

PubMed Central

Zolotukhin, Peter V; Belanova, Anna A; Soldatov, Mikhail A; Lastovina, Tatiana A; Kubrin, Stanislav P; Nikolsky, Anatoliy V; Mirmikova, Lidia I

2017-01-01

Background Iron oxide nanoparticles have numerous and versatile biological properties, ranging from direct and immediate biochemical effects to prolonged influences on tissues. Most applications have strict requirements with respect to the chemical and physical properties of such agents. Therefore, developing rational design methods of synthesis of iron oxide nanoparticles remains of vital importance in nanobiomedicine. Methods Low toxic superparamagnetic iron oxide nanoparticles (SPIONs) for theranostic applications in oncology having spherical shape and maghemite structure were produced using the fast microwave synthesis technique and were fully characterized by several complementary methods (transmission electron microscopy [TEM], X-ray diffraction [XRD], dynamic light scattering [DLS], X-ray photoelectron spectroscopy [XPS], X-ray absorption near edge structure [XANES], Mossbauer spectroscopy, and HeLa cells toxicity testing). Results TEM showed that the majority of the obtained nanoparticles were almost spherical and did not exceed 20 nm in diameter. The averaged DLS hydrodynamic size was found to be ~33 nm, while that of nanocrystallites estimated by XRD waŝ16 nm. Both XRD and XPS studies evidenced the maghemite (γ-Fe2O3) atomic and electronic structure of the synthesized nanoparticles. The XANES data analysis demonstrated the structure of the nanoparticles being similar to that of macroscopic maghemite. The Mossbauer spectroscopy revealed the γ-Fe2O3 phase of the nanoparticles and vibration magnetometry study showed that reactive oxygen species in HeLa cells are generated both in the cytoplasm and the nucleus. Conclusion Quasispherical Fe3+ SPIONs having the maghemite structure with the average size of 16 nm obtained by using the fast microwave synthesis technique are expected to be of great value for theranostic applications in oncology and multimodal anticancer therapy. PMID:28919740

Crystallization kinetics of the Cu{sub 50}Zr{sub 50} metallic glass under isothermal conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, Qian; Jian, Zengyun, E-mail: jianzengyun@xatu.edu.cn; Xu, Junfeng

2016-12-15

Amorphous structure of the melt-spun Cu{sub 50}Zr{sub 50} amorphous alloy ribbons were confirmed by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HR-TEM). Isothermal crystallization kinetics of these alloy ribbons were investigated using differential scanning calorimetry (DSC). Besides, Arrhenius and Johnson-Mehl-Avrami (JMA) equations were utilized to obtain the isothermal crystallization kinetic parameters. As shown in the results, the local activation energy E{sub α} decreases by a large margin at the crystallized volume fraction α<0.1, which proves that crystallization process is increasingly easy. In addition, the local activation energy E{sub α} is basically constant at 0.1

Study of irradiation induced surface pattern and structural changes in Inconel 718 alloy

NASA Astrophysics Data System (ADS)

Wan, Hao; Si, Naichao; Zhao, Zhenjiang; Wang, Jian; Zhang, Yifei

2018-05-01

Helium ions irradiation induced surface pattern and structural changes of Inconel 718 alloy were studied with the combined utilization of atomic force microscopy (AFM), x-ray diffraction (XRD) and transmission electron microscopy (TEM). In addition, SRIM-2013 software was used to calculate the sputtering yield and detailed collision events. The result shows that, irradiation dose play an important role in altering the pattern of the surface. Enhanced irradiation aggravated the surface etching and increased the surface roughness. In ion irradiated layer, large amount of interstitials, vacancies and defect sinks were produced. Moreover, in samples with increasing dose irradiation, the dependence of interplanar spacing variation due to point defects clustering on sink density was discussed.

Spectral characterization and white light generation by yttrium silicate nanopowders undoped and doped with Ytterbium(III) at different concentrations when excited by a laser diode at 975 nm

NASA Astrophysics Data System (ADS)

Cinkaya, Hatun; Eryurek, Gonul; Bilir, Gokhan; Collins, John; Di Bartolo, Baldassare

2017-01-01

We have studied nanophosphors of yttrium silicate (YSO) undoped and doped with different concentration of ytterbium (Yb3+) synthesized by using the sol-gel method. Structural and luminescence properties of the nanophosphors were studied experimentally by using different analytical techniques. For the structural analysis, we performed X-ray diffraction (XRD), Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectrometry (EDS) measurements. Upconversion (UC) and the white light (WL) emission properties were investigated by using the near infrared cw laser excitation of 975 nm. The spectral properties have been found to depend on several physical parameters.

Direct ultrasonic-assisted synthesis of sphere-like nanocrystals of spinel Co3O4 and Mn3O4.

PubMed

Askarinejad, Azadeh; Morsali, Ali

2009-01-01

A simple sonochemical method was developed to synthesize uniform sphere-like or cubic Co(3)O(4) and Mn(3)O(4) nanocrystals by using acetate salts and sodium hydroxide or tetramethylammonium hydroxide (TMAH) as precursors. Influence of some parameters such as time of reaction, alkali salts, and power of the ultrasound and the molar ratio of the starting materials on the size, morphology and degree of crystallinity of the products was studied. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), FTIR spectroscopy, Thermal gravimetry analysis and differential thermal analysis (TGA/DTA) were used to characterize the nanocrystals.

Green chemistry for the preparation of L-cysteine functionalized silver nanoflowers

NASA Astrophysics Data System (ADS)

Ma, Xinfu; Guo, Qingquan; Xie, Yu; Ma, Haixiang

2016-05-01

The preparation of size- and shape-controlled metallic nanostructures in an eco-friendly manner has been regarded as one of the key issues in nanoscience research today. In this paper, biosynthesis of silver nanoflowers (AgNFs) using L-cysteine as reducing and capping agent in alkaline solution via 70 °C water bath for 4 h has been demonstrated. The formation of L-cys-AgNPs was observed visually by color change of the samples. The prepared samples were characterized by UV-vis spectroscopy, Transmission electron microscopy (TEM) spectroscopy, X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). These results indicate that single-crystalline of AgNFs have been successfully synthesized.

Template-directed synthesis of MS (M=Cd, Zn) hollow microsphere via hydrothermal method

NASA Astrophysics Data System (ADS)

Wang, Shi-Ming; Wang, Qiong-Sheng; Wan, Qing-Li

2008-05-01

CdS, ZnS hollow microspheres were prepared with chitosan as the synthesis template at 140 and 150 °C, respectively, by hydrothermal method. The resultant products were characterized by X-ray diffraction (XRD) measurements in order to determine the crystalline phase of the products. The structural and morphological features of the nanoparticles were investigated by transmission electron microscopy (TEM) and ultraviolet-visible diffuse reflection spectroscopy (DRS). The experimental results indicated that all the nanoparticles aggregated into hollow microspheres and chitosan as a template played an important role in the formation of hollow microspheres. In addition, an intermediate complex structure-controlling possible reaction mechanism was proposed in this paper.

Efficient mechanochemical bifunctional nanocatalysts for the conversion of isoeugenol to vanillin

NASA Astrophysics Data System (ADS)

Ostovar, Somayeh; Franco, Ana; Puente-Santiago, Alain R.; Pinilla-de Dios, María; Rodríguez-Padrón, Daily; Shaterian, Hamid R.; Luque, Rafael

2018-04-01

A novel highly functionalized nanocatalyst composed of iron containing SBA-15 material modified with sulfonic acid groups was synthesized by a mechanochemical approach. A full characterization of the obtained nanoreactor was performed by N2 physisorption isotherms analysis, transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and Fourier-Infrared Spectroscopy (FT-IR). The mechanochemically synthesized nanocatalyst displays a high isoeugenol conversion to vanillin under mild conditions using H2O2 as oxidizing agent. Interestingly, this conversion resulted to be higher than that one obtained with the same material synthesized by an impregnation method. Additionally, the nanoreactor showed excellent reusability over four successive runs under the studied reaction conditions.

Synthesis and photocatalytic activity of N-doped TiO2 produced in a solid phase reaction

NASA Astrophysics Data System (ADS)

Xin, Gang; Pan, Hongfei; Chen, Dan; Zhang, Zhihua; Wen, Bin

2013-02-01

N-doped TiO2 was synthesized by calcining a mixture of titanic acid and graphitic carbon nitride (g-C3N4) at temperatures above 500 °C. The final samples were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), and UV-vis diffuse reflectance spectra. The photocatalytic activity of N-doped TiO2 was studied by assessing the degradation of methylene blue in an aqueous solution, under visible light and UV light irradiation. It was found that the N-doped TiO2 displayed higher photocatalytic activity than pure TiO2, under both visible and UV light.

Comparison of the morphology, chemical composition and microstructure of cryptocrystalline graphite and carbon black

NASA Astrophysics Data System (ADS)

Quan, Ying; Liu, Qinfu; Zhang, Shilong; Zhang, Shuai

2018-07-01

The structures of cryptocrystalline graphite (CG) and carbon black (CB) have been analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), organic elemental analysis (OEA), X-ray diffraction (XRD), RAMAN and high-resolution transmission electron microscopy (HRTEM). These results indicate that CG has the same elemental composition as CB, with carbon being the major element present. SL sample (CG with low graphitization degree) and CB exhibit similar microcrystalline structures. CG was shown to contain a layered graphitic structure that was significantly different to the primary spherical particles present in CB. It is proposed that these CG sheets may potentially be reduced and delaminated to afford multilayer graphene structures with improved material properties.

Green synthesis of gold nanoparticles using aspartame and their catalytic activity for p-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Wu, Shufen; Yan, Songjing; Qi, Wei; Huang, Renliang; Cui, Jing; Su, Rongxin; He, Zhimin

2015-05-01

We demonstrated a facile and environmental-friendly approach to form gold nanoparticles through the reduction of HAuCl4 by aspartame. The single-crystalline structure was illustrated by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The energy-dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FTIR) results indicated that aspartame played a pivotal role in the reduction and stabilization of the gold crystals. The crystals were stabilized through the successive hydrogen-bonding network constructed between the water and aspartame molecules. Additionally, gold nanoparticles synthesized through aspartame were shown to have good catalytic activity for the reduction of p-nitrophenol to p-aminophenol in the presence of NaBH4.

Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

NASA Astrophysics Data System (ADS)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

Growth of GaN@InGaN Core-Shell and Au-GaN Hybrid Nanostructures for Energy Applications

DOE PAGES

Kuykendall, Tevye; Aloni, Shaul; Jen-La Plante, Ilan; ...

2009-01-01

We demonstrated a method to control the bandgap energy of GaN nanowires by forming GaN@InGaN core-shell hybrid structures using metal organic chemical vapor deposition (MOCVD). Furthermore, we show the growth of Au nanoparticles on the surface of GaN nanowires in solution at room temperature. The work shown here is a first step toward engineering properties that are crucial for the rational design and synthesis of a new class of photocatalytic materials. The hybrid structures were characterized by various techniques, including photoluminescence (PL), energy dispersive x-ray spectroscopy (EDS), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD).

Solid state amorphization in the Al-Fe binary system during high energy milling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Urban, P., E-mail: purban@us.es; Montes, J. M.; Cintas, J.

2013-12-16

In the present study, mechanical alloying (MA) of Al75Fe25 elemental powders mixture was carried out in argon atmosphere, using a high energy attritor ball mill. The microstructure of the milled products at different stages of milling was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The results showed that the amorphous phase content increased by increasing the milling time, and after 50 hours the amorphization process became complete. Heating the samples resulted in the crystallization of the synthesized amorphous alloys and the appearance of the equilibrium intermetallic compounds Al{sub 5}Fe{submore » 2}.« less

Plasma in-liquid method for reduction of zinc oxide in zinc nanoparticle synthesis

NASA Astrophysics Data System (ADS)

Amaliyah, Novriany; Mukasa, Shinobu; Nomura, Shinfuku; Toyota, Hiromichi; Kitamae, Tomohide

2015-02-01

Metal air-batteries with high-energy density are expected to be increasingly applied in electric vehicles. This will require a method of recycling air batteries, and reduction of metal oxide by generating plasma in liquid has been proposed as a possible method. Microwave-induced plasma is generated in ethanol as a reducing agent in which zinc oxide is dispersed. Analysis by energy-dispersive x-ray spectrometry (EDS) and x-ray diffraction (XRD) reveals the reduction of zinc oxide. According to images by transmission electron microscopy (TEM), cubic and hexagonal metallic zinc particles are formed in sizes of 30 to 200 nm. Additionally, spherical fiber flocculates approximately 180 nm in diameter are present.

Structure and magnetic properties of Fe-doped ZnO prepared by the sol-gel method.

PubMed

Liu, Huilian; Yang, Jinghai; Zhang, Yongjun; Yang, Lili; Wei, Maobin; Ding, Xue

2009-04-08

Zn(0.97)Fe(0.03)O nanoparticles were synthesized by the sol-gel method. X-ray diffraction (XRD) and transmission electron microscope (TEM) analysis revealed that the samples had pure ZnO wurtzite structure and Fe ions were well incorporated into the ZnO crystal lattice. X-ray photoelectron spectroscopy (XPS) showed that both Fe(2+) and Fe(3+) existed in Zn(0.97)Fe(0.03)O. The result of x-ray absorption near-edge structure (XANES) further testified that Fe ions took the place of Zn sites in our samples. Magnetic measurements indicated that Zn(0.97)Fe(0.03)O was ferromagnetic at room temperature.

Crystalline phase transformation of colloidal cadmium sulfide nanocrystals

NASA Astrophysics Data System (ADS)

Ghali, M.; Eissa, A. M.; Mosaad, M. M.

2017-03-01

In this paper, we give a microscopic view concerning influence of the growth conditions on the physical properties of nanocrystals (NCs) thin films made of CdS, prepared using chemical bath deposition CBD technique. We show a crystalline phase transformation of CdS NCs from hexagonal wurtzite (W) structure to cubic zincblende (ZB) when the growth conditions change, particularly the solution pH values. This effect was confirmed using X-ray diffraction (XRD), transmission electron microscopy (TEM), optical absorption and photoluminescence (PL) measurements. The optical absorption spectra allow calculation of the bandgap value, Eg, where significant increase ˜200 meV in the CdS bandgap when transforming from Hexagonal to Cubic phase was found.

Water-assisted extrusion of bio-based PETG/clay nanocomposites

NASA Astrophysics Data System (ADS)

Lee, Naeun; Lee, Sangmook

2018-02-01

Bio-based polyethylene terephthalate glycol-modified (PETG)/clay nanocomposites were prepared using the water-assisted extrusion process. The effects of different types of clay and clay mixing methods (with or without the use of water) and the resulting nanocomposites properties were investigated by measuring the rheological and tensile properties and morphologies. The valuable properties were achieved when Cloisite 30B was mixed in a slurry state. The results of the X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies showed that the nano-clay was well dispersed within the PETG matrix. This shows that the slurry process could be an effective exfoliation method for many nanocomposites systems as well as for bio-based PETG/clay nanocomposites.

Formation of MoS2 inorganic fullerenes (IFs) by the reaction of MoO3 nanobelts and S.

PubMed

Li, Xiao Lin; Li, Ya Dong

2003-06-16

The reaction of MoO3 and S at temperatures higher than 300 degrees C in an argon atmosphere provides a convenient and effective method for the synthesis of MoS2 nanocrystalline substances. MoS2 nanotubes and fullerene-like nanoparticles have been obtained by the reaction at 850 degrees C under well-controlled conditions. The influences of reaction temperature and duration were carefully investigated in this paper. All of the nanostructures were characterized by Xray powder diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). A stepwise reaction model and rolling mechanism were proposed based on the experimental results.

Synthesis and electrochemical property of few-layer molybdenum disulfide nanosheets

NASA Astrophysics Data System (ADS)

Fu, Yanjue; Wang, Chunrui; Wang, Linlin; Peng, Xia; Wu, Binhe; Sun, Xingqu; Chen, Xiaoshuang

2016-12-01

Large-scale few-layer MoS2 nanosheets have been fabricated via a simple hydrothermal route using molybdenum powder as precursors. The as-prepared MoS2 samples were characterized by X-ray powder diffraction (XRD) analysis, transmission electron microscopy (TEM), and Raman and photoluminescence (PL) spectral analyses at room temperature. The results confirm that the as-prepared MoS2 displays a sheet-like morphology with a thickness of few (bi- to tri-) layers. Electrochemical measurements showed that the as-prepared few-layer MoS2 exhibited the highest reversible capacity of 1127 mAh g-1 and a stable reversible capacity of 1057 mAh g-1 after 30 cycles.

Synthesis, characterization and properties of L-arginine-passivated silver nanocolloids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sunatkari, A. L., E-mail: ashok.sunatkari@rediffmail.com; Talwatkar, S. S.; Tamgadge, Y. S.

2016-05-06

We investigate the effect of L-arginine-surface passivation on localised surface plasmon resonance (LSPR), size and stability of colloidal Silver Nanoparticles (AgNPs) synthesized by chemical reduction method. The surface Plasmon resonance absorption peak of AgNPs shows blue shift with the increase in L-arginine concentration. Transmission electron microscopy (TEM) analysis confirmed that the average size of AgNPs reduces from 10 nm to 6 nm as the concentration of L-Arginine increased from 1 to 5 mM. The X-ray diffraction study (XRD) confirmed the formation face-centred cubic (fcc) structured AgNPs. FT-IR studies revealed strong bonding between L-arginine functional groups and AgNPs.

Effects of Polyethylene Glycol and Citric Acid on Preparation and Hydrodechlorination Activity of Molybdenum Phosphide

NASA Astrophysics Data System (ADS)

Liu, Xiaomeng; Lu, Shaoxiang; Xu, Hanghui; Ren, Lili

2018-07-01

Molybdenum phosphide (MoP), modified by polyethylene glycol (PEG) and citric acid (CA), exhibited 2 to 3 times superior activity than the MoP modified by CA alone. And the optimal activity temperature was reduced from 500 to 450oC. The catalyst was fully characterized by a variety of techniques including X-ray diffraction (XRD), N2 adsorption-desorption isotherm, scanning electron microscopy (SEM), transmission electron microscopy (TEM). The results showed that the addition of PEG and CA increased the surface area of MoP and decreased the particle size of MoP. Furthermore, the reaction mechanism also has been discussed by combining the activity data and characterization results.

Amino acid-assisted synthesis of zinc oxide nanostructures

NASA Astrophysics Data System (ADS)

Singh, Baljinder; Moudgil, Lovika; Singh, Gurinder; Kaura, Aman

2018-05-01

In this manuscript we have used experimental approach that can provide a fundamental knowledge about the role played by biomolecules in designing the shape of nanostructure (NS) at a microscopic level. The three different amino acids (AAs) - Arginine (Arg), Aspartic acid (Asp) and Histidine (His) coated Zinc oxide (ZnO) NSs to explain the growth mechanism of nanoparticles of different shapes. Based on the experimental methodology we propose that AA-ZnO (Asp and Arg) nanomaterials could form of rod like configuration and His-ZnO NPs could form tablet like configuration. The synthesized samples are characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Results reveal that AAs are responsible for formation of different NSs

Structural characterizations of pure SnS and In-doped SnS thin films using isotropic and anisotropic models

NASA Astrophysics Data System (ADS)

Kafashan, Hosein

2018-04-01

An electrochemical route has been employed to prepare pure SnS and indium-doped SnS thin films. Six samples including undoped SnS and In-doped SnS thin films deposited on the fluorine-doped tin oxide (FTO) glass substrates. An aqueous solution having SnCl2 and Na2S2O3 used as the primary electrolyte. Different In-doped SnS samples were prepared by adding a different amount of 1 mM InCl3 solution into the first electrolyte. The applied potential (E), time of deposition (t), pH and bath temperature (T) were kept at ‑1 V, 30 min, 2.1 and 60 °C, respectively. For all samples, except the In-dopant concentration, all the deposition parameters are the same. After preparation, X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) with an energy dispersive X-ray analyzer (EDX) attachment, atomic force microscopy (AFM), and transmission electron microscopy (TEM) were used to determine structural properties of as-deposited films. XRD patterns revealed that the synthesized undoped- and In-doped SnS thin films were crystallized in the orthorhombic structure. The shape of SnS crystals was spherical in the TEM image. X-ray peak broadening studies was done by applying Scherrer’s method, Williamson-Hall (W–H) models (including uniform deformation model (UDM), uniform strain deformation model (UDSM), and uniform deformation energy density model (UDEDM)), and size-strain plot (SSP) method. Using these techniques, the crystallite size and the lattice strains have been predicted. There was a good agreement in the particle size achieved by W–H- and SSP methods with TEM image.

Magnetically recyclable Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O nano-photocatalyst: structural, optical, magnetic and photocatalytic properties.

PubMed

Qasim, Mohd; Asghar, Khushnuma; Singh, Braj Raj; Prathapani, Sateesh; Khan, Wasi; Naqvi, A H; Das, Dibakar

2015-02-25

A novel visible light active and magnetically separable nanophotocatalyst, Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O (denoted as NZF@Z), with varying amount of Ni0.5Zn0.5Fe2O4, has been synthesized by egg albumen assisted sol gel technique. The structural, optical, magnetic, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), fourier transform infrared spectroscopy (FTIR), UV-visible (UV-Vis) spectroscopy, and vibrating sample magnetometry (VSM) techniques. Powder XRD, TEM, FTIR and energy dispersive spectroscopic (EDS) analyses confirm coexistence of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O phases in the catalyst. Crystallite sizes of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O in pure phases and nanocomposites, estimated from Debye-Scherrer equation, are found to be around 15-25 nm. The estimated particle sizes from TEM and FESEM data are ∼(22±6) nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra, of Zn0.95Ni0.05O, 15%NZF@Z, 40%NZF@Z and 60%NZF@Z are 2.95, 2.72, 2.64, and 2.54 eV respectively. Magnetic measurements (field (H) dependent magnetization (M)) show all samples to be super-paramagnetic in nature and saturation magnetizations (Ms) decrease with decreasing ferrite content in the nanocomposites. These novel nanocomposites show excellent photocatalytic activities on Rhodamin Dye. Copyright © 2014 Elsevier B.V. All rights reserved.

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

NASA Astrophysics Data System (ADS)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.

A study on the stability and green synthesis of silver nanoparticles using Ziziphora tenuior (Zt) extract at room temperature.

PubMed

Sadeghi, Babak; Gholamhoseinpoor, F

2015-01-05

Biomolecules present in plant extracts can be used to reduce metal ions to nanoparticles in a single-step green synthesis process. This biogenic reduction of metal ion to base metal is quite rapid, readily conducted at room temperature and pressure, and easily scaled up. Mediated Synthesis by plant extracts is environmentally benign. The involved reducing agents include the various water soluble plant metabolites (e.g. alkaloids, phenolic compounds, terpenoids) and co-enzymes. Silver (Ag) nanoparticles have the particular focus of plant-based syntheses. Extracts of a diverse range of Ziziphora tenuior (Zt) have been successfully used in making nanoparticles. The aim of this study was to investigate the antioxidant properties of this plant and its ability to synthesize silver nanoparticles. Z.tenuior leaves were used to prepare the aqueous extract for this study. Silver nanoparticles were characterized with different techniques such as UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), Scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 8 to 40 nm. FT-IR spectroscopy revealed that silver nanoparticles were functionalized with biomolecules that have primary amine group (NH₂), carbonyl group, -OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of silver nanoparticles with size of 38 nm. In addition to plant extracts, live plants can be used for the synthesis. Here were view the methods of making nanoparticles using plant extracts. The scanning electron microscopy (SEM) implies the right of forming silver nanoparticles. The results of TEM, SEM, FT-IR, UV-VIS and XRD confirm that the leaves extract of Zt can synthesis silver nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Flower-like NiO structures: Controlled hydrothermal synthesis and electrochemical characteristic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chai, Hui; Chen, Xuan; Key Laboratory of Advanced Functional Materials, Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, Xinjiang

Graphical abstract: Flower-like porous NiO was obtained via thermal decomposition of the precursor prepared by a hydrothermal process using hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results of electrochemical measurements demonstrated that the flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials of electrochemical capacitors (ECs), which may be attributed to the unique microstrcture of NiO. Data analyses indicated that NiO with novel porousmore » structure attractive for practical and large-scale applications in electrochemical capacitors. Display Omitted Highlights: ► Synthesis and characterization of NiO with novel porous structure is presented in this work. ► The electrochemical performance of product was examined. ► NiO with excellent performance as electrode materials may be due to the unique microstrcture. ► NiO with novel porous structure attractive for practical with high capacity (340 F g{sup −1}). -- Abstract: Flower-like porous NiO was obtained by thermal decomposition of the precursor prepared by a hydrothermal process with hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resulting structures of NiO exhibited porous like petal building blocks. The electrochemical measurements’ results demonstrated that flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials for electrochemical capacitors, which may be attributed to the unique structure of NiO. The results indicated that NiO with novel porous structure has been attractive for practical and large-scale applications in electrochemical capacitors.« less

Hydrothermal synthesis of highly crystalline RuS{sub 2} nanoparticles as cathodic catalysts in the methanol fuel cell and hydrochloric acid electrolysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Yanjuan; College of Material Science and Engineering, Key Laboratory of Automobile Materials of Ministry of Education, Jilin University, 2699 Qianjin Street, Changchun 130012; Li, Nan, E-mail: lin@jlu.edu.cn

2015-05-15

Highlights: • Highly crystalline RuS{sub 2} nanoparticles have been first synthesized by a “one-step” hydrothermal method. • The product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} with average particle size of 14.8 nm. • RuS{sub 2} nanoparticles were used as cathodic catalysts in methanol fuel cell and hydrochloric acid electrolysis. • The catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}. - Abstract: Highly crystalline ruthenium sulfide (RuS{sub 2}) nanoparticles have been first synthesized by a “one-step” hydrothermal method at 400 °C, using ruthenium chloride and thiourea as reactants. The products were characterized bymore » powder X-ray diffraction (XRD), scanning electron microscopy/energy disperse spectroscopy (SEM/EDS), thermo gravimetric-differential thermal analyze (TG-DTA), transmission electron microscopy equipped with selected area electron diffraction (TEM/SAED). Fourier transform infrared spectra (IR), and X-ray photoelectron spectroscopy (XPS). XRD result illustrates that the highly crystalline product presents a pure cubic phase of stoichiometric ratio RuS{sub 2} and the average particle size is 14.8 nm. SEM and TEM images display the products have irregular shape of 6–25 nm. XPS analyst indicates that the sulfur exists in the form of S{sub 2}{sup 2−}. Cyclic voltammetry (CV), rotating disk electrode (RDE), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) measurements are conducted to evaluate the electrocatalytic activity and stability of the highly crystalline RuS{sub 2} nanoparticles in oxygen reduction reaction (ORR) for methanol fuel cell and hydrochloric acid electrolysis. The results illustrate that RuS{sub 2} is active towards oxygen reduction reaction. Although the activity of RuS{sub 2} is lower than that of Pt/C, the RuS{sub 2} catalyst outperforms commercial Pt/C in methanol tolerance and stability towards Cl{sup −}.« less

Structural, molecular orbital and optical characterizations of solvatochromic mixed ligand copper(II) complex of 5,5-Dimethyl cyclohexanate 1,3-dione and N,N,N',N'N″-pentamethyldiethylenetriamine.

PubMed

Taha, A; Farag, A A M; Ammar, A H; Ahmed, H M

2014-03-25

In this work, a new solvatochromic mononuclear mixed ligand complex with the formula, Cu(DMCHD)(Me5dien)NO3 (where, DMCHD=5,5-Dimethyl cyclohexanate 1,3-dione and (Me5dien)=N,N,N',N'N″-pentamethyldiethylenetriamine was synthesized and characterized by analytical, spectral, magnetic, molar conductance, thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and transmission electron microscope (TEM) measurements. The formation constant-value for copper (II)-DMCHD was found to be much lower than the expected for similar β-diketones, revealing monobasic unidentate nature of this ligand. The d-d absorption bands of the prepared complex exhibit a color changes in various solvent (solvatochromic). Specific and non-specific interactions of solvent molecules with the complex were investigated using Multi Parametric Linear Regression Analysis (MLRA). Structural parameters of the free ligands and their Cu (II) - complex were calculated on the basis of semi-empirical PM3 level and compared with the experimental data. The crystallite size and morphology of Cu(DMCHD)(Me5dien)NO3 were examined using XRD analysis and TEM, revealing that the complex is well crystalline and correspond to the monoclinic crystal structure. The lattice strain and mean crystallite size were estimated by Williamson-Hall (W-H) plot using X-ray diffraction data. The main important absorption parameters such as extinction molar coefficient, oscillator strength and electric dipole strength of the principal optical transitions in the UV-Vis region were calculated. The analysis of absorption coefficient near the fundamental absorption edge reveals that the optical band gaps are direct allowed transitions with values of 2.78 eV and 3.59 eV. The present copper (II) complex was screened for its antimicrobial activity against Staphylococcus Aureus and Bacillus Subtilis as Gram-positive bacteria, Escherichia Coli and Salmonella Typhimurium as Gram-negative bacteria and Candida Albicans as fungus strain. Copyright © 2013 Elsevier B.V. All rights reserved.

Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates.

PubMed

Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

2015-03-20

Inspired by coralline-derived hydroxyapatite, we designed a methodological route to synthesize carbonated-hydroxyapatite microspheres from the conversion of CaCO3 spherulite templates within a collagen matrix under mild conditions and thus constructed the composite hydrogel of collagen/hydroxyapatite-microspheres. Fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) were employed to confirm the successful generation of the carbonated hydroxyapatite phase originating from CaCO3, and the ratios of calcium to phosphate were tracked over time. Variations in the weight portion of the components in the hybrid gels before and after the phase transformation of the CaCO3 templates were identified via thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) shows these composite hydrogels have a unique multiscale microstructure consisting of a collagen nanofibril network and hydroxyapatite microspheres. The relationship between the hydroxyapatite nanocrystals and the collagen fibrils was revealed by transmission electron microscopy (TEM) in detail, and the selected area electron diffraction (SAED) pattern further confirmed the results of the XRD analyses which show the typical low crystallinity of the generated hydroxyapatite. This smart synthesis strategy achieved the simultaneous construction of microscale hydroxyapatite particles and collagen fibrillar hydrogel, and appears to provide a novel route to explore an advanced functional hydrogel materials with promising potentials for applications in bone tissue engineering and reconstruction medicine.

Synthesis of AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) alloy powders by mechanical alloying

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maulik, Ornov; Kumar, Vinod, E-mail: vkt.meta@mnit.ac.in; Adjunct Faculty, Materials Research Centre, Malaviya National Institute of Technology, Jaipur 302017

2015-12-15

Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7 mol) high-entropy alloys (HEAs) were synthesized by mechanical alloying. The effect of Mg content on the phase evolution of HEAs was investigated using X-Ray diffractometry (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) pattern analysis. The particle morphology and composition of HEAs were investigated by scanning electron microscopy (SEM). Thermodynamic parameters were calculated and analyzed to explain the formation of a solid solution. XRD analysis revealed BCC as major phase and FCC as a minor phase in as-milled AlFeCuCr and AlFeCuCrMg{sub 0.5} HEAs. Also, XRD analysis of as-milledmore » AlFeCuCrMg, AlFeCuCrMg{sub 1.7} confirmed the formation of two BCC phases (BCC 1 and BCC 2). TEM–SAED analysis of AlFeCuCrMg{sub x} HEAs concurred with XRD results. Microstructural features and mechanism for solid solution formation have been conferred in detail. Phase formation of the present HEAs has been correlated with calculated thermodynamic parameters. Differential thermal analysis (TGA-DTA) of these alloys confirmed that there is no substantial phase change up to 500 °C. - Highlights: • Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) HEAs were prepared by mechanical alloying. • Phase evolution and lattice parameter were studied by X-Ray Diffraction. • Crystallite size and lattice microstrain calculated failed to obey the Williamson–Hall method. • Criterions for formation of simple solid solution were compared to the thermodynamic parameters of the present HEAs. • Increase in the Mg concentration in AlMg{sub x}FeCuCr (x = 0, 0.5, 1, 1.7) HEAs supports the formation of BCC phase.« less

Process Parameters on the Crystallization and Morphology of Hydroxyapatite Powders Prepared by a Hydrolysis Method

NASA Astrophysics Data System (ADS)

Wang, Moo-Chin; Hon, Min-Hsiung; Chen, Hui-Ting; Yen, Feng-Lin; Hung, I.-Ming; Ko, Horng-Huey; Shih, Wei-Jen

2013-07-01

The effects of process parameters on the crystallization and morphology of hydroxyapatite (Ca10(PO4)6(OH)2, HA) powders synthesized from dicalcium phosphate dihydrate (CaHPO4·2H2O, DCPD) using a hydrolysis method have been investigated. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were used to characterize the synthesized powders. When DCPD underwent hydrolysis in 2.5 NaOH solution (Na(aq)) at 303 K to 348 K (30 °C to 75 °C) for 1 hour, the XRD results revealed that HA was obtained for all the as-dried samples. The SEM morphology of the HA powders for DCPD hydrolysis produced at 348 K (75 °C) shows regular alignment and a short rod shape with a size of 200 nm in length and 50 nm in width. With DCPD hydrolysis in 2.5 M NaOH(aq) holding at 348 K (75 °C) for 1 to 24 hours, XRD results demonstrated that all samples were HA and no other phases could be detected. Moreover, the XRD results also show that all the as-dried powders still maintained the HA structure when DCPD underwent hydrolysis in 0.1 to 5 M NaOH(aq) at 348 K (75 °C) for 1 hour. Otherwise, the full transformation from HA to octa-calcium phosphate (OCP, Ca8H2(PO4)6·5H2O) occurred when hydrolysis happened in 10 M NaOH(aq). FT-IR spectra analysis revealed that some carbonated HA (Ca10(PO4)6(CO3), CHA) had formed. The SEM morphology results show that the 60 to 65 nm width of the uniformly long rods with regular alignment formed in the HA powder aggregates when DCPD underwent hydrolysis in 2.5 M NaOH(aq) at 348 K (75 °C) for 1 hour.

The green synthesis of Ag/ZnO in montmorillonite with enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Sohrabnezhad, Sh.; Seifi, A.

2016-11-01

The Ag/ZnO-MMT nanocomposite was prepared using urtica dioica leaf extract. To improve the photocatalytic properties of ZnO-MMT nanocomposite, silver metal nanoparticles was deposited over nanocomposite. Zn(CH3COO)2, AgNO3 and Urtica dioica leaf extract were used as a zinc, silver precursor and reducing agent, respectively. The nanocomposite was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and ultraviolet-visible diffuse reflectance spectroscopy (DRS). The powder X-ray diffraction showed that Ag/ZnO nanoparticles located on the surface MMT layers. The diffuse reflectance spectra of nanocomposite indicated a strong surface plasmon resonance (SPR) absorption band in the visible region, resulting from metallic Ag nanoparticles. TEM image demonstrated the presence of silver nanoparticles with an average size of 2-4 nm over both MMT and flower-shape ZnO. The photocatalytic activity of nanocomposite was studied for destructive reaction methylene blue dye under visible light. In addition, the effects of different parameters such as amount of nanocomposite, concentration of the dye and pH of the solution were studied. The results showed that modiffication of ZnO-MMT nanocomposite with silver nanoparticles increased the percentage of discoloration methylene blue (MB) from 38.95 to 91.95. MMT matrix showed an important role in the reduction of recombination of electron-hole in nanocomposite.

Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

PubMed

Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

2017-02-01

In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

Laser ablation of Au-CuO core-shell nanocomposite in water for optoelectronic devices

NASA Astrophysics Data System (ADS)

Ismail, Raid A.; Abdul-Hamed, Ryam S.

2017-12-01

Core-shell gold-copper oxide Au-CuO nanocomposites were synthesized using laser ablation of CuO target in colloidal solution of Au nanoparticles (NPs). The effect of laser fluence on the structural, morphological, electrical, and optical properties of Au-CuO nanocomposites was investigated using x-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM), transmission electron microscope (TEM), photoluminescence (PL), Fourier transformed infrared spectroscopy (FTIR), Hall measurement, and UV-vis spectroscopy. X-ray diffraction results confirm the formation of polycrystalline Au-CuO NPs with monoclinic structure. The optical energy gap for CuO was 4 eV and for the Au-CuO core-shell nanocomposites was found to be in the range of 3.4-3.7 eV. SEM and TEM investigations revealed that the structure and morphology of Au-CuO core-shell nanocomposites were strongly depending on the laser fluence. A formation of Au-CuO nanospheres and platelets structures was observed. The photoluminescence data showed an emission of broad visible peaks between 407 and 420 nm. The effect of laser fluence on the dark and illuminated I-V characteristics of Au-CuO/n-Si heterojunction photodetectors was investigated and analyzed. The experimental data demonstrated that the photodetector prepared at optimum laser fluence exhibited photosensitivity of 0.6 AW-1 at 800 nm.

Improving the oxidation resistance and stability of Ag nanoparticles by coating with multilayered reduced graphene oxide

NASA Astrophysics Data System (ADS)

Li, Yahui; Zhang, Huayu; Wu, Bowen; Guo, Zhuo

2017-12-01

A kind of coating nanostructure, Ag nanoparticles coated with multilayered reduced graphene oxide (RGO), is fabricated by employing a three-step reduction method in an orderly manner, which is significantly different from the conventional structures that are simply depositing or doping with Ag nanoparticles on RGO via chemical reduction. The as-prepared nanostructure is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SEAD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The results show that the obtained Ag/RGO nanostructure is observed to be a perfect coating structure with well dispersed Ag particles, which is responsible for the remarkable oxidation resistance. The results of XPS spectra indicate the content of metallic Ag is far greater than that of Ag oxides despite of prolonged exposure to the air, which fully demonstrate the excellent stability of thus coating nanostructure.

Ultrasonic irradiation-assisted synthesis of Bi2S3 nanoparticles in aqueous ionic liquid at ambient condition.

PubMed

de la Parra-Arciniega, Salomé M; Garcia-Gomez, Nora A; Garza-Tovar, Lorena L; García-Gutiérrez, Domingo I; Sánchez, Eduardo M

2017-05-01

In this work, an easy, fast and environmentally friendly method to obtain Bi 2 S 3 nanostructures with sphere-like morphology is introduced. The promising material was successfully synthesized by a sonochemical route in 20% 1-ethyl-3-methylimidazolium ethyl sulfate [EMIM][EtSO 4 ] ionic liquid solution (IL). Morphological studies by electron microscopy (SEM and TEM) show that the use of IL in the synthesis of Bi 2 S 3 favors the formation of nanocrystals non-agglomerated. Micro Raman and energy dispersive X-ray spectroscopy (EDXS) were used to determine the composition and purity of the synthesized material. X-ray powder diffraction (XRD) and selective area electron diffraction (SAED) revealed that ultrasonic radiation accelerated the crystallization of Bi 2 S 3 into orthorhombic bismuthinite structure. The band gap calculated from the diffuse reflectance spectra (DRS) was found to be 1.5eV. Copyright © 2016 Elsevier B.V. All rights reserved.

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Electron backscatter diffraction analysis of gold nanoparticles on Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bochmann, A.; Teichert, S., E-mail: steffen.teichert@fh-jena.de; Katzer, C.

2015-06-07

It has been shown recently that the incorporation of gold nanoparticles into Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ} enhances the superconducting properties of this material in a significant way. Previous XRD and TEM investigations suggest different crystallographic relations of the gold nanoparticles with respect to the epitaxial Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ}. Here, detailed investigations of the crystal orientations for a large ensemble of gold nanoparticles with electron backscatter diffraction are reported. The average size of the gold nanoparticles is in the range of 60 nm–80 nm. We identified five different types of heteroepitaxial relationships between the gold nanoparticles and the superconductor film,more » resulting in complex pole figures. The observed different types of crystallographic orientations are discussed based on good lattice matching and the formation of low energy interfaces.« less

Facile synthesis of hollow Co3O4 microspheres and its use as a rapid responsive CL sensor of combustible gases.

PubMed

Teng, Fei; Yao, Wenqing; Zheng, Youfei; Ma, Yutao; Xu, Tongguang; Gao, Guizhi; Liang, Shuhui; Teng, Yang; Zhu, Yongfa

2008-09-15

The hollow Co(3)O(4) microspheres (HCMs) were prepared by the carbonaceous templates, which did not need the surface pretreatment. The chemiluminescence (CL) and catalytic properties for CO oxidation over these hollow samples were evaluated. The samples were characterized by scanning electron microscopy (SEM), energy disperse spectra (EDS), transmission electron microscopy (TEM), selected area electron diffraction (ED), X-ray diffraction (XRD), temperature-programmed desorption (TPD) and N(2) adsorption. The influences of filter' band length, flow rate of gas, test temperature, and particle structure on CL intensities were mainly investigated. It was found that compared with the solid Co(3)O(4) particles (SCPs), HCMs had a stronger CL intensity, which was ascribed to its hollow structure; and that CL properties of the catalysts were well correlated with their reaction activities. Moreover, HCMs were used to fabricate a highly sensitive gas detector, which is a rapid and effective method for the selection of catalysts or the detection of environmental deleterious gases.

Characterization of sodium phenytoin co-gelled with titania for a controlled drug-release system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lopez, T.; Instituto Nacional de Neurologia y Neurocirugia 'MVS', Av. Insurgentes Sur 3877. Col. La Fama. P.O. Box 14269 Mexico D. F.; Quintana, P.

2007-08-15

Sodium phenytoin, C{sub 15}H{sub 11}N{sub 2}NaO{sub 2}, in several concentrations was co-gelled with titania (TiO{sub 2}), by a sol-gel process. This technique is a promising method to encapsulate several drugs, in this case, phenytoin is an anticonvulsant used to control epileptic seizures. Samples were prepared by adding different concentrations (X = 50, 100, 200 and 250 mg per 20 g of titania matrix) of sodium phenytoin (Ph) to a solution of titanium n-butoxide. The resulting titania-Ph-X materials were characterized by transmission electron microscopy (TEM), Fourier transformed infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and Brunauer-Emmet-Teller (BET) surface areas. The porous nanomaterialsmore » showed a wide range of particle size, from 10 to 210 nm, with a mean pore diameter of 5 nm. X-ray diffraction showed an amorphous structure of the prepared samples.« less

Synthesis of boron nitride nanostructures from catalyst of iron compounds via thermal chemical vapor deposition technique

NASA Astrophysics Data System (ADS)

da Silva, Wellington M.; Ribeiro, Hélio; Ferreira, Tiago H.; Ladeira, Luiz O.; Sousa, Edésia M. B.

2017-05-01

For the first time, patterned growth of boron nitride nanostructures (BNNs) is achieved by thermal chemical vapor deposition (TCVD) technique at 1150 °C using a mixture of FeS/Fe2O3 catalyst supported in alumina nanostructured, boron amorphous and ammonia (NH3) as reagent gas. This innovative catalyst was synthesized in our laboratory and systematically characterized. The materials were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The X-ray diffraction profile of the synthesized catalyst indicates the coexistence of three different crystal structures showing the presence of a cubic structure of iron oxide and iron sulfide besides the gamma alumina (γ) phase. The results show that boron nitride bamboo-like nanotubes (BNNTs) and hexagonal boron nitride (h-BN) nanosheets were successfully synthesized. Furthermore, the important contribution of this work is the manufacture of BNNs from FeS/Fe2O3 mixture.

Fabrication and characterization of morphology-tuned single-crystal monodisperse Fe3O4 nanocrystals

NASA Astrophysics Data System (ADS)

Yu, Xuegang; Shan, Yan; Chen, Kezheng

2018-05-01

Monodisperse Fe3O4 nanocrystals with different size and morphology have been successfully fabricated by a facile high temperature reflow method. The presented materials were characterized by X-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, transmission electron microscope (TEM), selection area electron diffraction (SAED) and magnetic property measurement system (MPMS). The results showed that the as-prepared materials have face-centered cubic structures. Oleic acid plays a key role in the dispersion of Fe3O4 nanocrystals. The cubic and octahedral nanocrystals are enclosed by {1 0 0} and {1 1 1} lattice planes. The MPMS measurements show that magnetic properties are closely related to the sizes of the materials, and there is a stronger dipolar interaction between Fe3O4 nanocrystals with larger sizes. The controllable magnetic property and good dispersion endow the as-synthesized materials with great potential applications in magnetic fluid fields including sealing, medical equipment, mineral processing and other aspects.

CMC-coated Fe3O4 nanoparticles as new MRI probes for hepatocellular carcinoma

NASA Astrophysics Data System (ADS)

Sitthichai, Sudarat; Pilapong, Chalermchai; Thongtem, Titipun; Thongtem, Somchai

2015-11-01

Pure Fe3O4 nanoparticles and Fe3O4 magnetic nanoparticles (MNPs) coated with carboxymethyl cellulose (CMC) were successfully prepared by co-precipitating of FeCl2·4H2O and FeCl3·6H2O in the solutions containing ammonia at 80 °C for 3 h. Phase, morphology, particle-sized distribution, surface chemistry, and weight loss were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) including high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), thermogravimetric analysis (TGA), and Fourier transform infrared (FTIR) spectroscopy. In this research, CMC-coated Fe3O4 MNPs consisting of Fe2+ and Fe3+ ions with 543.3-mM-1 s-1 high relaxivity were detected and were able to be used for magnetic resonance imaging (MRI) application with very good contrast for targeting hepatocellular carcinoma (HCC) without any further vectorization.

In situ Studies of Phase Evolution in (Pr 1-x Nd x) 2 NiO 4 Electrodes with Various Interlayer Chemistries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dogdibegovic, Emir; Alabri, Nawf Saif; Wright, Christopher J.

The interest in Pr2NiO4 (PNO) electrode stems from the necessity to develop active and stable oxygen electrodes (1-6) for solid oxide fuel cells (SOFCs) (7-9). PNO is known for its highly active nature (7,8,10), originating from its superior oxygen ion diffusion, surface exchange coefficient (2,7,9-11) and structural flexibility over a wide temperature region (from 500 to 900oC) (3,12). PNO electrode, however, does undergo structural evolution to form a higher order phase (Pr3Ni2O7) and Pr6O11 (PrOx) (8). The structural change has been a major concern because it possibly links with the performance degradation over long-term operation (7,8) Conventional x-ray diffraction (XRD)more » has been extensively used to investigate the structural evolution in nickelates in the form of powders or planar electrodes (8,10). This method has two major limitations due to its low flux and low resolution: (1) it might overlook the presence of additional phases in the system, which is especially true for praseodymium nickelates where XRD diffraction patterns of higher order phase(s) (e.g. Pr3Ni2O7) may overlap with the parent PNO phase, making quantification challenging (8); and (2) the quantification of phase evolution in electrochemically operated PNO electrode may show major structural change with almost 100% of the parent phase transition from the conventional XRD analysis, while the transmission electron microscopy (TEM) studies clearly show the regions of preserved PNO phase (7).« less

In situ Studies of Phase Evolution in (Pr1-xNdx)2NiO4 Electrodes with Various Interlayer Chemistries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dogdibegovic, Emir; Alabri, Nawf S.; Wright, Christopher J.

2017-07-24

The interest in Pr2NiO4 (PNO) electrode stems from the necessity to develop active and stable oxygen electrodes (1-6) for solid oxide fuel cells (SOFCs) (7-9). PNO is known for its highly active nature (7,8,10), originating from its superior oxygen ion diffusion, surface exchange coefficient (2,7,9-11) and structural flexibility over a wide temperature region (from 500 to 900oC) (3,12). PNO electrode, however, does undergo structural evolution to form a higher order phase (Pr3Ni2O7) and Pr6O11 (PrOx) (8). The structural change has been a major concern because it possibly links with the performance degradation over long-term operation (7,8) Conventional x-ray diffraction (XRD)more » has been extensively used to investigate the structural evolution in nickelates in the form of powders or planar electrodes (8,10). This method has two major limitations due to its low flux and low resolution: (1) it might overlook the presence of additional phases in the system, which is especially true for praseodymium nickelates where XRD diffraction patterns of higher order phase(s) (e.g. Pr3Ni2O7) may overlap with the parent PNO phase, making quantification challenging (8); and (2) the quantification of phase evolution in electrochemically operated PNO electrode may show major structural change with almost 100% of the parent phase transition from the conventional XRD analysis, while the transmission electron microscopy (TEM) studies clearly show the regions of preserved PNO phase (7).« less

Carbon nanotubes/magnetite hybrids prepared by a facile synthesis process and their magnetic properties

NASA Astrophysics Data System (ADS)

Zhang, Li; Ni, Qing-Qing; Natsuki, Toshiaki; Fu, Yaqin

2009-07-01

In this paper, a facile synthesis process is proposed to prepare multiwalled carbon nanotubes/magnetite (MWCNTs/Fe 3O 4) hybrids. The process involves two steps: (1) water-soluble CNTs are synthesized by one-pot modification using potassium persulfate (KPS) as oxidant. (2) Fe 3O 4 is assembled along the treated CNTs by employing a facile hydrothermal process with the presence of hydrazine hydrate as the mineralizer. The treated CNTs can be easily dispersed in aqueous solvent. Moreover, X-ray photoelectron spectroscopy (XPS) analysis reveals that several functional groups such as potassium carboxylate (-COOK), carbonyl (-C dbnd O) and hydroxyl (-C-OH) groups are formed on the nanotube surfaces. The MWCNTs/Fe 3O 4 hybrids are characterized with respect to crystal structure, morphology, element composition and magnetic property by X-ray diffraction (XRD), transmission electron microscopy (TEM), XPS and superconducting quantum interference device (SQUID) magnetometer. XRD and TEM results show that the Fe 3O 4 nanoparticles with diameter in the range of 20-60 nm were firmly assembled on the nanotube surface. The magnetic property investigation indicated that the CNTs/Fe 3O 4 hybrids exhibit a ferromagnetic behavior and possess a saturation magnetization of 32.2 emu/g. Further investigation indicates that the size of assembled Fe 3O 4 nanoparticles can be turned by varying experiment factors. Moreover, a probable growth mechanism for the preparation of CNTs/Fe 3O 4 hybrids was discussed.

Green synthesis of silver nanoparticles using Cordia dichotoma fruit extract and its enhanced antibacterial, anti-biofilm and photo catalytic activity

NASA Astrophysics Data System (ADS)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.

Understanding the Magnesiothermic Reduction Mechanism of TiO2 to Produce Ti

NASA Astrophysics Data System (ADS)

Choi, Kyunsuk; Choi, Hanshin; Sohn, Il

2017-04-01

Titanium dioxide (TiO2) powders in the mineral form of rutile were reduced to metallic and an intermediate phase via a magnesiothermic reaction in molten Mg at temperatures between 973 K and 1173 K (700 °C and 900 °C) under high-purity Ar atmosphere. The reaction behavior and pathway indicated intermediate phase formation during the magnesiothermic reduction of TiO2 using XRD (X-ray diffraction), SEM (scanning electron microscope), and TEM (transmission electron microscope). Mg/TiO2 = 2 resulted in various intermediate phases of oxygen containing titanium, including Ti6O, Ti3O, and Ti2O, with metallic Ti present. MgTi2O4 ternary intermediate phases could also be observed, but they were dependent on the excess Mg present in the sample. Nevertheless, even with excessive amounts of Mg at Mg/TiO2 = 10, complete reduction to metallic Ti could not be obtained and some Ti6O intermediate phases were present. Although thermodynamics do not predict the formation of the MgTi2O4 spinel phase, detailed phase identification through XRD, SEM, and TEM showed significant amounts of this intermediate ternary phase even at excess Mg additions. Considering the stepwise reduction of TiO2 by Mg and the pronounced amounts of MgTi2O4 phase observed, the rate-limiting reaction is likely the reduction of MgTi2O4 to the TitO phase. Thus, an additional reduction step beyond thermodynamic predictions was developed.

Electronic properties and morphology of copper oxide/n-type silicon heterostructures

NASA Astrophysics Data System (ADS)

Lindberg, P. F.; Gorantla, S. M.; Gunnæs, A. E.; Svensson, B. G.; Monakhov, E. V.

2017-08-01

Silicon-based tandem heterojunction solar cells utilizing cuprous oxide (Cu2O) as the top absorber layer show promise for high-efficiency conversion and low production cost. In the present study, single phase Cu2O films have been realized on n-type Si substrates by reactive magnetron sputtering at 400 °C. The obtained Cu2O/Si heterostructures have subsequently been heat treated at temperatures in the 400-700 °C range in Ar flow and extensively characterized by x-ray diffraction (XRD) measurements, transmission electron microscopy (TEM) imaging and electrical techniques. The Cu2O/Si heterojunction exhibits a current rectification of ~5 orders of magnitude between forward and reverse bias voltages. High resolution cross-sectional TEM-images show the presence of a ~2 nm thick interfacial SiO2 layer between Cu2O and the Si substrate. Heat treatments below 550 °C result in gradual improvement of crystallinity, indicated by XRD. At and above 550 °C, partial phase transition to cupric oxide (CuO) occurs followed by a complete transition at 700 °C. No increase or decrease of the SiO2 layer is observed after the heat treatment at 550 °C. Finally, a thin Cu-silicide layer (Cu3Si) emerges below the SiO2 layer upon annealing at 550 °C. This silicide layer influences the lateral current and voltage distributions, as evidenced by an increasing effective area of the heterojunction diodes.

Synthesis of SiC nanoparticles by SHG 532 nm Nd:YAG laser ablation of silicon in ethanol

NASA Astrophysics Data System (ADS)

Khashan, Khawla S.; Ismail, Raid A.; Mahdi, Rana O.

2018-06-01

In this work, colloidal spherical nanoparticles NPs of silicon carbide SiC have been synthesized using second harmonic generation 532 nm Nd:YAG laser ablation of silicon target dipped in ethanol solution at various laser fluences (1.5-5) J/cm2. X-Ray diffraction XRD, scanning electron microscopy SEM, transmission electron microscope TEM, Fourier transformed infrared spectroscopy FT-IR, Raman spectroscopy, photoluminescence PL spectroscopy, and UV-Vis absorption were employed to examine the structural, chemical and optical properties of SiC NPs. XRD results showed that all synthesised SiC nanoparticles are crystalline in nature and have hexagonal structure with preferred orientation along (103) plane. Raman investigation showed three characteristic peaks 764,786 and 954 cm-1, which are indexing to transverse optic TO phonon mode and longitudinal optic LO phonon mode of 4H-SiC structure. The optical absorption data showed that the values of optical energy gap of SiC nanoparticles prepared at 1.5 J/cm2 was 3.6 eV and was 3.85 eV for SiC synthesised at 5 J/cm2. SEM investigations confirmed that the nanoparticles synthesised at 5 J/cm2 are agglomerated to form larger particles. TEM measurements showed that SiC particles prepared at 1.5 J/cm2 have spherical shape with average size of 25 nm, while the particles prepared at 5 J/cm2 have an average size of 55 nm.

Synthesis, characterization and effect of calcination temperature on phase transformation and photocatalytic activity of Cu,S-codoped TiO 2 nanoparticles

NASA Astrophysics Data System (ADS)

Hamadanian, M.; Reisi-Vanani, A.; Majedi, A.

2010-01-01

A novel copper and sulfur codoped TiO 2 photocatalyst was synthesized by modified sol-gel method using titanium(IV) isopropoxide, CuCl 2·2H 2O and thiourea as precursors. The samples were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy equipped with energy dispersive X-ray micro-analysis (SEM-EDX), transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) analysis. The XRD results showed undoped and Cu,S-codoped TiO 2 nanoparticles only include anatase phase. Effect of calcination temperature showed rutile phase appears in 650 and 700 °C for undoped and 0.1% Cu,S-codoped TiO 2, respectively. The SEM analysis revealed the doping of Cu and S does not leave any change in morphology of the catalyst surface. The increase of copper doping enhanced "red-shift" in the UV-vis absorption spectra. The TEM images confirmed the dopants suppressed the growth of TiO 2 grains. The photocatalytic activity of samples was tested for degradation of methyl orange (MO) solutions. The results showed photocatalytic activity of the catalysts with 0.05% Cu,0.05% S and 0.1% Cu,0.05% S were higher than that of other catalysts under ultraviolet (UV) and visible irradiation, respectively. Because of synergetic effect of S and Cu, the Cu,S-codoped TiO 2 catalyst has higher activity than undoped and Cu or S doped TiO 2 catalysts.

Enhanced broadband near-infrared luminescence from Pr3+-doped tellurite glass with silver nanoparticles

NASA Astrophysics Data System (ADS)

Cheng, Pan; Zhou, Yaxun; Zhou, Minghan; Su, Xiue; Zhou, Zizhong; Yang, Gaobo

2017-11-01

Pr3+-doped tellurite glasses containing metallic silver NPs were synthesized by the conventional melt-quenching technique. Structural, thermal and optical properties of the synthesized glass samples were characterized by X-Ray diffraction (XRD) curves, Raman spectra, differential scanning calorimeter (DSC) curves, transmission electron microscopy (TEM) images, UV/Vis/NIR absorption and near-infrared fluorescence emission spectra. The XRD curves confirmed the amorphous structural nature of the synthesized glasses, the Raman spectra identified the presence of different vibrational groups, the DSC curves verified the good thermal stability, and the TEM images revealed the nucleated silver NPs with average diameter about 10 nm dispersed in the glass matrix and its surface Plasmon resonance (SPR) absorption band was located at around 510 nm. Besides, Judd-Ofelt intensity parameters Ωt (t = 2, 4, 6) and other important spectroscopic parameters like transition probability, radiative lifetime, branching ratio were calculated to evaluate the radiative properties of Pr3+ levels from the measured optical absorption spectra. It was found that Pr3+-doped tellurite glasses could emit an ultra-broadband fluorescence extending from 1250 to 1650 nm under the 488 nm excitation, and this fluorescence emission increased further with the introduction of silver NPs. The enhanced fluorescence was mainly attributed to the increased local electric field around Pr3+ induced by silver NPs. The present results demonstrate that Pr3+-Ag codoped tellurite glass is a promising candidate for the near-infrared band ultra-broadband fiber amplifiers covering the expanded low-loss communication window.

Electron microscopy study of microbial mat in the North Fiji basin hydrothermal vent

NASA Astrophysics Data System (ADS)

Park, H.; Kim, J. W.; Lee, J. W.

2017-12-01

Hydrothermal vent systems consisting of hydrothermal vent, hydrothermal sediment and microbial mat are widely spread around the ocean, particularly spreading axis, continental margin and back-arc basin. Scientists have perceived that the hydrothermal systems, which reflect the primeval earth environment, are one of the best places to reveal the origin of life and extensive biogeochemical process of microbe-mineral interaction. In the present study multiline of analytical methods (X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM)) were utilized to investigate the mineralogy/chemistry of microbe-mineral interaction in hydrothermal microbial mat. Microbial mat samples were recovered by Canadian scientific submersible ROPOS on South Pacific North Fiji basin KIOST hydrothermal vent expedition 1602. XRD analysis showed that red-colored microbial mat contains Fe-oxides and Fe-oxyhydroxides. Various morphologies of minerals in the red-colored microbial mat observed by SEM are mainly showed sheath shaped, resembled with Leptothrix microbial structure, stalks shaped, similar with Marioprofundus microbial structure and globule shaped microbial structures. They are also detected with DNA analysis. The cross sectional observation of microbial structures encrusted with Fe-oxide and Fe-oxyhydroxide at a nano scale by Transmission Electron Microscopy (TEM) and Focused Ion Beam (FIB) technique was developed to verify the structural/biogeochemical properties in the microbe-mineral interaction. Systematic nano-scale measurements on the biomineralization in the microbial mat leads the understandings of biogeochemical environments around the hydrothermal vent.

γ-Fe{sub 2}O{sub 3} nanoparticles: An easily recoverable effective photo-catalyst for the degradation of rose bengal and methylene blue dyes in the waste-water treatment plant

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dutta, Amit Kumar; Maji, Swarup Kumar; Adhikary, Bibhutosh, E-mail: bibhutoshadhikary@yahoo.in

2014-01-01

Graphical abstract: - Highlights: • γ-Fe{sub 2}O{sub 3} NPs from a single-source precursor and characterized by XRD, TEM, UV–vis spectra. • The NPs were tested as effective photocatalyst toward degradation of RB and MB dyes. • The possible pathway of the photocatalytic decomposition process has been discussed. • The active species, OH·, was detected by TA photoluminescence probing techniques. - Abstract: γ-Fe{sub 2}O{sub 3} nanoparticles (NPs) were synthesized from a single-source precursor complex [Fe{sub 3}O(C{sub 6}H{sub 5}COO){sub 6}(H{sub 2}O){sub 3}]NO{sub 3} by a simple thermal decomposition process and have been characterized by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM)more » and UV–vis spectroscopic techniques. The NPs were highly pure and well crystallized having hexagonal morphology with an average particle size of 35 nm. The prepared γ-Fe{sub 2}O{sub 3} (maghemite) NPs show effective photo-catalytic activity toward the degradation of rose bengal (RB) and methylene blue (MB) dyes under visible light irradiation and can easily be recoverable in the presence of magnetic field for successive re-uses. The possible photo-catalytic decomposition mechanism is discussed through the detection of hydroxyl radical (OH·) by terephthalic acid photo-luminescence probing technique.« less

An improved green synthesis method and Escherichia coli antibacterial activity of silver nanoparticles.

PubMed

Van Viet, Pham; Sang, Truong Tan; Bich, Nguyen Ho Ngoc; Thi, Cao Minh

2018-05-01

Silver nanoparticles (Ag NPs) were synthesized by an improved green synthesis method via a photo-reduction process using low-power UV light in the presence of poly (vinyl pyrrolidone) (PVP) as the surface stabilizer. The effective synthesis process was achieved by optimized synthesis parameters such as C 2 H 5 OH: H 2 O ratio, AgNO 3 : PVP ratio, pH value, and reducing time. The formation of Ag NPs was identified by Ultraviolet-visible (UV-vis) absorption spectra, X-ray diffraction pattern (XRD) and Fourier transform infrared spectroscopy (FTIR) spectra. Ag NPs were crystallized according to (111), (200), and (220) planes of the face-centered cubic. The transmission electron microscopy (TEM) image showed that the morphology of Ag NPs was uniform spherical with the average particle size of 16 ± 2 nm. The results of XRD pattern, TEM image, and dynamic light scattering (DLS) analysis proved that Ag crystals with uniform size were formed after the reduction process. The mechanism of the formation of Ag NPs was proposed and confirmed by FTIR spectra. The antibacterial activity of Ag NPs against Escherichia coli (E. coli) was tested and approximately 100% of E. coli was eliminated by Ag NPs 35 ppm. In the future, this study can become a new process for the application of Ag NPs as an antibiotic in the industrial scale. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis, electrical and magnetic properties of sodium borosilicate glasses containing Co-ferrites nanoparticles

NASA Astrophysics Data System (ADS)

Othman, H. A.; Eltabey, M. M.; Ibrahim, Samia. E.; El-Deen, L. M. Sharaf; Elkholy, M. M.

2017-02-01

Co-ferrites nanoparticles that have been prepared by the co-precipitation method were added to sodium borosilicate (Na2O-B2O3-SiO2) glass matrix by the solid solution method and they were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and magnetization measurements. (XRD) revealed the formation of the Co-ferrite magnetic crystalline phase embedded in an amorphous matrix in all the samples. The investigated samples by (TEM) showed the formation of the cobalt ferrite nanoparticles with a spherical shape and highly monodispersed with an average size about 13 nm. IR data revealed that the BO3 and BO4 are the main structural units of these samples network. IR spectra of the investigated samples showed the characteristic vibration bands of Co-ferrite. Composition and frequency dependent dielectric properties of the prepared samples were measured at room temperature in the frequency range 100-100 kHz. The conductivity was found to increase with increasing cobalt ferrite content. The variations of conductivity and dielectric properties with frequency and composition were discussed. Magnetic hysteresis loops were traced at room temperature using VSM and values of saturation magnetization MS and coercive field HC were determined. The obtained results revealed that a ferrimagnetic behavior were observed and as Co-ferrite concentration increases the values of MS and HC increase from 2.84 to 8.79 (emu/g) and from 88.4 to 736.3 Oe, respectively.

New nano-sized Al2O3-BN coating 3Y-TZP ceramic composites for CAD/CAM-produced all-ceramic dental restorations. Part I. Fabrication of powders.

PubMed

Yang, Se Fei; Yang, Li Qiang; Jin, Zhi Hao; Guo, Tian Wen; Wang, Lei; Liu, Hong Chen

2009-06-01

Partially sintered 3 mol % yttria-stabilized tetragonal zirconium dioxide (ZrO(2), zirconia) polycrystal (3Y-TZP) ceramics are used in dental posterior restorations with computer-aided design-computer-aided manufacturing (CAD/CAM) techniques. High strength is acquired after sintering, but shape distortion of preshaped compacts during their sintering is inevitable. The aim of this study is to fabricate new machinable ceramic composites with strong mechanical properties that are fit for all-ceramic dental restorations. Aluminum oxide (Al(2)O(3))-coated 3Y-TZP powders were first prepared by the heterogeneous precipitation method starting with 3Y-TZP, Al(NO(3))(3) . 9H(2)O, and ammonia, then amorphous boron nitride (BN) was produced and the as-received composite powders were coated via in situ reaction with boric acid and urea. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to analyze the status of Al(2)O(3)-BN on the surface of the 3Y-TZP particles. TEM micrographs show an abundance of Al(2)O(3) particles and amorphous BN appearing uniformly on the surface of the 3Y-TZP particles after the coating process. The size of the Al(2)O(3) particles is about 20 nm. The XRD pattern shows clearly the peak of amorphous BN among the peaks of ZrO(2).

Enhancement of aptamer immobilization using egg shell-derived nano-sized spherical hydroxyapatite for thrombin detection in neuroclinic.

PubMed

Derkus, Burak; Arslan, Yavuz Emre; Emregul, Kaan C; Emregul, Emel

2016-09-01

In the present study, we describe the sonochemical isolation of nano-sized spherical hydroxyapatite (nHA) from egg shell and application towards thrombin aptasensing. In addition to the sonochemical method, two conventional methods present in literature were carried out to perform a comparative study. Various analysis methods including Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Energy-Dispersive Analysis of X-Rays (EDAX), and Thermal Gravimetric Analysis (TGA) have been applied for the characterization of nHA and its nanocomposite with marine-derived collagen isolated from Rhizostoma pulmo jellyfish. TEM micrographs revealed the sonochemically synthesized nHA nanoparticles to have a unique porous spherical shape with a diameter of approximately 60-80nm when compared to hydroxyapatite nanoparticles synthesized using the other two methods which had a typical needle shaped morphology. EDAX, XRD and FTIR results demonstrated that the obtained patterns belonged to hydroxyapatite. Electrochemical impedance spectroscopy (EIS) is the main analyzing technique of the developed thrombin aptasensor. The proposed aptasensor has a detection limit of 0.25nM thrombin. For clinical application of the developed aptasensor, thrombin levels in blood and cerebrospinal fluid (CSF) samples obtained from patients with Multiple Sclerosis, Myastenia Gravis, Epilepsy, Parkinson, polyneuropathy and healthy donors were analyzed using both the aptasensor and commercial ELISA kit. The results showed that the proposed system is a promising candidate for clinical analysis of thrombin. Copyright © 2016 Elsevier B.V. All rights reserved.

Transparent Al+3 doped MgO thin films for functional applications

NASA Astrophysics Data System (ADS)

Maiti, Payel; Sekhar Das, Pradip; Bhattacharya, Manjima; Mukherjee, Smita; Saha, Biswajit; Mullick, Awadesh Kumar; Mukhopadhyay, Anoop Kumar

2017-08-01

The present work reports the utilization of a relatively simple, cost effective sol-gel technique based route to synthesize highly transparent, spin coated 4.1 at% Al+3 doped MgO thin films on quartz substrates. The films were characterized by XRD, XPS, Raman spectroscopy, and SIMS techniques. The microstructures were characterized by FESEM and TEM while the nanomechanical properties were assessed by the nanoindentation technique. Finally the optical transmittance was measured by UV-vis technique. The x-ray diffraction (XRD) study suggests the crystal facet (2 0 0) of MgO lattice to be distorted after incorporation of Al+3 into MgO lattice. From FESEM the doped films were found to have a dense microstructure with a crystallite size of about 20 nm as revealed by the TEM studies. Nanoindentation measurements indicated drastic increase of elastic modulus for the Al+3 doped MgO thin films by ~73% compared to that of the pristine MgO thin films along with retaining the nanohardness at ~8 GPa. The transmittance of Al+3 doped MgO thin films in the visible range was significantly higher (~99%) than that of pristine MgO (~90%) thin films. The films also had a relatively higher refractive index of about 1.45 as evaluated from the optical properties. The enhanced transmittance as well as the improved elastic modulus of Al+3 doped MgO thin films suggest its promising candidature in magnetic memory devices and as buffer layers of solar cells.

To study the effect of dopant NiO concentration and duration of calcinations on structural and optical properties of MgO-NiO nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Deptt. of Physics,Vaish College of Engineering, Rohtak-124001, Haryana; Praveen,

2016-05-06

In present work Magnesium oxide (MgO) samples were doped with different concentration of Transition metal Nickel Oxide(NiO) by using Chemical co-precipitation method. The doping levels were varied from NiO (5%, 10%, 15%) and all the samples were calcined at 600°C for 4hrs and 8hrs respectively. Structural analysis of these calcined materials is carried out by X-ray diffraction (XRD) techniques which reveals that average crystalline sizes are in nano region i.e. 21.77nm-31.13 nm and tabulated in table 1. The powder of calcined samples were also characterized by using various other techniques i.e. Scanning Electron Microscopy (SEM), Fourier Transformation Infrared Spectroscopy (FTIR), UV-Visiblemore » spectroscopy, Transmission Electron Microscopy (TEM) etc. The effects of dopant concentration, calcined temperature, calcinations duration on samples were studied and also investigate the effect of varying dopant concentration on morphology and optical properties of calcined nanomaterials. From results it was observed that the crystallite size of nanocomposites increases with increases dopant concentration or increases calcinations duration. The optical band gap decreases with increases sintering time and increase with increases dopant concentrations. TEM results coincide with XRD results and show that particles are polycrystalline in nature. FTIR spectra show that for all samples particles are pure in composition and transmission rate increases with calcinations duration.« less

Photocatalytic degradation of organic contaminants under solar light using carbon dot/titanium dioxide nanohybrid, obtained through a facile approach

NASA Astrophysics Data System (ADS)

Hazarika, Deepshikha; Karak, Niranjan

2016-07-01

In the present study, a novel, simple and green method was developed to synthesize highly luminescent nitrogen containing carbon dot (CD) using carbon resources like bio-based citric acid and glycerol in the presence of cost free cow urine. The as-synthesized CD showed exciting wavelength dependent down- and up-conversion flourescence properties. To utilize the advantage of up-conversion flourescence, a nanohybrid (CD@TiO2) was synthesized from the above carbon resources and titanium butoxide through a facile one pot single step hydrothermal protocol. Nanomaterials like bare TiO2 and nanohybrid of TiO2 in presence of CD (CD/TiO2) were also synthesized for comparison purpose. The optical properties and structural characteristics of the prepared CD, bare TiO2, CD@TiO2 and CD/TiO2 were examined by Fourier transform infrared (FTIR), UV-vis and fluorescence spectroscopic, scanning electron microscopic (SEM), transmission electron microscopic (TEM) and X-ray diffraction (XRD) studies. The elemental compositions of bare CD and CD@TiO2 nanohybrid were obtained from EDX analyses. The poor crystalline nature and narrow distribution of spherical CD and anatase form of TiO2 were confirmed from XRD and TEM studies. Amongst the studied nanomaterials, CD@TiO2 exhibited the most promising photocatalytic degradation of organic pollutants like benzene and phenol as well as an anthrogenic pesticide under sunlight.

Understanding the formation and growth of Ag nanoparticles on silver chromate induced by electron irradiation in electron microscope: A combined experimental and theoretical study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fabbro, Maria T.; Department of Inorganic and Organic Chemistry, Universitat Jaume I, Campus del Riu Sec, E-12071 Castellón; Gracia, Lourdes

Ag{sub 2}CrO{sub 4} microcrystals were synthesized using the co-precipitation method. These microcrystals were characterized through X-ray diffraction (XRD) with Rietveld analysis, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), micro-Raman (MR). XRD patterns and Rietveld refinement data showed that the material exhibits an orthorhombic structure without any deleterious phases. FE-SEM and TEM micrographs revealed the morphology and the growth of Ag nanoparticles on Ag{sub 2}CrO{sub 4} microcrystals during electron beam irradiation. These events were directly monitored in real-time. Their optical properties were investigated using ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy that allowed the calculation of themore » optical band gap energy. Theoretical analyses based on the density functional theory level indicate that the incorporation of electrons is responsible for structural modifications and formation of defects on the [AgO{sub 6}] and [AgO{sub 4}] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag{sub 2}CrO{sub 4} orthorhombic structure. Display Omitted - Highlights: • The Ag{sub 2}CrO{sub 4} microcrystals indicate an orthorhombic structure. • The formation of Ag{sup 0} promotes Ag-nanoparticle growth on the surface of the Ag{sub 2}CrO{sub 4}. • Electron irradiation of the material induces the formation of Ag vacancies.« less

Eco-friendly preparation of zinc oxide nanoparticles using Tabernaemontana divaricata and its photocatalytic and antimicrobial activity.

PubMed

Raja, A; Ashokkumar, S; Pavithra Marthandam, R; Jayachandiran, J; Khatiwada, Chandra Prasad; Kaviyarasu, K; Ganapathi Raman, R; Swaminathan, M

2018-04-01

The present work reports the green synthesis of Zinc Oxide Nanoparticles (ZnO NPs) using aqueous Tabernaemontana divaricata green leaf extract. ZnO NPs have been characterized by X-ray diffraction (XRD), Ultra Violet-Visible (UV-Vis) studies, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Fourier Transform-Infra Red (FT-IR) analysis. XRD pattern analysis confirms the presence of pure hexagonal wurtzite crystalline structure of ZnO. The TEM images reveal the formation of spherical shape ZnO NPs with the sizes ranging from 20 to 50 nm. The FT-IR analysis suggests that the obtained ZnO NPs have been stabilized through the interactions of steroids, terpenoids, flavonoids, phenyl propanoids, phenolic acids and enzymes present in the leaf extract. Mechanism for the formation of ZnO NPs using Tabernaemontana divaricata as bioactive compound is proposed. As prepared ZnO NPs reveals antibacterial activity against three bacterial strains, Salmonella paratyphi, Escherichia coli and Staphylococcus aureus. The ZnO NPs shows higher antibacterial activity against S. aureus and E. coli and lesser antibacterial activity against S. paratyphi compared to the standard pharmaceutical formulation. Photocatalytic activity of synthesized ZnO NPs was analyzed for methylene blue (MB) dye degradation with sunlight. Almost complete degradation of dye occurred in 90 min. This nano-ZnO, prepared by eco-friendly method will be much useful for dye removal and bacterial decontamination. Copyright © 2018. Published by Elsevier B.V.

Microstructural, Magnetic, and Optical Properties of Pr-Doped Perovskite Manganite La0.67Ca0.33MnO3 Nanoparticles Synthesized via Sol-Gel Process

NASA Astrophysics Data System (ADS)

Xia, Weiren; Wu, Heng; Xue, Piaojie; Zhu, Xinhua

2018-05-01

We report on microstructural, magnetic, and optical properties of Pr-doped perovskite manganite (La1 - xPrx)0.67Ca0.33MnO3 (LPCMO, x = 0.0-0.5) nanoparticles synthesized via sol-gel process. Structural characterizations (X-ray and electron diffraction patterns, (high resolution) TEM images) provide information regarding the phase formation and the single-crystalline nature of the LPCMO systems. X-ray and electron diffraction patterns reveal that all the LPCMO samples crystallize in perovskite crystallography with an orthorhombic structure ( Pnma space group), where the MnO6 octahedron is elongated along the b axis due to the Jahn-Teller effect. That is confirmed by Raman spectra. Crystallite sizes and grain sizes were calculated from XRD and TEM respectively, and the lattice fringes resolved in the high-resolution TEM images of individual LPCMO nanoparticle confirmed its single-crystalline nature. FTIR spectra identify the characteristic Mn-O bond stretching vibration mode near 600 cm- 1, which shifts towards high wavenumbers with increasing post-annealing temperature or Pr-doping concentration, resulting in further distortion of the MnO6 octahedron. XPS revealed dual oxidation states of Mn3+ and Mn4+ in the LPCMO nanoparticles. UV-vis absorption spectra confirm the semiconducting nature of the LPCMO nanoparticles with optical bandgaps of 2.55-2.71 eV. Magnetic measurements as a function of temperature and magnetic field at field cooling and zero-field cooling modes, provided a Curie temperature around 230 K, saturation magnetization of about 81 emu/g, and coercive field of 390 Oe at 10 K. Such magnetic properties and the semiconducting nature of the LPCMO nanoparticles will make them as suitable candidate for magnetic semiconductor spintronics.

Characterization, antioxidant and cytotoxicity evaluation of green synthesized silver nanoparticles using Cleistanthus collinus extract as surface modifier

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kanipandian, Nagarajan; Kannan, Soundarapandian; Ramesh, Ramar

Graphical abstract: The figure is the TEM image of green synthesized silver nanoparticles from Cleistanthus collinus. In this investigation we have used the poisonous plant as a reducing and capping agent. This is a first time data to synthesis the metal nanoparticles using poisonous plant. - Highlights: • A hitherto unreported venomous plant mediated AgNPs synthesis. • The particle size is observed in the range of 20–40 nm. • Surface morphology of the well-dispersed silver nanoparticles is studied using SEM and TEM. • Crystalline nature of AgNPs is confirmed by X-ray diffraction analysis. • Antioxidant activities of green synthesized AgNPsmore » are tested in vitro. - Abstract: We report, here a simple green method for the preparation of silver nanoparticles (AgNPs) using the plant extract of Cleistanthus collinus as potential phyto reducer. The synthesized AgNPs were characterized by UV–vis spectra, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained results confirmed that the AgNPs were crystalline in nature and the morphological studies reveal the spherical shape of AgNPs with size ranging from 20 to 40 nm. The in vitro antioxidant activity of AgNPs showed a significant effect on scavenging of free radicals. The cytotoxicity study exhibited a dose-dependent effect against human lung cancer cells (A549) and normal cells (HBL-100), the inhibitory concentration (IC{sub 50}) were found to be 30 μg/mL and 60 μg/mL respectively. The in vivo histopathology of mouse organs proved that AgNPs does not possess toxic effect and can be extensively applied in biomedical sciences.« less

The synthesis of biocompatible and SERS-active gold nanoparticles using chitosan.

PubMed

Potara, Monica; Maniu, Dana; Astilean, Simion

2009-08-05

In this study we present a clean, nontoxic, environmentally friendly synthesis procedure to generate a large variety of gold nanoparticles (GNPs) by using chitosan, a biocompatible, biodegradable, natural polymer, as reducing and stabilizing agent. The formation of gold-chitosan nanocomposites was characterized by UV-vis absorption spectroscopy, transmission electron microscopy (TEM), x-ray diffraction (XRD) and Raman spectroscopy. The results show that the reaction temperature plays a crucial role in controlling the size, shape and crystalline structure of GNPs. In addition, it is demonstrated that chitosan can perform as a scaffold for the assembly of GNPs, which were successfully applied as substrate for surface-enhanced Raman scattering (SERS). To test the SERS activity, a relevant biological molecule--tryptophan--was adopted as the analyte.

Synthesis and characterization of intercalated polyaniline-clay nanocomposite using supercritical CO2

NASA Astrophysics Data System (ADS)

Abdelraheem, A.; El-Shazly, A. H.; Elkady, M. F.

2018-05-01

Lately, supercritical CO2 (SCCO2) have been getting great interest. It can be used in numerous applications because it is environmentally friendly, safe, comparatively low cost, and nonflammable. One of its applications is being a solvent in the synthesis of polymeric-clay nanocomposite. In this paper, intercalated polyaniline-clay nanocomposite (PANC) was prepared using SCCO2. The intercalation structure of polyaniline chains between clay layers was verified by various characterization techniques. Scanning electron microscope and transmission electron microscope (SEM-TEM) were used to show the morphology of the synthesized nanocomposite. The molecular structure of PANC nanocomposite was confirmed using Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The BET surface area and the conductivity of the nanocomposite were determined.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach.

PubMed

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. This journal is © The Royal Society of Chemistry 2011

Catalytic performance of Mn 3O 4 and Co 3O 4 nanocrystals prepared by sonochemical method in epoxidation of styrene and cyclooctene

NASA Astrophysics Data System (ADS)

Askarinejad, Azadeh; Bagherzadeh, Mojtaba; Morsali, Ali

2010-09-01

A simple sonochemical method was developed to synthesis uniform sphere-like Co 3O 4 and Mn 3O 4 nanocrystals. Epoxidation of styrene and cyclooctene by anhydrous tert-butyl hydroperoxide over the prepared Co 3O 4 and Mn 3O 4 nanocatalysts was investigated. The results of conversion activity were compared with bulk Co 3O 4 and Mn 3O 4. Under optimized reaction conditions, the nanocatalysts showed a superior catalytic performance as compared to the bulk catalysts. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and BET surface area, were used to characterize and investigate the nanocatalysts.

XANES: observation of quantum confinement in the conduction band of colloidal PbS quantum dots

NASA Astrophysics Data System (ADS)

Demchenko, I. N.; Chernyshova, M.; He, X.; Minikayev, R.; Syryanyy, Y.; Derkachova, A.; Derkachov, G.; Stolte, W. C.; Piskorska-Hommel, E.; Reszka, A.; Liang, H.

2013-04-01

The presented investigations aimed at development of inexpensive method for synthesized materials suitable for utilization of solar energy. This important issue was addressed by focusing, mainly, on electronic local structure studies with supporting x-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis of colloidal galena nano-particles (NPs) and quantum dots (QDs) synthesized using wet chemistry under microwave irradiation. Performed x-ray absorption near edge structure (XANES) analysis revealed an evidence of quantum confinement for the sample with QDs, where the bottom of the conduction band was shifted to higher energy. The QDs were found to be passivated with oxides at the surface. Existence of sulfate/sulfite and thiosulfate species in pure PbS and QDs, respectively, was identified.

Low temperature hall effect investigation of conducting polymer-carbon nanotubes composite network.

PubMed

Bahrami, Afarin; Talib, Zainal Abidin; Yunus, Wan Mahmood Mat; Behzad, Kasra; M Abdi, Mahnaz; Din, Fasih Ud

2012-11-14

Polypyrrole (PPy) and polypyrrole-carboxylic functionalized multi wall carbon nanotube composites (PPy/f-MWCNT) were synthesized by in situ chemical oxidative polymerization of pyrrole on the carbon nanotubes (CNTs). The structure of the resulting complex nanotubes was characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The effects of f-MWCNT concentration on the electrical properties of the resulting composites were studied at temperatures between 100 K and 300 K. The Hall mobility and Hall coefficient of PPy and PPy/f-MWCNT composite samples with different concentrations of f-MWCNT were measured using the van der Pauw technique. The mobility decreased slightly with increasing temperature, while the conductivity was dominated by the gradually increasing carrier density.

Effect of Ni Core Structure on the Electrocatalytic Activity of Pt-Ni/C in Methanol Oxidation

PubMed Central

Kang, Jian; Wang, Rongfang; Wang, Hui; Liao, Shijun; Key, Julian; Linkov, Vladimir; Ji, Shan

2013-01-01

Methanol oxidation catalysts comprising an outer Pt-shell with an inner Ni-core supported on carbon, (Pt-Ni/C), were prepared with either crystalline or amorphous Ni core structures. Structural comparisons of the two forms of catalyst were made using transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), and methanol oxidation activity compared using CV and chronoamperometry (CA). While both the amorphous Ni core and crystalline Ni core structures were covered by similar Pt shell thickness and structure, the Pt-Ni(amorphous)/C catalyst had higher methanol oxidation activity. The amorphous Ni core thus offers improved Pt usage efficiency in direct methanol fuel cells. PMID:28811402

Synthesis, characterization, in vitro anti-proliferative and hemolytic activity of hydroxyapatite

NASA Astrophysics Data System (ADS)

Palanivelu, R.; Ruban Kumar, A.

2014-06-01

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP) nanoparticles are widely used in several biomedical applications due to its compositional similarities to bone mineral, excellent biocompatibility and bioactivity, osteoconductivity. In this present investigation, HAP nanoparticles synthesized by precipitation technique using calcium nitrate and di-ammonium phosphate. The crystalline nature and the functional group analysis are confirmed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Fourier transform Raman spectroscopy (FT-Raman) respectively. The morphological observations are ascertained from field emission electron scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). In vitro anti-proliferative and hemolytic activities are carried out on the synthesized HAP samples and the studies reveals that HAP have mild activity against erythrocytes.

Preparation of silver nanoparticles loaded graphene oxide nanosheets for antibacterial activity

NASA Astrophysics Data System (ADS)

T, T. T., Vi; Lue, S. J.

2016-11-01

A simple, facile method to fabricate successfully silver nanoparticle (AgNPs) decorated on graphene oxide (GO) layers via grafted thiol groups. Samples were prepared with different concentrations of AgNO3. Resulting AgNPs were quasi-spherical in shape and attached on the layers of GO. Physical properties were confirmed by X-ray diffraction (XRD), zeta potential, dynamic light scattering (DLS), Fourier transform infrared (FTIR) spectra, thermogravimetric analyzer (TGA), transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM). Antimicrobial test was effectively showed using MRSA (Staphylococcus areus). The GO-Ag NPs with appropriate Ag NPs content of 0.2 M AgNO3 exhibited the strongest antibacterial activity at 48.77% inhibition after 4 hours incubation.

Pt nanoparticle-reduced graphene oxide nanohybrid for proton exchange membrane fuel cells.

PubMed

Park, Dae-Hwan; Jeon, Yukwon; Ok, Jinhee; Park, Jooil; Yoon, Seong-Ho; Choy, Jin-Ho; Shul, Yong-Gun

2012-07-01

A platinum nanoparticle-reduced graphene oxide (Pt-RGO) nanohybrid for proton exchange membrane fuel cell (PEMFC) application was successfully prepared. The Pt nanoparticles (Pt NPs) were deposited onto chemically converted graphene nanosheets via ethylene glycol (EG) reduction. According to the powder X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) analysis, the face-centered cubic Pt NPs (3-5 nm in diameter) were homogeneously dispersed on the RGO nanosheets. The electrochemically active surface area and PEMFC power density of the Pt-RGO nanohybrid were determined to be 33.26 m2/g and 480 mW/cm2 (maximum values), respectively, at 75 degrees C and at a relative humidity (RH) of 100% in a single-cell test experiment.

Effect of reduced graphene oxide-carbon nanotubes hybrid nanofillers in mechanical properties of polymer nanocomposites

NASA Astrophysics Data System (ADS)

Sa, Kadambinee; Mahakul, Prakash C.; Subramanyam, B. V. R. S.; Raiguru, Jagatpati; Das, Sonali; Alam, Injamul; Mahanandia, Pitamber

2018-03-01

Graphene and carbon nanotubes (CNTs) have tremendous interest as reinforcing fillers due to their excellent physical properties. However, their reinforcing effect in polymer matrix is limited due to agglomeration of graphene and CNTs within the polymer matrix. Mechanical properties by the admixture of reduced graphene oxide (rGO) and CNTs in Poly (methyl methacrylate) (PMMA) prepared by solution mixing method has been investigated. The prepared samples are characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and Raman spectroscopy. The hybrid composite shows improvement in the mechanical properties compared to rGO/PMMA and MWCNTs/PMMA composites due to better interaction between rGO-MWCNTs and polymer matrix.

Colloidal synthesis of monodispersed ZnS and CdS nanocrystals from novel zinc and cadmium complexes

NASA Astrophysics Data System (ADS)

Onwudiwe, Damian C.; Mohammed, Aliyu D.; Strydom, Christien A.; Young, Desmond A.; Jordaan, Anine

2014-06-01

Monodispersed spherical and hexagonal shaped ZnS and CdS nanocrystals respectively, have been synthesized using novel heteroleptic complexes of xanthate (S2CObu) and dithiocarbamate (S2CNMePh). The nanocrystals were prepared via colloidal route and stabilized in hexadecylamine (HDA). The morphology of the as-prepared nanocrystals was characterized using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), and powdered X-ray diffraction (p-XRD) analysis. An average diameter of 7.2 nm and 8.6 nm were obtained for the ZnS and CdS respectively. The optical properties of the nanoparticles studied by UV-vis and photoluminescence (PL) spectroscopy showed a blue shift in the absorption spectra, and band edge emission respectively.

Tunable Properties of Exfoliated Polyvinylalcohol Nanocomposites by In Situ Coprecipitation of Layered Double Hydroxides

NASA Astrophysics Data System (ADS)

Liu, Jiajia; Yuen, Richard K. K.; Hu, Yuan

2017-10-01

Poly(vinyl alcohol) (PVA) nanocomposites were prepared by a “one step” method based on the coprecipitation of layered double hydroxide (LDH) nanosheets in the polymer aqueous solution. The morphology, fire resistance properties, mechanical and optical properties of the PVA/LDH nanocomposites were studied. The LDH nanosheets were homogeneously dispersed in the PVA matrix as indicated by X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) characterization. Meanwhile, the peak of heat release rate (pHRR) and total heat release (THR) were decreased by 58% and 28%, respectively. Storage modulus at 30 °C was increased, and the transmittance of more than 90% at the visible region was obtained upon addition of 5 wt% LDH.

Influence of Synthesis Temperature on the Growth and Surface Morphology of Co₃O₄ Nanocubes for Supercapacitor Applications.

PubMed

Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Sanjay, Kali; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

2017-10-31

A facile hydrothermal route to control the crystal growth on the synthesis of Co₃O₄ nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co₃O₄ nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co₃O₄ synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes.

Biosynthesis and characterization of silver nanoparticles prepared from two novel natural precursors by facile thermal decomposition methods

NASA Astrophysics Data System (ADS)

Goudarzi, Mojgan; Mir, Noshin; Mousavi-Kamazani, Mehdi; Bagheri, Samira; Salavati-Niasari, Masoud

2016-09-01

In this work, two natural sources, including pomegranate peel extract and cochineal dye were employed for the synthesis of silver nanoparticles. The natural silver complex from pomegranate peel extract resulted in nano-sized structures through solution-phase method, but this method was not efficient for cochineal dye-silver precursor and the as-formed products were highly agglomerated. Therefore, an alternative facile solid-state approach was investigated as for both natural precursors and the results showed successful production of well-dispersed nanoparticles with narrow size distribution for cochineal dye-silver precursor. The products were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray microanalysis (EDX), and Transmission Electron Microscopy (TEM).

Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

USDA-ARS?s Scientific Manuscript database

Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

PubMed

Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

2016-12-01

This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO 2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO 2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO 2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO 2 : anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO 2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO 2 nanoparticles.

Nanocomposites prepared from acrylonitrile butadiene rubber and organically modified montmorillonite with vinyl groups

NASA Astrophysics Data System (ADS)

Han, Mijeong; Kim, Hoonjung; Kim, Eunkyoung

2006-01-01

Nanocomposites were prepared from acrylonitrile-butadiene rubber (NBR), vinyl groups containing organically modified montmorillonite and additives, such as zinc oxide, stearic acid, and sulfur. The organically modified montmorillonites used in these nanocomposites were prepared by ion exchange reactions of N,N'-dimethylalkyl-(p-vinylbenzyl)-ammonium chlorides (DAVBAs, alkyl = octyl, dodecyl, and octadecyl) with sodium montmorillonite (Na+-MMT). NBR nanocomposites were obtained by controlling both the mixing and vulcanization conditions, by using a Brabender mixer and hot-press process. X-ray diffraction (XRD) analysis shows that, depending on the amount of montmorillonite that is added, both exfoliated and intercalated nanocomposite structures are formed. The NBR/DAVBA-MMT nanocomposites exhibit much higher mechanical properties (e.g., tensile strength, Young's modulus, 300% modulus, and hardness) as well as gas barrier properties as compared to NBR Na+-MMT or NBR composites generated from modified montmorillonites without vinyl groups. Consistent with the results of XRD, transmission electron microscopy (TEM) reveals that the intercalation and exfoliation structures of the nanocomposites coexist and that the DAVBA-MMT layers are well dispersed in NBR.

Synergistic effect on the visible light activity of Ti3+ doped TiO2 nanorods/boron doped graphene composite

PubMed Central

Xing, Mingyang; Li, Xiao; Zhang, Jinlong

2014-01-01

TiO2/graphene (TiO2-x/GR) composites, which are Ti3+ self-doped TiO2 nanorods decorated on boron doped graphene sheets, were synthesized via a simple one-step hydrothermal method using low-cost NaBH4 as both a reducing agent and a boron dopant on graphene. The resulting TiO2 nanorods were about 200 nm in length with exposed (100) and (010) facets. The samples were characterized by X-ray diffraction (XRD), UV-visible diffuse reflectance spectroscopy, X-band electron paramagnetic resonance (EPR), X-ray photoelectron spectra (XPS), transmission electron microscope (TEM), Raman, and Fourier-transform infrared spectroscopy (FTIR). The XRD results suggest that the prepared samples have an anatase crystalline structure. All of the composites tested exhibited improved photocatalytic activities as measured by the degradation of methylene blue and phenol under visible light irradiation. This improvement was attributed to the synergistic effect of Ti3+ self-doping on TiO2 nanorods and boron doping on graphene. PMID:24974890

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Study of the presence of fluorine in the recycled fractions during carbothermal treatment of EAF dust.

PubMed

Menad, N; Ayala, J N; Garcia-Carcedo, Fernando; Ruiz-Ayúcar, E; Hernández, A

2003-01-01

Carbothermal treatment tests of electric arc furnace dusts (EAFD) using the Waelz kiln process were carried out in pilot-scale for the production of zinc oxide. The association of halides in the EAFD, and the recycled products, such as zinc oxide fumes and high-grade iron contents fractions were examined by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. XRD reveals the presence of chlorine and fluorine in the dusts in the form of KCl, NaCl and CaF2. An ultra-pure fraction of zinc was obtained after the Double Leaching Waelz Oxide (DLWO) process was performed on the zinc oxide fumes. The halide contents were reduced to approximately 100 ppm Cl and 700 ppm F. The rest of these elements are in the form of CaF2. About 65% F is volatilised as lead and zinc fluorides, 15% is expected in the magnetic fractions and 20% in non-magnetic fractions as CaF2 and MnF2, respectively.

Nano-sized, quaternary titanium(IV) metal-organic frameworks with multidentate ligands.

PubMed

Baranwal, Balram Prasad; Singh, Alok Kumar

2010-12-01

Some mononuclear nano-sized, quaternary titanium(IV) complexes having the general formula [Ti(acac)(OOCR)2(SB)] (where Hacac=acetylacetone, R=C15H31 or C17H35, HSB=Schiff bases) have been synthesized using different multidentate ligands. These were characterized by elemental analyses, molecular weight determinations and spectral (FTIR, 1H NMR and powder XRD) studies. Conductance measurement indicated their non-conducting nature which may behave like insulators. Structural parameters like the values of limiting indices h, k, l, cell constants a, b, c, angles α, β, γ and particle size are calculated from powder XRD data for complex 1 which indicated nano-sized triclinic system in them. Bidentate chelating nature of acetylacetone, carboxylate and Schiff base anions in the complexes was established by their infrared spectra. Molecular weight determinations confirmed mononuclear nature of the complexes. On the basis of physico-chemical studies, coordination number 8 was assigned for titanium(IV) in the complexes. Transmission electron microscopy (TEM) and the selected area electron diffraction (SAED) studies indicated spherical particles with poor crystallinity. Copyright © 2010 Elsevier B.V. All rights reserved.

Structural and magnetic properties of Ni1-xZnxFe2O4 synthesized through the sol-gel method

NASA Astrophysics Data System (ADS)

Guan, Beh Hoe; Zahari, Muhammad Hanif; Chuan, Lee Kean

2016-11-01

Modification of crystal structure by means of substitution would result in the modification of the overall physical properties of crystallite materials especially in ferrites. This study aims to investigate the effect of non-magnetic Zn substitution in spinel NiFe2O4 and its direct effect towards its microstructural and magnetic properties. Magnetic nanoparticles of Nickel-Zinc ferrite with the chemical formula, Ni1-xZnxFe2O4 (x=0.00, 0.25, 0.50, 0.75) were synthesized through the sol-gel route. Phase formation and structural properties of the synthesized ferrite were identified through X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). Magnetic properties such as the magnetic saturation, coercivity and remanence were measured by a vibrating sample magnetometer (VSM). XRD measurements reveals successful synthesis of single-phased Nickel ferrite and Nickel—Zinc ferrite. Both crystallite and grain size shows fluctuation with increasing Zn content. The ferrites were found to be ferrimagnetic in nature and show differing values with different x values.

Al3+ ions dependent structural and magnetic properties of Co-Ni nano-alloys.

PubMed

Kadam, R H; Alone, Suresh T; Gaikwad, Anil S; Birajdar, A P; Shirsath, Sagar E

2014-06-01

Ferrite samples with a chemical formula Co0.5Ni0.5Al(x)Fe(2-x)O4 (where x = 0.0, 0.25, 0.5, 0.75 and 1.0) were synthesized by sol-gel auto-combustion method. The synthesized samples were annealed at 600 degrees C for 4 h. An analysis of X-ray diffraction (XRD) patterns reveals the formation of single phase cubic spinel structure. The lattice parameter decreased linearly with the increasing Al content x. Nano size of the powders were confirmed by the transmission electron micrographs (TEM). Particle size, bulk density decreased whereas specific surface area and porosity of the samples increased with the Al substitution. Cation distribution of constituent ions shows linear dependence of Al substitution. Based on the cation distribution obtained from XRD data, structural parameters such as lattice parameters, ionic radii of available sites and the oxygen parameter 'u' is calculated. Saturation magnetization (M(s)), magneton number (n(B)) and coercivity (H(c)) decreased with the Al substitution. Possible explanation for the observed structural and magnetic behavior with various Al content are discussed.

Intercalation of cellulase enzyme into a hydrotalcite layer structure

NASA Astrophysics Data System (ADS)

Zou, N.; Plank, J.

2015-01-01

A new inorganic-organic hybrid material whereby cellulase enzyme is incorporated into a hydrotalcite type layered double hydroxide (LDH) structure is reported. The Mg2Al-cellulase-LDH was synthesized via co-precipitation from Mg/Al nitrate at pH=9.6. Characterization was performed using X-ray powder diffraction (XRD), small angle X-ray scattering (SAXS), elemental analysis, infrared spectroscopy (IR) and thermogravimetry (TG). From XRD and SAXS measurements, a d-value of ~5.0 nm was identified for the basal spacing of the Mg2Al-cellulase-LDH. Consequently, the cellulase enzyme (hydrodynamic diameter ~6.6 nm) attains a slightly compressed conformation when intercalated. Formation of the LDH hybrid was also confirmed via scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mg2Al-cellulase-LDH phases appear as ~20 nm thin foils which are intergrown to flower-like aggregates. Activity of the enzyme was retained after deintercalation from the Mg2Al-LDH framework using anion exchange. Accordingly, cellulase is not denatured during the intercalation process, and LDH presents a suitable host structure for time-controlled release of the biomolecule.

CTAB-assisted hydrothermal synthesis of YVO 4:Eu 3+ powders in a wide pH range

NASA Astrophysics Data System (ADS)

Wang, Juan; Hojamberdiev, Mirabbos; Xu, Yunhua

2012-01-01

Rhombus-, rod-, soya bean- and aggregated soya bean-like YVO 4:Eu 3+ micro- and nanostructures were synthesized by a cetyltrimethylammonium bromide (CTAB)-assisted hydrothermal method at 180 °C for 24 h in a wide pH range. The as-synthesized powders were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL). The XRD results confirmed the formation of phase-pure YVO 4:Eu 3+ powders with tetragonal structure under hydrothermal process in a wide pH range. Electron microscopic observations evidenced the morphological transformation of YVO 4:Eu 3+ powders from rhombus-like microstructure to rod-, soya bean, and aggregated soya bean-like nanostructures with an increase in the pH of the synthesis solution. The results from the PL measurements revealed that the intensities of PL emission peaks were significantly affected by the morphologies and crystallinity of samples due to the absence of an inversion symmetry at the Eu 3+ lattice site, and the highest luminescence intensity was observed for rod-like YVO 4:Eu 3+ powders.

One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex

PubMed Central

Barakat, Assem; Al-Noaimi, Mousa; Suleiman, Mohammed; Aldwayyan, Abdullah S.; Hammouti, Belkheir; Ben Hadda, Taibi; Haddad, Salim F.; Boshaala, Ahmed; Warad, Ismail

2013-01-01

[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM). PMID:24351867

Influence of the synthesis parameters on the properties of amidoxime grafted sepiolite nanocomposites

NASA Astrophysics Data System (ADS)

Taimur, Shaista; Yasin, Tariq

2017-11-01

Novel polyacrylonitrile (PAN) grafted sepiolite nanocomposites were synthesized via emulsion polymerization. The influence of synthesis parameters on the degree of grafting was studied by varying the concentrations of monomer, initiator and surfactant. The nitrile groups of PAN were chemically modified into amidoxime. Both the grafting and amidoxime percentages were determined gravimetrically and maximum grafting of 373% was achieved at 5% acrylonitrile, 1% surfactant and 0.1% initiator concentrations. The presence of vibration at 2242 cm-1 in Fourier transform infrared (FT-IR) spectrum and x-ray diffraction (XRD) reflection at 2θ = 16.9° (010) confirmed the grafting of PAN chains onto modified sepiolite. XRD patterns also indicated a decrease in crystallinity of sepiolite and appearance of new amorphous region in grafted nanocomposites. The morphological changes of sepiolite during silanization and grafting of PAN is also confirmed by field emission scanning electron microscope (FESEM). Transmission electron microscope (TEM) images clearly showed the shortening of fibers after silanization of sepiolite and the same were involved in heterogeneous nucleation in micelles. These developed amidoxime grafted sepiolite nanocomposites can be used as adsorbent for the metal recovery.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Oleic acid coated magnetic nano-particles: Synthesis and characterizations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Panda, Biswajit, E-mail: bpanda@mes.ac.in; Goyal, P. S.

2015-06-24

Magnetic nano particles of Fe{sub 3}O{sub 4} coated with oleic acid were synthesized using wet chemical route, which involved co-precipitation of Fe{sup 2+} and Fe{sup 3+} ions. The nano particles were characterized using XRD, TEM, FTIR, TGA and VSM. X-ray diffraction studies showed that nano particles consist of single phase Fe{sub 3}O{sub 4} having inverse spinel structure. The particle size obtained from width of Bragg peak is about 12.6 nm. TEM analysis showed that sizes of nano particles are in range of 6 to 17 nm with a dominant population at 12 - 14 nm. FTIR and TGA analysis showed that -COOH groupmore » of oleic acid is bound to the surface of Fe{sub 3}O{sub 4} particles and one has to heat the sample to 278° C to remove the attached molecule from the surface. Further it was seen that Fe{sub 3}O{sub 4} particles exhibit super paramagnetism with a magnetization of about 53 emu/ gm.« less

Biomimetics of silver nanoparticles by white rot fungus, Phaenerochaete chrysosporium.

PubMed

Vigneshwaran, Nadanathangam; Kathe, Arati A; Varadarajan, P V; Nachane, Rajan P; Balasubramanya, R H

2006-11-01

Extracellular synthesis of silver nanoparticles by a white rot fungus, Phaenerochaete chrysosporium is reported in this paper. Incubation of P. chrysosporium mycelium with silver nitrate solution produced silver nanoparticles in 24h. These silver nanoparticles were characterized by means of UV-vis spectroscopy, X-ray diffraction analysis, scanning electron microscopy, transmission electron microscopy, and photoluminescence spectroscopy. The synthesized silver nanoparticles absorbed maximum at 470 nm in the visible region. XRD spectrum of the silver nanoparticles confirmed the formation of metallic silver. The SEM characterization of the fungus reacted on the Ag+ indicated that the protein might be responsible for the stabilization of silver nanoparticles. This result was further supported by the TEM examination. Though shape variation was noticed, majority of the nanoparticles were found to be of pyramidal shape as seen under TEM. Photoluminescence spectrum showed a broad emission peak of silver nanoparticles at 423 nm when excited at 350 nm. Apart from eco-friendliness, fungus as bio-manufacturing unit will give us an added advantage in ease of handling when compared to other classes of microorganisms.

Optoelectronic and Electrochemical Properties of Vanadium Pentoxide Nanowires Synthesized by Vapor-Solid Process

PubMed Central

Pan, Ko-Ying; Wei, Da-Hua

2016-01-01

Substantial synthetic vanadium pentoxide (V2O5) nanowires were successfully produced by a vapor-solid (VS) method of thermal evaporation without using precursors as nucleation sites for single crystalline V2O5 nanowires with a (110) growth plane. The micromorphology and microstructure of V2O5 nanowires were analyzed by scanning electron microscope (SEM), energy-dispersive X-ray spectroscope (EDS), transmission electron microscope (TEM) and X-ray diffraction (XRD). The spiral growth mechanism of V2O5 nanowires in the VS process is proved by a TEM image. The photo-luminescence (PL) spectrum of V2O5 nanowires shows intrinsic (410 nm and 560 nm) and defect-related (710 nm) emissions, which are ascribable to the bound of inter-band transitions (V 3d conduction band to O 2p valence band). The electrical resistivity could be evaluated as 64.62 Ω·cm via four-point probe method. The potential differences between oxidation peak and reduction peak are 0.861 V and 0.470 V for the first and 10th cycle, respectively. PMID:28335268

Tetraethylorthosilicate (TEOS) applied in the surface modification of hydroxyapatite to develop polydimethylsiloxane/hydroxyapatite composites.

PubMed

Bareiro, O; Santos, L A

2014-03-01

Nanometric hydroxyapatite (HAp) particles were modified with 5 or 10 wt.% tetraethylorthosilicate (TEOS) solutions in order to prepare polydimethylsiloxane/hydroxyapatite (PDMS/HAp) composites. The surface modification of the HAp particles was studied by transmission electron spectroscopy (TEM) and by scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDS) equipment. The dispersion state of the modified particles in the PDMS matrix was also assessed by SEM. The composite phase composition was characterized by X-ray diffraction (XRD). The composite thermodynamic parameters of cross-linking were analyzed by differential scanning calorimetry (DSC). TEM micrographs and EDS spectra indicated evidence of silica-coating formation on the surface of modified HAp particles. SEM results showed that the HAp particles formed agglomerates in the PDMS matrix. It was found that the introduction of HAp particles into the PDMS changed the enthalpy of cross-linking and the temperature of the beginning of the cross-linking reaction. EDS results indicated that the surface modification of HAp produced composites showing thermodynamic parameters that were more similar to those of unfilled PDMS. Copyright © 2013 Elsevier B.V. All rights reserved.

Structural, microstructural and vibrational analyses of the monoclinic tungstate BiLuWO6

NASA Astrophysics Data System (ADS)

Ait Ahsaine, H.; Taoufyq, A.; Patout, L.; Ezahri, M.; Benlhachemi, A.; Bakiz, B.; Villain, S.; Guinneton, F.; Gavarri, J.-R.

2014-10-01

The bismuth lutetium tungstate phase BiLuWO6 has been prepared using a solid state route with stoichiometric mixtures of oxide precursors. The obtained polycrystalline phase has been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. In the first step, the crystal structure has been refined using Rietveld method: the crystal cell was resolved using monoclinic system (parameters a, b, c, β) with space group A2/m. SEM images showed the presence of large crystallites with a constant local nominal composition (BiLuW). TEM analyses showed that the actual local structure could be better represented by a superlattice (a, 2b, c, β) associated with space groups P2 or P2/m. The Raman spectroscopy showed the presence of vibrational bands similar to those observed in the compounds BiREWO6 with RE=Y, Gd, Nd. However, these vibrational bands were characterized by large full width at half maximum, probably resulting from the long range Bi/Lu disorder and local WO6 octahedron distortions in the structure.

Nanostructures formed by cyclodextrin covered procainamide through supramolecular self assembly - Spectral and molecular modeling study

NASA Astrophysics Data System (ADS)

Rajendiran, N.; Mohandoss, T.; Sankaranarayanan, R. K.

2015-02-01

Inclusion complexation behavior of procainamide (PCA) with two cyclodextrins (α-CD and β-CD) were analyzed by absorption, fluorescence, scanning electron microscope (SEM), transmission electron microscope (TEM), Raman image, FT-IR, differential scanning colorimeter (DSC), Powder X ray diffraction (XRD) and 1H NMR. Blue shift was observed in β-CD whereas no significant spectral shift observed in α-CD. The inclusion complex formation results suggest that water molecules also present in the inside of the CD cavity. The present study revealed that the phenyl ring of the PCA drug is entrapped in the CD cavity. Cyclodextrin studies show that PCA forms 1:2 inclusion complex with α-CD and β-CD. PCA:α-CD complex form nano-sized particles (46 nm) and PCA:β-CD complex form self-assembled to micro-sized tubular structures. The shape-shifting of 2D nanosheets into 1D microtubes by simple rolling mechanism were analysed by micro-Raman and TEM images. Thermodynamic parameters (ΔH, ΔG and ΔS) of inclusion process were determined from semiempirical PM3 calculations.

Microstructure evolution of Al-doped zinc oxide films prepared by in-line reactive mid-frequency magnetron sputtering

NASA Astrophysics Data System (ADS)

Hong, R. J.; Jiang, X.

2006-07-01

Aluminium-doped zinc oxide (ZnO:Al or AZO) thin films were deposited on glass substrates by reactive mid-frequency (MF) magnetron sputtering from Zn/Al metallic targets. Strong (002) preferred orientation was detected by X-ray diffraction (XRD). It was observed by plan-view transmission electron microscopy (TEM) that an AZO film deposited at low substrate temperature was composed of irregular large grains; but the film prepared at high temperature was composed of moderate sized grains with a regular shape. A secondary phase of ZnO2 was also observed for the film deposited at low substrate temperature. The cross-sectional TEM study of the AZO film showed that prior to the well-aligned columnar growth an initial interfacial zone with nano crystallites were formed. The nano crystallites formed initially with a large tilt angle normal to the substrate surface and during the growth of the transition zone, the tilt angle decreased until it vanished. The evolution of the film structure is discussed in terms of evolutionary selection model and the dynamic deposition process.

Direct synthesis of carbon nanofibers from South African coal fly ash

NASA Astrophysics Data System (ADS)

Hintsho, Nomso; Shaikjee, Ahmed; Masenda, Hilary; Naidoo, Deena; Billing, Dave; Franklyn, Paul; Durbach, Shane

2014-08-01

Carbon nanofibers (CNFs), cylindrical nanostructures containing graphene, were synthesized directly from South African fly ash (a waste product formed during the combustion of coal). The CNFs (as well as other carbonaceous materials like carbon nanotubes (CNTs)) were produced by the catalytic chemical vapour deposition method (CCVD) in the presence of acetylene gas at temperatures ranging from 400°C to 700°C. The fly ash and its carbonaceous products were characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), laser Raman spectroscopy and Brunauer-Emmett-Teller (BET) surface area measurements. It was observed that as-received fly ash was capable of producing CNFs in high yield by CCVD, starting at a relatively low temperature of 400°C. Laser Raman spectra and TGA thermograms showed that the carbonaceous products which formed were mostly disordered. Small bundles of CNTs and CNFs observed by TEM and energy-dispersive spectroscopy (EDS) showed that the catalyst most likely responsible for CNF formation was iron in the form of cementite; X-ray diffraction (XRD) and Mössbauer spectroscopy confirmed these findings.

Fabrication, ultra-structure characterization and in vitro studies of RF magnetron sputter deposited nano-hydroxyapatite thin films for biomedical applications

NASA Astrophysics Data System (ADS)

Surmeneva, Maria A.; Surmenev, Roman A.; Nikonova, Yulia A.; Selezneva, Irina I.; Ivanova, Anna A.; Putlyaev, Valery I.; Prymak, Oleg; Epple, Matthias

2014-10-01

A series of nanostructured low-crystalline hydroxyapatite (HA) coatings averaging 170, 250, and 440 nm in thickness were deposited onto previously etched titanium substrates through radio-frequency (RF) magnetron sputtering. The HA coatings were analyzed using infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). Cross sections of the thin specimens were prepared by FIB to study the microstructure of the coatings by TEM. The deposition process formed nano-scale grains, generating an amorphous layer at the substrate/coating interface and inducing the growth of a columnar grain structure perpendicular to the substrate surface. A microstructural analysis of the film confirmed that the grain size and crystallinity increased when increasing the deposition time. The nanostructured HA coatings were not cytotoxic, as proven by in vitro assays using primary dental pulp stem cells and mouse fibroblast NCTC clone L929 cells. Low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules on the surface better than uncoated titanium substrates.

Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles.

PubMed

Kuśnieruk, Sylwia; Wojnarowicz, Jacek; Chodara, Agnieszka; Chudoba, Tadeusz; Gierlotka, Stanislaw; Lojkowski, Witold

2016-01-01

Hydroxyapatite (HAp) nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis (MHS). The following parameters of the obtained nanostructured HAp were determined: pycnometric density, specific surface area, phase purity, lattice parameters, particle size, particle size distribution, water content, and structure. HAp nanoparticle morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction measurements confirmed crystalline HAp was synthesized, which was pure in terms of phase. It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. The average diameter of the HAp nanoparticles was determined by Scherrer's equation via the Nanopowder XRD Processor Demo web application, which interprets the results of specific surface area and TEM measurements using the dark-field technique. The obtained nanoparticles with average particle diameter ranging from 8-39 nm were characterized by having homogeneous morphology with a needle shape and a narrow particle size distribution. Strong similarities were found when comparing the properties of some types of nanostructured hydroxyapatite with natural occurring apatite found in animal bones and teeth.

Diffraction properties of opaque disks outside and inside a laser cavity

NASA Astrophysics Data System (ADS)

de Saint Denis, Renaud; Passilly, Nicolas; Fromager, Michael; Cagniot, Emmanuel; Ait-Ameur, Kamel

2008-02-01

Diffraction of symmetrical Laguerre-Gauss TEMp0 beams incident on an opaque disk known as a stop is considered. The near- and far-field patterns are studied. Thanks to zero-field occluding, conversion from TEM10 beam to dark hollow beam can be achieved with better efficiency than from a TEM00 beam. It is shown that the fundamental mode of a laser cavity including a diaphragm and a stop can be TEM00- or TEM10-like in shape depending on their size. This result is interpreted from the new divergence hierarchy, which characterises the diffracted TEMp0 beams emerging from the stop.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise.

PubMed

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R; Thorogood, Gordon; Nelwamondo, Aubrey N; Ntsoane, Tshepo P; Roberts, Sarah K; Holliday, Kiel S

2018-01-01

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE PAGES

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; ...

2018-01-24

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Synthesis of Cu/CuO nanoparticles in mesoporous material by solid state reaction

NASA Astrophysics Data System (ADS)

Sohrabnezhad, Sh.; Valipour, A.

2013-10-01

The Mobil Composition of Matter No. 41 (MCM-41) containing 1.0 and 5.0 wt.% of Cu was synthesized under solid state reaction. The calcinations of samples were done at two different temperatures, 500 and 300 °C. X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM) were used for samples characterization. Powder X-ray diffraction showed that when Cu(CH3COO)2 content is about 1.0 wt.% in Cu/MCM-41, the guest CuO-NPs and copper ions is formed on the silica channel wall, and more exists in the crystalline state. When Cu(CH3COO)2 content exceeds this value (5.0 wt.%), CuO nanoparticles and Cu2+ ions can be observed in low crystalline state. From the diffuse reflectance spectra it was confirmed that 5 wt.% Cu/MCM-41 sample calcined at 500 °C show plasmon resonance band due to Cu nanoparticles in the range between 500 and 600 nm and small copper clusters Cun in 450 nm. It also shows that some of the Cu2+ ions are present octahedrally in extraframework position in all samples. Both fourier transform infrared and diffuse reflectance spectra indicate that some of Cu2+ ions are tetrahedrally within the framework position in 1 wt.% Cu/MCM-41 samples. TEM images indicated that nanoparticles size of CuO is in range of 30-40 nm.

Ionic liquid-assisted preparation of square-shaped Y{sub 2}O{sub 3} nanoplates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Lei; Fang, Hao; Xu, Hualan

Highlights: • Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets were prepared by an ionic liquid-assisted mixed solvothermal route. • Y{sub 2}O{sub 3} nanosheets were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets. • The Y{sub 2}O{sub 3} nanosheets are with length of about 300 nm and thickness of several nanometers. - Abstract: Uniform square-shaped Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates with side length of about 300 nm and thickness of tens of nanometers have been successfully prepared by an ionic liquid-assisted mixed solvothermal route. Y{sub 2}O{sub 3} nanoplates with similar size were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates atmore » 800 °C. The products were analyzed by powder X-ray diffraction (XRD), thermogravimetric analysis (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM), and electron diffraction (ED). The effects of reaction time, composition of solvents, and the molar ratio of reagents on the morphology of the products have been investigated. The possible formation mechanism of the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates was also discussed. Y{sub 2}O{sub 3}:Eu{sup 3+} nanoplates were also synthesized and their photoluminescent properties were examined.« less

Photocatalytic characteristics of single phase Fe-doped anatase TiO{sub 2} nanoparticles sensitized with vitamin B{sub 12}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gharagozlou, Mehrnaz, E-mail: gharagozlou@icrc.ac.ir; Bayati, R.

Highlights: • Anatase TiO{sub 2}/B{sub 12} hybrid nanostructured catalyst was successfully synthesized by sol–gel technique. • The nanoparticle catalyst was doped with iron at several concentrations. • Nanoparticles were characterized in detail by XRD, Raman, TEM, EDS, and spectroscopy techniques. • The formation mechanism and role of point defects on photocatalytic properties were discussed. • A structure-property-processing correlation was established. - Abstract: We report a processing-structure-property correlation in B{sub 12}-anatase titania hybrid catalysts doped with several concentrations of iron. Our results clearly show that low-level iron doping alters structure, defect content, and photocatalytic characteristics of TiO{sub 2}. XRD and Ramanmore » studies revealed formation of a single-phase anatase TiO{sub 2} where no iron based segregation in particular iron oxide, was detected. FT-IR spectra clearly confirmed sensitization of TiO{sub 2} nanoparticles with vitamin B{sub 12}. TEM micrographs and diffraction patterns confirmed crystallization of anatase nanoparticles with a radius of 15–20 nm. Both XRD and Raman signals showed a peak shift and a peak broadening which are surmised to originate from creation of point defects, namely oxygen vacancy and titanium interstitial. The doped samples revealed a narrower band gap as compared to undoped samples. Photocatalytic activity of the samples was assessed through measuring the decomposition rate of rhodamine B. It was found that sensitization with vitamin B{sub 12} and Fe-doping significantly enhances the photocatalytic efficiency of the anatase nanoparticles. We also showed that there is an optimum Fe-doping level where the maximum photocatalytic activity is achieved. The boost of photocatalytic activity was qualitatively understood to originate from a more effective use of the light photons, formation of point defects, which enhance the charge separation, higher carrier mobility.« less

Austenite-martensite transformation in electrodeposited Fe70Pd30 NWs: a step towards making bio-nano-actuators tested on in vivo systems

NASA Astrophysics Data System (ADS)

Zuzek Rozman, K.; Pecko, D.; Trafela, S.; Samardzija, Z.; Spreitzer, M.; Jaglicic, Z.; Nadrah, P.; Zorko, M.; Bele, M.; Tisler, T.; Pintar, A.; Sturm, S.; Kostevsek, N.

2018-03-01

Fe69±3Pd31±3 nanowires (NWs) with lengths of a few microns and diameters of 200 nm were synthesized via template-assisted pulsed electrodeposition into alumina-based templates. The as-deposited Fe69±3Pd31±3 NWs exhibited α-Fe (bcc-solid solution of Fe, Pd) nanocrystalline structure as seen from the x-ray diffraction (XRD), that got confirmed by transmission electron microscopy (TEM) with some larger grains up 50 nm observed. Annealing of the as-deposited Fe69±3Pd31±3 NWs at 1173 K/45 min was followed by quenching in ice water and resulted in a transformation to the fcc crystal structure (XRD) with grain sizes up to 200 nm (TEM). To induce the austenite-to-martensite, i.e., fcc-to-fct phase transformation the fcc Fe69±3Pd31±3 NWs were cooled to 73 K. The XRD showed the disappearance of the (200) fcc reflection (at room temperature) and the appearance of the (200) fct reflection (at 73 K), confirming the fcc-to-fct transformation took place. The magnetic measurements revealed that the fcc Fe69±3Pd31±3 NWs measured at low temperatures (50 K) had a larger coercivity than at room temperature, which suggests the fct phase was present in the undercooled state, exhibiting a larger magnetocrystalline anisotropy than the fcc phase present at room temperature. As part of our interest in magnetic-shape-memory actuators, the as-deposited Fe69±3Pd31±3 NWs were tested for toxicity on zebrafish. In vivo tests showed no acute lethal or sub-lethal effects, which implies that the Fe69±3Pd31±3 NWs have the potential to be used as nano-actuators in biomedical applications.

Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

NASA Astrophysics Data System (ADS)

Cheng, Gang; Yang, Hanmin; Rong, Kaifeng; Lu, Zhong; Yu, Xianglin; Chen, Rong

2010-08-01

Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2CO 3) is one of commonly used antibacterial agents against Helicobacter pylori ( H. pylori). Different (BiO) 2CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2CO 3 nanostructures. The possible formation mechanism of different (BiO) 2CO 3 nanostructures fabricated under different conditions was also discussed.

Mesoporous activated carbon from corn stalk core for lithium ion batteries

NASA Astrophysics Data System (ADS)

Li, Yi; Li, Chun; Qi, Hui; Yu, Kaifeng; Liang, Ce

2018-04-01

A novel mesoporous activated carbon (AC) derived from corn stalk core is prepared via a facile and effective method which including the decomposition and carbonization of corn stalk core under an inert gas atmosphere and further activation process with KOH solution. The mesoporous activated carbon (AC) is characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) measurements. These biomass waste derived from activated carbon is proved to be promising anode materials for high specific capacity lithium ion batteries. The activated carbon anode possesses excellent reversible capacity of 504 mAh g-1 after 100 cycles at 0.2C. Compared with the unactivated carbon (UAC), the electrochemical performance of activated carbon is significantly improved due to its mesoporous structure.

Piper betle-mediated synthesis, characterization, antibacterial and rat splenocyte cytotoxic effects of copper oxide nanoparticles.

PubMed

Praburaman, Loganathan; Jang, Jum-Suk; Muthusamy, Govarthanan; Arumugam, Sengottaiyan; Manoharan, Koildhasan; Cho, Kwang-Min; Min, Cho; Kamala-Kannan, Seralathan; Byung-Taek, Oh

2016-09-01

The study reports a simple, inexpensive, and eco-friendly synthesis of copper oxide nanoparticles (CuONPs) using Piper betle leaf extract. Formation of CuONPs was confirmed by UV-visible spectroscopy at 280 nm. Transmission electron microscopy (TEM) images showed that the CuONPs were spherical, with an average size of 50-100 nm. The scanning electron microscopy (SEM)-energy dispersive spectroscopy (EDS) peak was observed approximately at 1 and 8 keV. The X-ray diffraction (XRD) studies indicated that the particles were crystalline in nature. CuONPs effectively inhibited the growth of phytopathogens Ralstonia solanacearum and Xanthomonas axonopodis. The cytotoxic effect of the synthesized CuONPs was analyzed using rat splenocytes. The cell viability was decreased to 94% at 300 μg/mL.

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Synthesis of copper nanocolloids using a continuous flow based microreactor

NASA Astrophysics Data System (ADS)

Xu, Lei; Peng, Jinhui; Srinivasakannan, C.; Chen, Guo; Shen, Amy Q.

2015-11-01

The copper (Cu) nanocolloids were prepared by sodium borohydride (NaBH4) reduction of metal salt solutions in a T-shaped microreactor at room temperature. The influence of NaBH4 molar concentrations on copper particle's diameter, morphology, size distribution, and elemental compositions has been investigated by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The ultraviolet-visible spectroscopy (UV-vis) was used to verify the chemical compounds of nanocolloids and estimate the average size of copper nanocolloids. The synthesized copper nanocolloids were uniform in size and non-oxidized. A decrease in the mean diameter of copper nanocolloids was observed with increasing NaBH4 molar concentrations. The maximum mean diameter (4.25 nm) occurred at the CuSO4/NaBH4 molar concentration ratio of 1:2.

Simultaneous Surface Modification and Chemical Reduction of Graphene Oxide Using Glucose.

PubMed

Pan, Hui; Liu, Ruiqi; Li, Guanglong; Wang, Xiaodong; Ding, Tao

2018-05-01

In this paper, we develop a simple and facile approach to prepare graphene nanosheets through chemical reduction with glucose as reducing agent and modification agent. The reduced and modified graphene by glucose (denoted as g-rGO) was characterized with techniques of Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Raman spectra, scanning electron microscopy (SEM) and transmission electron microscopy (TEM), etc. It is found that, besides the desired reduction capability to graphene oxide (denoted as GO), glucose plays an important role as a modifying reagent in stabilizing the as-prepared graphene nanosheets simultaneously and the g-rGO exhibits good dispersibility and stability in water and waterborne polyurethane matrix (denoted as WPU). Moreover, the g-rGO can improve evidently the mechanical properties, weather ability and water resistance of WPU.

Tetrapeptide-coumarin conjugate 3D networks based on hydrogen-bonded charge transfer complexes: gel formation and dye release.

PubMed

Guo, Zongxia; Gong, Ruiying; Jiang, Yi; Wan, Xiaobo

2015-08-14

Oligopeptide-based derivatives are important synthons for bio-based functional materials. In this article, a Gly-(L-Val)-Gly-(L-Val)-coumarin (GVGV-Cou) conjugate was synthesized, which forms 3D networks in ethanol. The gel nanostructures were characterized by UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), SEM and TEM. It is suggested that the formation of charge transfer (CT) complexes between the coumarin moieties is the main driving force for the gel formation. The capability of the gel to encapsulate and release dyes was explored. Both Congo Red (CR) and Methylene Blue (MB) can be trapped in the CT gel matrix and released over time. The present gel might be used as a functional soft material for guest encapsulation and release.

Depositing of CuS nanocrystals upon the graphene scaffold and their photocatalytic activities

NASA Astrophysics Data System (ADS)

Wang, Yongbin; Zhang, Lixin; Jiu, Hongfang; Li, Na; Sun, Yixin

2014-06-01

A series of copper sulfide nanocrystals/graphene nanocomposites (CuS/GR) with different weight ratios of GR were fabricated via a one-step hydrothermal approach by using dimethylsulfoxide (DMSO) as the source of sulfur and solvent. The as-prepared samples were studied by X-ray diffraction (XRD), UV-vis diffuse reflectance spectra (DRS), transmission scanning electron microscopy (TEM) and photoluminescence spectra (PL) are employed to determine the properties of the samples. The results show that the CuS nanocrystals with an average size of 16 nm almost overspread on the GR graphene scaffold. The samples exhibit excellent photocatalytic activities in degrading the methylene blue (MB) compared with pure CuS. This work shows that CuS/GR nanocomposites would be promising in dye wastewater treatment as Fenton-like reagents.

Influence of Synthesis Temperature on the Growth and Surface Morphology of Co3O4 Nanocubes for Supercapacitor Applications

PubMed Central

Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

2017-01-01

A facile hydrothermal route to control the crystal growth on the synthesis of Co3O4 nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co3O4 nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co3O4 synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes. PMID:29088061

Rapid preparation process of antiparkinsonian drug Mucuna pruriens silver nanoparticle by bioreduction and their characterization

PubMed Central

Arulkumar, Subramanian; Sabesan, Muthukumaran

2010-01-01

Backgorund: Development of biologically inspired experimental processes for the synthesis of nanoparticles is evolving an important branch of nanotechnology. Methods: The bioreduction behavior of plant seed extract of Mucuna pruriens in the synthesis of silver nanoparticles was investigated employing UV/visible spectrophotometry, X-ray diffraction (XRD), and transmission electron microscopy (TEM), Fourier transform – infra red (FT- IR). Result: M. pruriens was found to exhibit strong potential for rapid reduction of silver ions. The formation of nanoparticles by this method is extremely rapid, requires no toxic chemicals, and the nanoparticles are stable for several months. Conclusion: The main conclusion is that the bioreduction method to produce nanoparticles is a good alternative to the electrochemical methods and it is expected to be biocompatible. PMID:21808573

Synthesis, characterization, in vitro anti-proliferative and hemolytic activity of hydroxyapatite.

PubMed

Palanivelu, R; Ruban Kumar, A

2014-06-05

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP) nanoparticles are widely used in several biomedical applications due to its compositional similarities to bone mineral, excellent biocompatibility and bioactivity, osteoconductivity. In this present investigation, HAP nanoparticles synthesized by precipitation technique using calcium nitrate and di-ammonium phosphate. The crystalline nature and the functional group analysis are confirmed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Fourier transform Raman spectroscopy (FT-Raman) respectively. The morphological observations are ascertained from field emission electron scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). In vitro anti-proliferative and hemolytic activities are carried out on the synthesized HAP samples and the studies reveals that HAP have mild activity against erythrocytes. Copyright © 2014 Elsevier B.V. All rights reserved.

Removal of Carmine from Aqueous Solution by Carbonated Hydroxyapatite Nanorods

PubMed Central

Liu, Guanxiong; Xue, Caibao; Zhu, Peizhi

2017-01-01

In this study, carbonated hydroxyapatite (CHA) nanorods were prepared by a novel hydrothermal method. The crystallinity and chemical structure of synthesized CHA nanorods was characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), respectively. Carmine was selected as representative organic dyes to study the adsorption capacities of CHA nanorods. Mechanistic studies of carmine adsorption by CHA nanorods show that the adsorption processes both follow the pseudo-second-order kinetic model and fit the Langmuir isotherm model well. The CHA nanorods exhibited a high adsorption capacity of 85.51 mg/g for carmine at room-temperature. The experimental results prove that CHA nanorods can be promising absorbents for removing organic dye pollutants in wastewater from paper and textile plants. PMID:28587250

TEA controllable preparation of magnetite nanoparticles (Fe3O4 NPs) with excellent magnetic properties

NASA Astrophysics Data System (ADS)

Han, Chengliang; Zhu, Dejie; Wu, Hanzhao; Li, Yao; Cheng, Lu; Hu, Kunhong

2016-06-01

A fast and controllable synthesis method for superparamagnetic magnetite nanoparticles (Fe3O4 NPs) was developed in Fe(III)-triethanolamine (TEA) solution. The phase structure, morphology and particle size of the as-synthesized samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the magnetic particles were pure Fe3O4 with mean sizes of approximately 10 nm. The used TEA has key effects on the formation of well dispersing Fe3O4 NPs. Vibrating sample magnetometer (VSM) result indicated that the as-obtained Fe3O4 NPs exhibited superparamagnetic behavior and the saturation magnetization (Ms) was about 70 emu/g, which had potential applications in magnetic science and technology.

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

NASA Technical Reports Server (NTRS)

Ren, Z. F.; Wang, C. A.; Wang, J. H.; Miller, D. J.; Goretta, K. C.

1995-01-01

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Room temperature ferromagnetism in Mg-doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Jaspal, E-mail: jaspal0314@gmail.com; Vashihth, A.; Gill, Pritampal Singh

Zn{sub 1-x}Mg{sub x}O (x = 0, 0,10) nanoparticles were successfully synthesized using sol-gel method. X-ray diffraction (XRD) confirms that the synthesized nanoparticles possess wurtzite phase having hexagonal structure. Morphological analysis was carried out using transmission electron microscopy (TEM) which depicts the spherical morphology of ZnO nanoparticles. Energy dispersive spectroscopy (EDS) showed the presence of Mg in ZnO nanoparticles. Electron spin resonance (ESR) signal was found to be decreasing with increasing of Mg-doping concentration. The room temperature ferromagnetism was observed in undoped and Mg-doped ZnO nanoparticles. The increase of Mg-doping concentration resulted in decrease of saturation magnetization value which could bemore » attributed to decrease of oxygen vacancies present in host nanoparticles.« less

Atmospheric pressure chemical vapor deposition: an alternative route to large-scale MoS2 and WS2 inorganic fullerene-like nanostructures and nanoflowers.

PubMed

Li, Xiao-Lin; Ge, Jian-Ping; Li, Ya-Dong

2004-11-19

Large-scale MoS2 and WS2 inorganic fullerene-like (IF) nanostructures (onionlike nanoparticles, nanotubes) and elegant three-dimensional nanoflowers (NF) have been selectively prepared through an atmospheric pressure chemical vapor deposition (APCVD) process with the reaction of chlorides and sulfur. The morphologies were controlled by adjusting the deposition position, the deposition temperature, and the flux of the carrier gas. All of the nanostructures have been characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). A reaction mechanism is proposed based on the experimental results. The surface area of MoS2 IF nanoparticles and the field-emission effect of as-prepared WS2 nanoflowers is reported.

Synthesis of Bimetallic Platinum Nanoparticles for Biosensors

PubMed Central

Leteba, Gerard M.; Lang, Candace I.

2013-01-01

The use of magnetic nanomaterials in biosensing applications is growing as a consequence of their remarkable properties; but controlling the composition and shape of metallic nanoalloys is problematic when more than one precursor is required for wet chemistry synthesis. We have developed a successful simultaneous reduction method for preparation of near-spherical platinum-based nanoalloys containing magnetic solutes. We avoided particular difficulties in preparing platinum nanoalloys containing Ni, Co and Fe by the identification of appropriate synthesis temperatures and chemistry. We used transmission electron microscopy (TEM) to show that our particles have a narrow size distribution, uniform size and morphology, and good crystallinity in the as-synthesized condition. Energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) confirms the coexistence of Pt with the magnetic solute in a face-centered cubic (FCC) solid solution. PMID:23941910

One-pot catalytic conversion of cellulose into polyols with Pt/CNTs catalysts.

PubMed

Yang, Li; Yan, Xiaopei; Wang, Qiwu; Wang, Qiong; Xia, Haian

2015-03-02

A series of Pt nanoparticles supported on carbon nanotubes (CNTs) were synthesized using the incipient-wetness impregnation method. These catalysts were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscope (TEM) techniques. The characterization results indicate that the Pt nanoparticles were highly dispersed on the surface of the CNTs, and the mean size was less than 5 nm. These catalysts were utilized to convert cellulose to hexitol, ethylene glycerol (EG), and 1,2-propylene glycol (1,2-PG) under low H2 pressure. The total yields were as high as 71.4% for EG and 1,2-PG using 1Pt/CNTs as the catalyst in the hydrolytic hydrogenation of cellulose under mild reaction conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.