IMPEDANCE SPECTROSCOPY (IS), XRD AND SEM OF OXIDE-ADDED Si3N4

2002 ◽  
Vol 16 (14) ◽  
pp. 525-537
Author(s):  
SAADAT. A. SIDDIQI ◽  
NASIR A. KHAN ◽  
M. SABIEH ANWAR

Impedance spectroscopy (IS) is a non-destructive technique used for obtaining valuable information about bulk conductivities, dielectric constants, phase composition and grain boundaries of important ceramic materials, amongst many others. We obtained Nyquist plots for four different hot-pressed Si 3 N 4 samples in two different frequency regimes: 1 Hz to 30 MHz and 1 kHz to 100 kHz. The information obtained was compared against results from scanning electron microscopy (SEM) and X-ray diffraction (XRD). The limitations of the frequency response techniques are also discussed.

2013 ◽  
Vol 203-204 ◽  
pp. 133-136
Author(s):  
Anna Góral ◽  
Marek Nowak ◽  
Joanna Wojewoda-Budka

Our interests are focused on the Ni/Al2O3 nanocomposite coatings electrochemically deposited in modified Watt’s-type baths into which α-Al2O3 nanopowder is added on steel substrates. The effect of different amounts of α-Al2O3 phase in the electrolyte baths on microstructure of electrodeposited Ni/Al2O3 coatings is investigated. In order to study the coatings the non-destructive X-ray diffraction techniques are applied. As indirect techniques, they are supported by imaging methods, especially scanning electron microscopy.


1997 ◽  
Vol 500 ◽  
Author(s):  
P. Mondal ◽  
H. Hahn

ABSTRACTImpedance Spectroscopy, X-Ray Diffraction and High Resolution Scanning Electron Microscopy have been used to study the effect of extremely fine grain size on electrical properties such as dc-conductivity and activation energies in nanocrystalline Y-stabilized tetragonal zirconia. The samples were prepared from powders produced by the Inert Gas condensation method. X-Ray Diffraction was used to characterize phase and average grain size of the sample. In addition, grain size and microstructure of the sample was examined using High Resolution Scanning Electron Microscopy. With Impedance Spectroscopy relaxations of O−2-ions in the lattice and in the grain boundaries could be resolved. The dc-conductivities of the lattice and the grain boundaries were deduced from the data. The activation energies for ac- and dc-conductivity of the lattice and grain boundary relaxation are reported.


Author(s):  
K. Bhagyasree ◽  
Y.Madhava Kumar ◽  
N.O. Gopal ◽  
Ch. Ramu

<div><p><em>This paper reports on structural, morphological and electrical properties of solid polymer electrolyte films based on PVC complexed with different concentrations of VO<sup>2+</sup> using solution cast technique. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and impedance spectroscopy studies. X- ray diffraction (XRD) results revealed that the amorphous nature of PVC polymer matrix increased with the increase of VO<sup>2+</sup> ions concentration. The electrical conductivity was evaluated from impedance spectroscopy studies in the temperature range 303- 373 K and the conductivity was found to increase with increasing dopant concentration. The polymer complexes exhibited Arrhenius type dependence of conductivity with temperature. The variation in film morphology was examined by scanning electron microscopy (SEM).</em></p></div>


DYNA ◽  
2016 ◽  
Vol 83 (195) ◽  
pp. 84-92
Author(s):  
John Deiver Bonilla-Jaimes ◽  
Jose Antonio Henao-Martínez ◽  
Carolina Mendoza-Luna ◽  
Oscar Mauricio Castellanos-Alarcón ◽  
Carlos Alberto Ríos-Reyes

Mediante el uso de la difracción de rayos-X de polvo (DRXP), microdifracción de rayos-X (<span style="font-family: Symbol;">m</span>DXR) y microscopía electrónica de barrido, la caracterización estructural de minerales resulta ser mucho más fiable y precisa. La identificación y cuantificación elemental y composicional de los minerales mediante estas técnicas no destructivas, mejoran la calidad de los resultados y permiten realizar un análisis completo del material. Los datos obtenidos mediante estas técnicas revelaron la presencia de granate tipo espesartina, además de los elementos y compuestos trazas que conforman el material en general. El refinamiento estructural de la espesartina fue realizado mediante el método Rietveld a partir de los datos obtenidos por difracción convencional y con ayuda del software de análisis MDI RIQAS. Con los datos adquiridos por <span style="font-family: Symbol;">m</span>DXR usando un detector de área, un menor tiempo de exposición (comparado con el requerido en detectores 0D y 1D) y sin la necesidad de la disminución del tamaño de partícula del mineral, fue posible la identificación de la espesartina y otros compuestos en menor concentración (mediciones "in situ"). Mediante la combinación de las técnicas de microscopía electrónica de barrido y microdifracción de rayos X, tanto de trabajo desde un punto de vista de la caracterización. El examen por difracción de micro-rayos X no requiere la separación física de la muestra. Usando esta información y las técnicas analíticas avanzadas anteriores, la identificación de granate puede ser mucho más fiable.


Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts

Calcium is an important element in the growth and development of plants and one form of calcium is calcium oxalate. Calcium oxalate has been found in leaf seed, stem material plant tissue culture, fungi and lichen using one or more of the following methods—polarized light microscopy (PLM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction.Two methods are presented here for qualitatively estimating calcium oxalate in dried or fixed tobacco (Nicotiana) leaf from different stalk positions using PLM. SEM, coupled with energy dispersive x-ray spectrometry (EDS), and powder x-ray diffraction were used to verify that the crystals observed in the dried leaf with PLM were calcium oxalate.


Author(s):  
Howard S. Kaufman ◽  
Keith D. Lillemoe ◽  
John T. Mastovich ◽  
Henry A. Pitt

Gallstones contain precipitated cholesterol, calcium salts, and proteins. Calcium (Ca) bilirubinate, palmitate, phosphate, and carbonate occurring in gallstones have variable morphologies but characteristic windowless energy dispersive x-ray (EDX) spectra. Previous studies of gallstone microstructure and composition using scanning electron microscopy (SEM) with EDX have been limited to dehydrated samples. In this state, Ca bilirubinates appear as either glassy masses, which predominate in black pigment stones, or as clusters, which are found mostly in cholesterol gallstones. The three polymorphs of Ca carbonate, calcite, vaterite, and aragonite, have been identified in gallstones by x-ray diffraction, however; the morphologies of these crystals vary in the literature. The purpose of this experiment was to study fresh gallstones by environmental SEM (ESEM) to determine if dehydration affects gallstone Ca salt morphology.Gallstones and bile were obtained fresh at cholecystectomy from 6 patients. To prevent dehydration, stones were stored in bile at 37°C. All samples were studied within 4 days of procurement.


2016 ◽  
Vol 5 (1) ◽  
pp. 6
Author(s):  
Budi Setiawan ◽  
Erizal Zaini ◽  
Salman Umar

Sebuah penelitian tentang sistem dispersi padat dari asiklovir dengan poloxamer 188 telah dilakukan formulasi dengan pencampuran secara fisika dengan rasio 1 : 1, 1 : 3, 1 : 5 dan dispersi padat 1 : 1, 1 : 3, 1 : 5 dan penggilingan 1:1 sebagai pembanding. Dispersi padat dibuat menggunakan metode pencairan (fusi), yang digabung dengan poloxamer 188 pada hotplate kemudian asiklovir dimasukkan ke dalam hasil poloxamer 188 lalu di kocok hingga membentuk masa homogen. Semua formula yang terbentuk termasuk asiklovir poloxamer 188 murni dianalisis karakterisasinya dengan Differential Thermal Analysis (DTA), X-ray Diffraction, Scanning Electron Microscopy (SEM), dan Fourier Transform Infrared (FTIR), kemudian pengambilan dilakukan  (penentuan kadar) mengunakan spektrofotometer UV pada panjang gelombang 257,08 nm dan uji laju disolusi dengan aquadest bebas CO2 menggunakan metode dayung. Hasil pengambilan  (penentuan kadar) menunjukkan bahwa semua formula memenuhi persyaratan farmakope Amerika edisi 30 dan farmakope Indonesia edisi 4 yaitu 95-110%. Sedangkan hasil uji laju disolusi untuk campuran fisik 1: 1, dan dispersi padat 1: 1, dan penggilingan 1: 1 menunjukkan peningkatan yang nyata dibandingkan asiklovir murni. Hal ini juga dapat dilihat dari hasil perhitungan statistik  menggunakan analisis varian satu arah  SPSS 17.


2018 ◽  
Vol 21 (7) ◽  
pp. 495-500 ◽  
Author(s):  
Hassan A. Almarshad ◽  
Sayed M. Badawy ◽  
Abdalkarem F. Alsharari

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.


2021 ◽  
Vol 9 (1) ◽  
Author(s):  
Xiaojian Bai ◽  
Chen Jia ◽  
Zhigen Chen ◽  
Yuxuan Gong ◽  
Huwei Cheng ◽  
...  

AbstractWith exquisite design and unique style, the painted sculptures of Tutang Buddha and two attendants Buddha in Jingyin Temple are precious cultural heritages of China. The sculpture of Tutang Buddha, which was carved from a mound and painted by ancient craftsmen, was rarely found in ancient China. However, due to natural and human factors, the sculptures were severely damaged. Obviously, they require urgent and appropriate protection and restoration. In this study, samples taken from the sculptures were analysed through multiple analytical techniques, including scanning electron microscopy with energy dispersive spectrometry (SEM–EDS), Raman spectroscopy, X-ray diffraction (XRD), optical microscopy (OM) and granulometry. The analysis results enable us to infer the techniques used by the craftsmen in making the sculptures and provide a reliable evidence for the conservation and future protection of these and similar sculptures.


2012 ◽  
Vol 620 ◽  
pp. 314-319
Author(s):  
Nur Amira Mamat Razali ◽  
Fauziah Abdul Aziz ◽  
Saadah Abdul Rahman

Hardwood is wood from angiosperm trees. The characteristic of hardwood include flowers, endosperm within seeds and the production of fruits that contain the seeds. This paper aims to discuss the preparation and characterization of cellulose obtained from hardwood. The hardwood Merbau (Intsia bijuga) was chosen as raw material in this study. Alkaline treatment and delignification methods were used for the preparation of cellulose. Acid hydrolysis was employed to produce cellulose nanocrystal (CNC). The treated and untreated samples were characterized using x-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM). The final product, from both trated and untreated samples were then compared.


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