Studi Difraksi Sinar-X Struktur Nano Seng Oksida (ZnO)

2018 ◽  
Vol 2 (2) ◽  
pp. 53-57
Author(s):  
Suhufa Alfarisa ◽  
Dwi Ahmad Rifai ◽  
Parmin Lumban Toruan

Abstrak – Kajian terhadap difraksi sinar-X struktur nano ZnO dengan waktu sonikasi yang berbeda telah dilakukan menggunakan metode hidrotermal-sonokimia. Variasi waktu sonikasi yang digunakan dalam kajian ini adalah 0 (tanpa sonikasi), 30, 45, dan 60 menit. Pola difraksi sinar-X diplotkan dan dibandingkan untuk mengetahui struktur, kristalinitas dan kemurnian ZnO yang dihasilkan. Estimasi ukuran kristal ZnO juga dihitung menggunakan persamaan Scherrer. Hasil penelitian menunjukkan bahwa struktur nano ZnO yang disintesis tanpa proses sonikasi memiliki kemurnian kristal yang rendah dengan ukuran kristal yang sedang berkisar dari 22,36 – 32,90 nm. Proses sonikasi telah menyebabkan kristalinitas dan kemurnian ZnO meningkat jadi lebih baik. Namun, memperpanjang waktu sonikasi hingga 45 sampai 60 menit menyebabkan membesarnya ukuran kristal ZnO. Waktu sonikasi yang paling optimal adalah 30 menit dimana mampu menghasilkan ZnO dengan kristalinitas dan kemurnian yang baik dan rentang ukuran kristal ZnO yang lebih kecil antara 22,09 – 21,97 nm.                                                                                   Kata kunci: difraksi sinar-X, struktur nano, ZnO, sonikasi, Scherrer Abstract – Research on the X-ray diffraction study of ZnO nanotructure synthesized at different sonication times has been done using hydrothermal-sonochemical method. Sonication variation times that were used in this study were 0 (without sonication), 30, 45, and 60 minutes. The X-ray diffraction patterns were plotted and compared to understand the structure, crystallinity and purity of the resulted ZnO. The estimated crystallite size of ZnO nanostructure were also calculated using Scherrer equation. The results showed that the ZnO nanostructure synthesized without sonication process has a low crystal purity and a fair crystallite size in the range of 22.36 - 32.90 nm. Sonication process has led to a better crystallinity and purity of ZnO. However, longer sonication times up to 45 to 60 minutes has caused to the larger crystal size of ZnO. The most optimum sonication time was found to be 30 minutes which resulted in a good crstallinity and purity of ZnO and smaller crystallite size in the range of 22.09 – 31.97 nm.Key words: X-ray diffraction, nanostructures, ZnO, sonication, Scherrer

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

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


2010 ◽  
Vol 09 (03) ◽  
pp. 215-223 ◽  
Author(s):  
A. A. EL-MELIGI ◽  
A. M. AL-SAIE ◽  
H. AL-BUFLASA ◽  
M. BOUOUDINA

The crystalline semiconductor material (MnPS3) has interlayer d-spacing gap of 6.4 Å. The main advantage of this gap is the ability to accommodate organic and inorganic compounds. Pyridine was intercalated in the MnPS3 interlayer gap under specific conditions. Four phases (d-spacing = 12.48 Å, 10.8 Å, 9.7 Å and 7.3 Å) were observed and the corresponding lattice expansions were determined, 5.8 Å, 4.4 Å, 3.3 Å and 1 Å, respectively. X-ray diffraction patterns of the samples after the experiment were stopped to reveal the presence of three phases together. The phase transformation occurred for the aforementioned phases. The crystallite size of certain phases is within nanorange. The magnetic properties of the materials are affected by the phase transformation. Complete intercalation was confirmed by the XRD and infrared (IR) measurements.


2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Sandra M. Londoño-Restrepo ◽  
Rodrigo Jeronimo-Cruz ◽  
Beatriz M. Millán-Malo ◽  
Eric M. Rivera-Muñoz ◽  
Mario E. Rodriguez-García

1982 ◽  
Vol 26 ◽  
pp. 307-312 ◽  
Author(s):  
D. A. Carpenter ◽  
R. A. Vandermeer

An x-ray diffraction study of the reversible deformation inodes associated with the shape memory effect has been carried out on a series of uranium-niobium alloys near the monotectoid composition (6.2 wt. % Nb). Diffraction patterns were measured as a function of strain, in situ, while the specimens were under stress as part of an attempt to explain the “easy-flow”, low-strain plateau in the stress-strain curve. The alloys, consisting of highly twinned, metastable α” (monoclinic) and γ° (tetragonal) phases derived from the high-temperature BCC γ phase, produced broad, overlapping diffraction lines difficult to analyze by conventional techniques. One solution to this problem was to use a segmented step-scan technique so as to apportion the scan time to concentrate on the most difficult regions. This paper discusses data obtained from an α” alloy and a dual-phase α” + γ° alloy.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1131-C1131
Author(s):  
Alejandro Rodriguez-Navarro ◽  
Krzysztof Kudłacz

Polycrystalline materials properties and behaviour are ultimately determined by their crystallinity, phase composition and microstructure (i.e., crystal size, preferential orientation). Two-dimensional (2D) diffraction patterns collected with an area detector (i.e., CDD), available in modern X-ray diffractometers, contain detailed information about all these important material characteristics. Furthermore, recent advances in detector technologies permits the collection of high resolution diffraction patterns in which the microstructure of the material can be directly imaged. If the size of beam relative to the crystal size in the sample is adequately choosen, the diffraction pattern produced will have spotty rings in which the spots are the diffracted images of individual grains. The resolution of the image is mainly dependent on the characteristics of the X-ray beam (i.e., diameter, angular divergence), which can be modulated by X-ray optics, sample to detector distance, the pixel size of the detector and the sharpness of the point spread function. From these patterns, the crystal size distribution of different crystalline phases present in the sample can be independently determined using specialized software capable of extracting and combining the information contained in these patterns. This technique is applicable to materials with crystal sizes ranging from submicron to mm sizes and is complementary to techniques based on peak profile analyses (i.e., Scherrer method) which are applicable only to nanocrystalline materials. Finally, given the high sensitivity of current detectors, crystal size evolution can be followed in real-time to study important transformation processes such as crystallization, annealing, etc. The use of 2D X-ray diffraction as applied to microstructure characterization will be illustrated through several examples.


Author(s):  
Ricka Prasdiantika ◽  
Niyar Candra Agustin ◽  
Abdul Rohman

This study aims to prepare iron sand, determine the type of iron oxide, and determine the effect of washing iron sand with sonochemical methods. Iron sand samples were obtained from Jomblom Beach, Kendal Regency. Iron sand was separated using an external magnet to obtain magnetic material. The magnetic material obtained was washed using distilled water manually stirred and using the sonochemical method. The material was dried at 80 °C. Material characterization was carried out using X-Ray Fluorescence (XRF) to determine the elements contained in iron sand, Fourier Transform Infrared (FT-IR) Spectrophotometer to identify functional groups in iron sand, X-Ray Diffraction (XRD) to find out the crystal size and crystallinity of iron sand, and the Transmission Electron microscope (TEM) to determine the morphology of iron sand. The characterization results showed that the iron sand of Jomblom Beach contained Fe (72.28%), Ti (7.89%), Al (7.00%), and Si (7.60%). The iron oxide contained in the Jomblom Beach iron sand was dominated by magnetite (Fe3O4). Washing iron sand magnetic material using the sonochemical method increased the composition of the element Fe, increased the crystallinity of the magnetic material, prevented aggregation, and reduced the crystal size of the magnetic material. Magnetic material which was washed using the sonochemical method produced 79.47% Fe element, crystallinity 74.94%, and crystal size 52.78 nm.


1970 ◽  
Vol 48 (23) ◽  
pp. 2852-2856 ◽  
Author(s):  
A. E. Curzon

Electron diffraction patterns obtained with 65 kV electrons (wavelength = 0.0466 Å) from polycrystalline carbon dioxide at about 77 °K are in reasonable agreement with the patterns to be expected from a lattice having the accepted Th6 symmetry of solid carbon dioxide. The calculated and observed intensities of the rings agree, provided the parameter u which measures the separation of adjacent carbon and oxygen atoms is taken to be larger than u = 0.1083 which was obtained from earlier X-ray work. Agreement between experiment and theory is obtained for u such that 0.1083 < u < 0.1250 but further work is required if u is to be determined precisely.Detailed consideration is given to those rings for which H = √17 and H = √18, where H = √(h2 + k2 + l2). In the present experiments the observed intensities of these rings agree with the calculated intensities but similar agreement was not found in earlier X-ray diffraction work.


2019 ◽  
Vol 4 (2) ◽  
pp. 59-63
Author(s):  
Erick Gastellóu ◽  
Crisoforo Morales ◽  
Godofredo García ◽  
Rafael García ◽  
Gustavo Alonso Hirata ◽  
...  

Undoped GaN layers were grown via radio-frequency magnetron sputtering, using a target manufactured with undoped GaN powders. Where the GaN powders were sintetized by nitridation of metallic gallium at 1000 °C in ammonia flow for two hours. X-ray diffraction patterns demonstrated that there are not a significant difference between the diffraction angles of the GaN powders and the GaN layers. The x-ray diffraction patterns for the GaN powders showed narrow peaks with a crystal size of 41 nm, while the GaN layers showed broad peaks with a crystal size of 7.7 nm. Scanning electron microscopy micrographs demonstrated the formation of crystals of irregular size with an average length of 1.56 μm for the GaN powders, while a homogeneous surface morphology with a thickness of 6.6 μm for the GaN layers was observed. Photoluminescence spectra showed a high emission at 3.49 eV (355.13 nm) for the GaN powders and an emission band energy located at 3.42 eV (361.54 nm) for the GaN layers, both emission bands were related to the band-to-band transition for the GaN. Raman spectra for the GaN powders showed the A1(TO), E1(TO), and E2(High) classical vibration modes. The GaN layers only showed the A1(TO) mode.


2017 ◽  
Author(s):  
◽  
I. A. Flores-Urquizo

Magnetic nanoparticles are proposed as heat mediators in hyperthermia treatments. In this work, three core-shell materials of different composition and magnetic anisotropy were developed to determine their properties as crystal size, saturation magnetization and their coating with organic molecules. The magnetic core of these materials was made by means of the coprecipitation reaction, following the stoichiometric ratio X+2Fe2+3O4 where X is Fe, Co or Ni for each material. From the X-ray diffraction patterns the crystal size of each material was determined, these were 10.39 nm, 7.27 nm y 3.86 nm. In addition, magnetization was 55.84 emu/g, 36.56 emu/g y 16.21 emu/g for magnetite, cobalt ferrite and nickel respectively. Each material was coated with aminosilane and by FTIR the vibrational modes of the C-N, N-H, C-H and Si-O bonds involved in the coating were identified.


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