HighScore Plus Research Articles

Phase analysis and cation distribution correlated with magnetic properties of spinel Ba1−xSrxFe2O4 ferrites prepared at different annealing temperatures

Nano Ba1-xSrxFe2O4 samples were prepared by sol-gel autocombustion procedure. The phases developed due to different annealing temperatures and Sr-substitution amounts were determined by X'Pert HighScore Plus software. The effect of composition and annealing temperature on the lattice parameters and the crystallite size was investigated using X-ray diffraction technique. Rietveld analysis has been performed to determine the cation distribution between different crystallographic sites upon the Sr-substituted BaFe2O4 sample. Sr ion was found to prefer residing at 4a(II) site and the coordinates of this site dramatically changed with the Sr content (x). Fourier transform infrared spectrometry (FTIR) confirmed the orthorhombic structure of BaFe2O4 and the presence of the hexagonal structure ascribed to Ba0.5Sr0.5Fe2O4 for Sr-substituted samples. BaFe2O4 and Ba0.5Sr0.5Fe2O4 samples prepared at 700 °C revealed hysteresis loop with wasp-waist nature. The saturation magnetization and coercivity changed irregularly upon varying the annealing temperatures. For Ba1-xSrxFe2O4 samples annealed at 900 °C, the saturation magnetization changed depending on the amount of Sr doping in the sample. Ba0.5Sr0.5Fe2O4 has the lowest coercively (424 Oe) at 700 °C annealing temperature, while its highest saturation magnetization (3.83 emu/g) is obtained at 1050°C. Many factors were considered to explain the irregular behavior of coercivity in the Ba1-xSrxFe2O4 nano system.

Electrical properties of, Na1−0.315K0.315Nb1−yTayO3 (0 ≤ y ≤ 0.05) system

Na0.685K0.315Nb1−yTay O3 (where y = 0, 0.01, 0.02, 0.03, 0.04, 0.05) based ceramics were synthesized by the conventional solid-state reaction process. The effects of (Ta) – doping on the phase structure and electrical properties of (NKNTaO3) were observed. The cell parameters were refined by High Score Plus software, using Rietveld method, The monoclinic Pm(6) space group was chosen in these refinements. X-ray diffraction analysis shows that the crystal structure of the ceramics, without and with Ta-doping possessed monoclinic symmetry. Among the prepared compositions, a break in the XRD peaks shifting tendency was observed at y = 0.03, and also maximum dielectric permittivity, loss tangent and electrical conductivity observed at the composition with y = 0.03.

Determination of metallization degree of pre-reduced chromite with image and rietveld analysis

Metallization degree of pre-reduced chromite was determined using two methods. The chromite samples were reduced in the solid state by methane-hydrogen gas mixtures. First method was image analysis of micrographs obtained by scanning electron microscope where heavier metallic phases appeared as bright white areas which were relatively easy to segment using a thresholding algorithm. The second technique was Rietveld analysis of X-ray powder diffraction pattern which fitted a calculated profile onto a measured X-ray diffraction pattern to gain information about phase quantities. Rietveld refinement and phase composition analysis was performed with PANalytical?s X?Pert HighScore Plus software from the XRPD (X-ray powder diffraction) data. Both techniques were in good agreement. Metallization degrees for the investigated samples ranged from 15 to 65 % depending on the extent of reduction which was a function of time, reduction temperature, and methane content of the gas mixture. These results were promising and indicate that either image analysis or X-ray Rietveld analysis can be used as a relatively fast method to determine the degree of metallization of pre-reduced samples in comparison to the slow and tedious chemical analysis.

Optimization of processing parameters for graphitization of oil palm trunk waste at lower heating temperature

Previously synthetic graphite was produced at higher temperature which is around 2,500 °C in complex processing method. The method bear the name of the scientist whose discover the synthetic graphite namely “Acheson Process”. However, via pyrolysis process, in controlled heating condition, and specific heating rate by utilizing oil palm trunk waste, synthetic graphite was managed to produce at much lower heating temperature. In this research, the heating temperature were varied in the range of 500 °C, 800 °C, and 1,000 °C. The heating rate applied also varied, from 5 °/min to 10 °/min and 20 °/min. After heating treatment, the samples were characterized using X-ray Diffraction (XRD) and analysed by X’Pert Highscore Plus software. Graphitic nature of the synthetic graphite produced was further supported by RAMAN analysis. The morphological study was carried out by using Scanning Electron Microscope (SEM). Based on the analysis, optimum processing parameters was optimized. It is at the temperature of 800 °C and at the heating rate of 20 °/min.

Tailorable nano MgO.xAl2O3 spinel compositions along line of homogeneity via gel combustion route: Influence on phase evolution

Very fine sized (∼5–15 nm) magnesium aluminate spinel (MgO.xAl2O3) powder of different degree of solid solubility (x = 1, 1.25, 1.50, 1.75, and 2) have been attempted for synthesis following a gel combustion method to meet its high demand in the fields of refractory, photo catalysis, sensor and strategic applications, etc. Nitrates of magnesium and aluminum were used as oxidants for exothermic reactions fuelled by urea added with formaldehyde solution acting as reductant. Thermal decomposition reactions of polymer gels resulting in phases containing varied cationic ratio (Mg2+:Al3+) were investigated through DTA-TGA studies. Phase identification of synthesized powders derived from varying mole ratio of metal nitrates was performed by X-ray diffractometry (XRD) through Rietveld refinement using HighScore Plus software and was reconfirmed by Fourier Transform Infrared Spectroscopy (FTIR). Particle morphology was examined under Field Emission Scanning Electron Microscope (FESEM) & Transmission Electron Microscope (TEM). XRD pattern revealed the as-synthesized stoichiometric magnesium aluminate spinel (MgAl2O4) powder to be in amorphous state. In contrast, increasing trends in the extent of crystallinity in the as-synthesized form was obvious for alumina richer compositions. Dependence of development of crystallinity was explained in the light of thermal stability of polymer containing varied valent cations. Unlike crystallinity, a reverse trend is observed in case of cell parameter of the as-synthesized different non-stoichiometric spinel varieties where lattice parameter decreased with increasing alumina concentrations following Vegard's law. Variation in cell dimension against alumina concentration is caused by the insertion of smaller substituting Al3+ ions (0.054 nm) for Mg2+ ions (0.072 nm) in the unit cell. TEM observation reveals that the synthesized powder is aggregate of fine nano crystals. Crystallites were larger with increasing alumina concentration. An initial sintering behavior of the powder synthesized at 1400 °C has also been reported. Initial sintering trials were attempted under spark plasma sintering process.

Formation and characterization of collagen and hydroxyapatite composite

The formation of composite of collagen and hydroxyapatite (HA) was investigated by ex-situ precipitation method. Synthesis of HA was carried out by precipitation of Ca(OH)2 1 M and (NH4)2.HPO4 0.6 M with the molar ratio of Ca/P 1.67, the mixture was exposed to microwave irradiation (450 W) for 45 min. Subsequently, the result was sintered to produce the powders of HA. Verification of HA powders was performed using X-Ray Diffraction (XRD). Chicken collagen was prepared in our laboratory (Physics Department, Universitas Indonesia). Composite was synthesized by ex-situ precipitation method with a mass fraction of collagen and HA was 2:1. The mixture was stirring continuously for 2 h and aged for 20 h at room temperature. The precipitate was dried by freeze-drying method. The composite result was examined by Scanning Electron Microscopy (SEM). XRD pattern of sintered powder shown as HA crystal. The unit cell of HA crystals was evaluated by High Score Plus Program (a=b=9.425 and c=6.884) with the accuracy 98.175% for a and b lattice and 98.406% for c lattice. The collagen had been verified by SDS PAGE as type 1 collagen and the micrograph illustrated the presence of micropores. Based on SEM examination, the composite revealed that HA had been deposited onto collagen and filled part of void space of collagen. The preliminary study will be beneficial for leading the formation of composites of collagen-HA as biomaterials.

Study on Morphology and Crystal Structure of Pd Doped Nd1.2FeO3

Study on morphology and crystal structure of Nd1.2PdxFe1-xO3 doped Pd (1,2,3,4 and 5 wt%) synthesized by solid state reaction method have been investigated. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to identify phase and morphology of sample. Further analysis using X’Pert High Score Plus software show that samples have two phases: Nd1.2PdxFe1-xO3 as major phase and Nd2O3 as a minor phase. Nd1.2PdxFe1-xO3 crystalline size obtained by Scherrer equation has a value ranging from 43 to 50 nm and also has spherical shapes with the small existence of Pd confirmed by EDS results.

Synthetic graphite production of oil palm trunk chip at various heating rate via pyrolisis process

Abstract Synthetic graphite was synthesized from oil palm trunk chip in controlled heating condition or pyrolysis process. The heating rate (5 °/min, 10 °/min and 20 °/min) were varied whilst the heating temperature at 800 °C was fixed. After heat treatment process, the samples were characterized by X-Ray Diffraction (XRD) and analyzed using X’Pert Highscore Plus software. Graphite phase was analysed by XRD and it was further supported by RAMAN spectroscopy analysis to confirm the graphitic nature of the synthetic graphite obtained. The morphological study was carried out by using Scanning Electron Microscope (SEM). Based on the analysis, it was confirm that synthetic graphite was successfully synthesized by heat treatment at 800 °C (20 °/min heating rate). Synthetic graphite were observed in the form of amorphous carbon based on the XRD diffraction pattern that match with the reference code of 00-041-1487. RAMAN spectroscopy also showed the formation on D, G and 2D peaks at the respective wavenumber of 1250 cm-1, 1625 cm-1 and 2700 cm-1.

Synthesis and characterization of porous structures of rutile TiO2 /Na0.8Ti4O8/Na2Ti6O13 for biomedical applications

This method involves the use of molding, pressing and sintering techniques applied to different powder mixtures of TiO2 with sodium bicarbonate NaHCO3 (15 wt% and 30 wt% NaHCO3), to obtain porous structures of rutile TiO2/Na0.8Ti4O8/Na2Ti6O13 and Na0.8Ti4O8/Na2Ti6O13 for possible biomedical implant applications. The method validation includes X-ray diffraction patterns (XRD) analysis refined by the Rietveld method using X'Pert HighScore Plus. The surface morphology was observed by using a scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS), and, finally, a Chinese hamster ovary (CHO) cell line was cultured with the porous structures to determine the effect of material composition on the cellular response using a LDH cytotoxicity assay.•The method does not require the use of toxic solvents to remove residues.•The porous structure formed is composed mainly of crystalline phases Na2Ti6O13/TiO2 reported as biocompatible.•It did not need complicated solid-liquid separation processes.

XRD Analysis of Calcined Magnesium Substituted Biphasic Calcium Phosphate (Mg-BCP)

The incorporation of magnesium (Mg) in biphasic calcium phosphate (BCP) was prepared through precipitation method. The concentration of added Mg was varied with respect to calcium (Ca) precursor molarity as such Mg/Ca molar ratio were 0.05 and 0.1, while the (Ca + Mg)/P ratio was maintained at 1.59 throughout the experiment to ensure that calcium deficient apatite was formed. Precipitate obtained was aged for 24 h in ambient condition followed by decantation, centrifugation and drying at 90°C overnight. The as-synthesized powders were calcined at 600°C and characterized by X-ray diffraction (XRD) via Rietveld refinement (X’Pert HighScore Plus software). Both as-synthesized and calcined Mg-BCP powder contains hydroxyapatite (HA) and beta-tricalcium phosphate (β-TCP) phase with Mg in its lattice. The substitution of Mg in calcium-deficient apatite resulted in the formation of biphasic mixtures of β-TCP/HA after calcinations with shifted peaks β-TCP when compared to reference β-TCP peaks. High deficiency of calcium in apatite enables more substitution of magnesium thus stabilizing β-TCP phase when subjected to high temperature.

Rietveld Analysis on X-Ray Diffraction Of South Kalimantan Kaolin Clays

At least 13 million tons of kaolin claystone lie in several regencies of South Kalimantan covering Banjar, Tapin, Hulu Sungai Utara and Kotabaru regencies. This paper reports an attempt to explore their crystalline state characteristics, projecting their potential use for geopolymer. Sungai Tabuk, Cintapuri and Tatakan, due to their largest kaolin claystone deposits, were chosen as the sampling sites. The kaolin samples were prepared by syphoning method prior to X-ray diffraction (XRD) characterizations in determining their crystalline phases. X’Pert HighScore Plus and Rietica software were respectively responsible for the qualitative and quantitative phase analyses. The qualitative analysis used search and match method at peak position and peak height between measured and calculated diffraction patterns. Our study revealed the existence of two main phases in the sample, i.e. quartz (SiO2) and kaolinite (Al2Si2O5(OH)4). In addition, the Quantitative analysis used the Rietveld method with the least squares method approach. Rietveld refinement was based on a goodness of fit score of less than 4% by minimizing the difference in the character of the diffraction pattern (position, height, width and peak shape) between the observed and the calculated XRD patterns. The Rietveld quantitative analysis shows, Tatakan is an area with kaolinite-richest deposit (±84%), followed by Cintapuri (±76%) and Tabuk (±70%); quartz is found in reverse.

High permittivitty (La0.5Sr0.5)CoO3-δ-La(Co0.5Ti0.5)O3-δ ceramic composites for next generation MIM capacitors

Dielectrics with low capacitance loss and high relative permittivity are of high demand in metal-insulator-metal (MIM) capacitor that offers higher level of miniaturization, flexibility and performance. In order to achieve high relative permittivity, developing ceramics with metallic inclusions, has been suggested as a working strategy. But such materials may have high leakage currents and often lack thermal stability. With the objective for MIM applications, a series of (1-x)La(Co0.5Ti0.5)O3-δ-x(La0.5Sr0.5)CoO3-δ ceramics [x = 0.0, 0.02, 0.04, 0.06, 0.08, 0.1, 0.2, 0.3, 0.4, 0.5, 1] were developed. The crystal structure analysis was performed for La(Co0.5Ti0.5)O3-δ, (La0.5Sr0.5)CoO3-δ and 0.5La(Co0.5Ti0.5)O3-δ-0.5(La0.5Sr0.5)CoO3-δ using X-pert High Score Plus. The composite with x = 0.5 in (1-x)La(Co0.5Ti0.5)O3-δ-x(La0.5Sr0.5)CoO3-δ showed a maximum relative permittivity of 4920 with promising ac electrical resistivity (∼202 Ω-cm). The thermal, electrical and dielectric properties together suggest that the composition 0.5La(Co0.5Ti0.5)O3-δ-0.5(La0.5Sr0.5)CoO3-δ is suitable for MIM capacitors in DRAM and RF devices.

Synthesis of highly crystalline phase pure calcium metastannate by molten salt method

Calcium metastannate CaSnO3 with orthorhombic crystal system has been synthesized at low temperature by molten salt method using KCl-LiCl as a reaction medium and equimolar of SnO2 and CaCO3 as precursors. The process parameters including the reaction temperature, salt type, and salt to precursor weight ratio were investigated. Rietveld refinements on X-ray powder diffraction patterns were performed using X'Pert HighScore Plus software to calculate phase percent of each phase present in the obtained powder. The results of these calculations were followed in order to choose the salt system that requires the least reaction temperature to produce the highest CaSnO3 percent. The as-prepared compound was characterized by various techniques such as X-Ray diffraction (XRD), energy dispersive X-Ray spectrometry (EDX), Fourier transform infrared spectrometry (FTIR), and field emission scanning electron microscope (FE-SEM). The experimental results showed that highly crystalline phase pure CaSnO3 laminar plates could be prepared at 1000 °C for short period of time without any other detectable secondary phases.

UJI DENSITAS DAN POROSITAS SERTA KARAKTERISASI MENGGUNAKAN XRD DAERAH MATA AIR PANAS SEMURUP SUNGAI MEDANG KABUPATEN KERINCI PROVINSI JAMBI

Test Density and Porosity of rock have been done to see the relation to temperature influence 100 ᵒC, 200 ᵒC and 300 ᵒC. Rocks that will be tested first heated temperature with furnace tool then weighed with a digital balance. Density and Porosity measurement data were analyzed using Matlab Software with ASTMC373 equation. The result of Matlab in the form of graph shows average temperature change to Semurup rock density of 0.03 g / cm3 and the effect of temperature on Semurup rock porosity at 300 ᵒC is 30.29%. The average temperature change to Medang River rock density is 0.003 g / cm3 and the effect of temperature on Medang River rock porosity at 300 ᵒC is 0,55%. Looking at the rock crystal structure used XRD. Data from Characterization using XRD was analyzed with High Score Plus software. The result of rock characterization using XRD, from semurup showed that component of CaCO3 is 94%, crystal structure not yet fully formed and still in amorphous form, meanwhile rock from medang river show that component of CaCO3 is with 98%, crystalline structure have formed crystal.

THE MAIN CHARACTERISTICS OF POCERLAIN PRODUCTS BASED ON ANORTHITE CAS2

It is very difficult to synthesize pure CAS2 because of high melting temperature (1553 oC) In this paper, the formation of CAS2 during sintering period from the raw materials of kaolin, wollastonite, feldspar, sand and alumina at 1250 oC with holding time of 10 and 30 minutes is studied. The change during heating process was studied by the differential thermal analysis (DSC - TG). CAS2 minerals was analyzed by means of Rőntghen diffraction analysis (XRD) and phase idenfitication was performed by X'Pert High Score Plus software. The micro structure of the products has been studied through microscope images of scanning electron microscopy (SEM). The results showed that the water absorption of the products was less than 0.006 %, flexural strength reached 71-122 MPa, the Vicker’s hardness was in range from 2369 to 2666 MPa, the density was in range 2.36 – 2.59 g/cm3, the whiteness was in the range L* = 91.27 to 91.89 (according to CIELAB whiteness scale).

Characterization of natural puya sand extract of Central Kalimantan by using X-Ray Diffraction

Start Zircon sand extraction in this study use natural sand material from Kereng Pangi village of Central Kalimantan, also known as Puya sand. There are only three ways to extract the Puya sand. The first is magnetic separation, the second is immersion in HCl, and the third is reaction with NaOH. In addition, sample of each extraction step is analyzed with X-Ray Diffraction (XRD). Then based on the quantitative analysis using X'Pert Highscore Plus software, the samples are identified mostly as zircon (ZrSiO4) and silica (SiO2). Moreover, after the immersion process with HCl, the silica compound goes down and the zircon compound climbs to 74%. In the reaction process with NaOH zircon compound content further to increase to 88%.

Rietveld Quantitative Stability of Portland Blast Furnace Slag Cement Between Internal and External Standard Methods

Abstract The internal and external standard (G-factor) methods were applied to Rietveld/XRD quantitative analysis of Portland blast furnace slag cement using X’Pert Highscore Plus and GSAS-EXPGUI software. The Rietveld quantitative result derived from G-factor calculation and application was compared by internal standard methodology, which was employed by separately adding 20 and 50 % (weight percentage) of SiO2. The results show that the quantitations obtained by both of the above independent methods are almost consistent. In addition, the quantitative difference of most crystalline phases are less than 1 % except C4AF, about 1.2 %, while the amorphous determination has the quantitative difference of 2.1 %. Beside the careful sample preparation, proper XRD pattern collection, and satisfactory Rietveld refined procedure, the polished quartz rock used for mean G-factor calculation and the modified formula for amorphous calculation contributed to the Rietveld quantitative stability and reasonability. The formula based on amorphous quantification by internal standard was expressed as WAmor = 1−(WS(1−WS(PS+Sta)′))/((WS(PS+Sta)′−WS(PS)′)(1−WS)).

Effects of Laser Shock Peening on Mechanical Properties and Surface Morphology of AA2024 Alloy

This paper presents the after effect of laser shock peening (LSP) on AA2024 alloy specimen irradiated with the L-Spiral scanning pattern at different pulse energies. The surface morphology indicates an increase in surface roughness after LSP. The X-Ray diffraction analysis of the LSP treated specimens were compared with the untreated specimen. The sin²Ψ method of the X-ray diffraction technique indicates an improvement in the magnitude of compressive residual stress distribution after LSP. The hardness profile after LSP also shows substantial increment. The results suggested an improvement in the microstructural structure owing to the ultra-high strain rate deformation and refined grains. The High Score Plus software is used to analyse the crystallite size and microstrain of the alloy treated by different pulse energies.

The effect of time variation on the results of increasing titanomagnetite in iron sand at magnetization temperature (800°C) with Na2SO4 addition as additive

Indonesia has rich deposit of Iron Sand that can be found along of the Java southern part island. Iron sand contains some Ti-Rich minerals such as ilmenite, titanomagnetite dan rutile. This study aims to determine the effect of time variation on the results of Increasing titanomagnetite in iron sand and addition of 15% Na2SO4 as a catalyst. Variation of this reasearch was respectively 10 minutes, 20 minutes and 30 minutes with reduction temperature at 800°C. It takes the stage of roasting to condition the ore to be more easily reduced and increase the metal content so that it can maximize the iron sand purity with addition of Na2CO3 additive with mass ratio 1:0.4. Based on the XRD and Semi-Quant equation using Software HighScore Plus, optimal time for reducing iron sand with coal at 800°C is 30 minutes, which produce content of titanomagnetite as much as 36%.

Sideritic ironstones as indicators of depositional environments in the Weald Basin (Early Cretaceous) SE England

AbstractThe Lower Cretaceous Wealden sideritic ironstones have a wide occurrence and great potential to aid the reconstruction of the depositional environments of the Weald Basin in SE England. However, mineralogical and geochemical datasets on the ironstones are scarce in the literature. Geochemical and mineralogical data on the sideritic ironstones are presented from the Wadhurst Clay Formation within the Weald Basin. The mineralogy of the ironstones was examined using a PANalytical X'Pert Pro X-ray diffractometer and PANalytical's HighScore Plus software. Elemental composition of the ironstones was measured using a PANalytical MiniPal2 ED-XRF (benchtop X-ray spectrometer). The examination of the mineralogy of the Wealden ironstones confirms the presence of early diagenetic siderites. The trace-element assemblage shows that the sideritic ironstones are chemically pure pointing to a freshwater origin. The sideritic ironstones reveal anoxic conditions and palaeo-salinity in the basin. More generally, it is suggested that the composition of the host rocks has significant controls on the composition of sideritic ironstones in sedimentary basins. This work reinforces the importance of the composition of sideritic ironstones as useful non-traditional data for understanding the depositional settings of sedimentary basins, especially when traditional datasets are not readily available or insufficient.