Rietveld refinement of powder X-ray diffraction,microstructural and mechanical studies of magnesium matrix composites processed by high energy ball milling

This research reports the processing of magnesium matrix composites reinforced with silicon carbide(SiC)and aluminium oxide(Al_(2)O_(3))using powder metallurgy technique through high energy milling.Samples of Mg-SiC and Mg-Al_(2)O_(3)composites subjected to high energy ball milling for different vol%of secondary particles 20,30 and 40%of SiC and Al_(2)O_(3)are studied by X-Ray diffraction technique.The rietveld method as implemented in the Fullprof program is applied in order to determine the quantities of the resulting crystalline phases and amorphous phases at each stage of the mechanical treatment.Microstructural examination is carried out using Scanning Electron Microscope(SEM).In addition,crystal structural analysis using appropriate size and strain models is performed in order to handle the distinctive anistrophy that is observed in convinced crystallographic directions for the magnesium composite.The results are furnished in terms of crystalline domains size enlargement of the magnesium composites phases upon prolonged milling duration and discussed in the light of up to date views and theories on crystal growth of nanocrystaline materials.The hardness of the composite samples is calculated by Vickers’s Hardness tester.Further,dry sling wear test and corrosion test are performed for the fabricated composites.Composite with 30%secondary particles incorporated magnesium composites exhibits better wear and corrosion resistance than the other composites.

Spectroscopic studies and Rietveld refinement of strontium-britholites

Strontium-britholites whose chemical formula was Sr10-xLax（PO4）6-x（SiO4）xF2, where x=0, 1, 2, and 4 were prepared by solid state reaction. The structural refinement carried out using the Rietveld method indicated that La^3＋ ions were located into the two sites with a strong preference for metal （2） sites especially for low contents. A progressive shift of the F position along the c-axis outside the centre of the triangle formed by metal （2）-atoms was observed with the increase of x. The infrared and Raman spectra exhibited the characteristic vibration modes of PO4 and SiO4groups confirming the incorporation of this last group into the apatite structure. The 295i MAS-NMR spectra exhibited one resonance peak confirming the data obtained by X-ray diffraction, indicating that P and Si were located in the same crystallographic site.

Rietveld Refinement of New Solid Solution Al_xSb_ ( 3-x)Y_5 (0≤x≤2.16)

The X-ray diffraction analyses show that the existence of a continuous solid solution of Al_xSb_ 3-xY_5 (0≤x≤216). Al_xSb_ 3-xY_5 crystallizes in the hexagonal system with the space group P6_3/mcm (193) and Mn_5Si_3 structure type. The cell parameters for Al_2SbY_5 compound at 25 ℃ are a=0.88086 (2) nm, c=0.64662 (2) nm.

Phase and Rietveld Refinement of Pyrochlore Gd_2Zr_2O_7 Used for Immobilization of Pu(Ⅳ)

The phase of pyrochlore Gd_2Zr_2O_7 used for immobilization of Pu （Ⅳ） was investigated, tetravalent cerium was used as the simulacrum for plutonium with tetravalence, and the compounds in the system Gd_2Zr_2-_xCe_xO_7 （0.0≤x≤2.0） were synthesized via a high temperature solid reaction method with Gd_2O_3 and ZrO_2 powders being used as the starting materials. Based on the collected XRD data of the gained samples, the phase and microstructural change of compounds were calculated by means of rietveld structural refinement method. The experimental results indicated that the phases of compounds were changed from pyrochlore to fluorite-type phase with the increasing x. The linear relation between a and x was discovered in the range of fluorite-type phase, which accorded with a = 0.52748 ＋ 0.00825 x （0.2≤x≤2.0）, while V= 0.14668 ＋ 0.00711 x （0.2≤x≤2.0） was also achieved.

X-ray diffraction analysis by Rietveld refinement of FeAl alloys doped with terbium and its correlation with magnetostriction

Fe_(81)Al_(19) polycrystalline alloys doped with Tb(0-0.25 at%) were obtained by arc melting.The introduction of Tb favors the formation of columnar grains in the micro structure of the alloys,which develops a texture in the [100]crystal direction.Microstructural examination shows that the alloys are composed in great proportion by the disordered body-centered cubic(bcc),A2 phase and by a small proportion of the ordered bcc,B2 phase.As a consequence of doping with Tb,the lattice parameter increases,so the calculated apparent crystallite size increases,indicating a decrease in dislocation density and therefore in microstrains.The change in the magnetostriction with the magnetic field,dλ_(T)/dH,is directly related to strain anisotropy that can favor the iron easy magnetization axis on the [100] direction.An increase in total magnetostriction is found in the doped alloys with a maximum of 90 × 10^(-6) at 300 K for the alloy containing 0.027 at% Tb.This enhancement is a threefold value of the undoped alloy,which is attributed to the smaller maximum strain value and the preferential orientation formation by the columnar grains.

Application of high energy X-ray diffraction and Rietveld refinement in layered lithium transition metal oxide cathode materials

Layered lithium transition metal oxide(LTMO)cathode materials have attracted much attention for lithium-ion batteries and are shining in the current market.Establishing a clear structure-performance relationship is necessary for the performance improvement of LTMO cathode materials.The combination of synchrotron X-ray diffraction(XRD)with high intensity and XRD Rietveld refinement is powerful for revealing the structural characteristics of LTMO cathode materials.This review summarizes the application of high energy XRD and Rietveld refinement in LTMO cathode materials,including the brief introduction of synchrotron XRD and Rietveld refinement and their applications in understanding the structural evolution related to the synthetic,thermal runaway,cycling,and high-rate charge/discharge process of LTMO cathode materials.Synchrotron XRD can provide insights into the intermediates and reaction paths in the synthesis process,the origin of thermal runaway,the mechanism of structural decay during cycles,and the structural evolution during high-rate charging/discharging.Future works should focus on the development of higher intensity X-rays to gain more in-depth insights into the intrinsic relationship between their structural characteristics and properties.

Rietveld refinement and optical properties of SrWO_4:Eu^(3+) powders prepared by the non-hydrolytic sol-gel method

We investigated the effect of annealing time on the structure and optical properties of Sr WO4：Eu^3＋ powders prepared by the non-hydrolytic sol-gel method and heat treated at 800 ℃ for 2,4,8 and 16 h.Thermogravimetric and differential thermal analyses revealed that Sr WO4：Eu^3＋ powders were obtained at about 800 ℃.X-ray diffraction patterns and Rietveld refinement data confirmed that all powders had a scheelite-type tetragonal structure.Micro-Raman and Fourier transform infrared spectra indicated structural order at short range and anti-symmetric stretching vibrations of O-W-O bonds associated with tetrahedral[WO4]clusters.Optical properties were investigated by ultraviolet-visible（UV-vis）diffuse reflectance,and photoluminescence（PL）data which provided the evolution of quantum efficiency（η）and lifetime（τ）.UV-vis spectroscopy evidenced intermediate energy levels within the band gap of Sr WO4：Eu^3＋ powders.PL properties validated that the Eu^3＋ electric-dipole（^5D0→^7F2）transition in PL emission spectra was dominant which proved that Eu^3＋ ions were positioned in a site without an inversion center.[（^5D0→^7F2）/（^5D0→^7F1）]band ratios showed that Eu^3＋ ions were located in a low symmetry environment.The PL emission,ηandτproved the dependence on the annealing time in the behavior of Sr WO4：Eu3＋powders with a higher relative emission PL intensity as well as higherηandτvalues related to other samples when heat treated at 800℃ for 8 h.

Structural analysis by Rietveld refinement of calcium and lanthanum phosphosilicate apatites

Britholites with the general formula Ca10-xLnx（PO4）6-x（SiO4）xF2, （0≤x≤6） are considered to be promising matrices for the confinement of the by-products in the nuclear industry. A thermodynamic study showed that the stability of these compounds de-creased as the substitution rate increased. The present work was an attempt to gain more information about the structural changes in-duced by the substitution, in order to understand the observed stability decrease. The samples were successfully synthesized as a sin-gle-phase apatite by a solid-state reaction between 1200 and 1400 °C. The structural refinement indicated that the La3＋ions preferen-tially occupied the 6（h） sites. A progressive shift of F-along the c-axis outside its ideal position occurred as a result of the substitution increase. This might be the cause of the observed stability decrease, especially as the energies of the La-O, La-F and Si-O bonds are higher than those of Ca-O, Ca-F and P-O. The distribution of La3＋ between the two non-equivalent sites was confirmed by the charge distribution method.

Xray Diffraction Data and Rietveld Structure Refinement for CeNi_5Sn

The compound CeNi 5Sn was studied by means of X ray powder diffraction technique and refined by Rietveld method. It has a hexagonal structure with space group P 6 3/ mmc (No.194), Z =4, the lattice constants a =0 48912(3) nm, c =1 973(2) nm and D x=8 974 g·cm -3 . The Rietveld structural refinement was performed, leading to R p=0 138 and R wp =0 185. The figure of merit F N for the XRD data is F 30 =82 1(0 0068, 54). The X ray powder diffraction data are presented.

X-ray Powder Diffraction Data and Rietveld Refinement for NdCoGe_3

オ-ray powder diffraction data and crystal structure of RE compound NdCoGe3 were studied by using X-ray powder diffraction and refined by the Rietveld profile fitting method. The compound has the tetragonal BaNiSn3type structure, space group I4mm (No.107) a=0.42961(2) nm, c=098147(4) nm, V=0.018114 nm3, Z=2 and Dx=7.717 g·cm-3. The figure of merit FN for the powder data is F30=623 (0.0107, 45). Structure refinement was performed with 110 reflections and led to Rp=11.78% and Rwp=16.56%.

Analysis of the new ternary phase with C_(6)Cr_(23) structure in Mg-Co-B system by Rietveld method and physical properties of its Ni-substituting effect

A new ternary Mg_(1.4)Co_(21.6)B_(6) compound in the Mg-Co-B system was synthesized via a conventional solid-state reaction method and the effect of Ni-substitution on its crystal structure,thermal stability,solid solubility and physical properties were systematically investigated.The crystal structure of the Mg_(1.4)Co_(21.6)B_(6) compound was fully determined by the X-ray diffraction technique with Rietveld refinement method.It is found that Mg_(1.4)Co_(21.6)B_(6) crystallizes in the form of C_(6)Cr_(23) structure type(space group:Fm-3m(No.225),a=10.5617(2)A,Z=4).The results showed that the 4a sites have been occupied completely by Co atoms in present compound which with M_(2-x)Ni_(21+x)B_(6) form belonging to the W_(2)Cr_(21)C_(6)-type.When Mg_(1.4)Co_(21.6)B_(6) is repeatedly sintered at elevated temperatures,it becomes unstable and decomposes into Co3B and Mg.The lattice parameters of the Mg_(1.4)Co_(21.6)B_(6) solid solution alters dramtically with increasing Ni substitution,with no regular trend being observed.The electrical and magnetic performances of the 3.6Mg:3Co:17Ni:6B and 3.6Mg:3Co:18Ni:6B(nominal compositions)samples suggest that both samples are typical ferromagnetic materials.The temperature in the maximum drop of theρ(T)curve decreases as a function of the Ni content.Base on the correlation between the critical temperature and Ni content,a linear fitting equation is obtained and the critical temperature of Mg_(1.4)Co_(21.6)B_(6) calculated utilizing the linear fitting equation.The findings in this work may provide certain reference values for material science on electrical magnetic properties and other references for researching the material further.

Synthesis of LiNi_(0.8)Co_(0.1)Mn_(0.1)O_2 cathode material by chloride co-precipitation method

LiNi0.8Co0.1Mn0.1O2 was prepared by a chloride co-precipitation method and characterized by thermogravimetric analysis, X-ray diffractometry with Rietveld refinement,electron scanning microscopy and electrochemical measurements.Effects of lithium ion content and sintering temperature on physical and electrochemical performance of LiNi0.8Co0.1Mn0.1O2 were also investigated. The results show that the sample synthesized at 750℃with 105%lithium content has fine particle sizes around 200 nm and homogenous sizes distribution.The initial discharge capacity for the powder is 184 mA·h/g between 2.7 and 4.3 V at 0.1C and room temperature.

One-pot hydrothermal preparation of hierarchical manganese oxide nanorods for high-performance symmetric supercapacitors

An eco-friendly,new,and controllable approach for the preparation of manganese oxide(a-MnO_(2))nanorods has been introduced using hydrothermal reaction for supercapacitor application.The in-depth crystal structure analysis ofα-MnO_(2) is analyzed by X-ray Rietveld refinement by using Full Prof program with the help of pseudo-Voigt profile function.The developed a-MnO_(2) electrode attains a remarkable capacitance of 577.7 F/g recorded at a current density value of 1 A/g with an excellent cycle life when is used for 10,000 repeated cycles due to the porous nanorod-morphology assisting the ease penetration of electrolyte ions into the electroactive sites.The diffusive and capacitive contributions of the electrode have been estimated by considering standard numerical packages in Python.After successfully assembling the aqueous symmetric supercapacitor(SSC)cell by utilizing the as-preparedα-MnO_(2),an excellent capacitance of 163.5 F/g and energy density of 58.1 Wh/kg at the constant current density of 0.5 A/g are obtained with an expanded potential frame of 1.6 V.Moreover,the cell has exceptionally withstood up to 10,000 cycles with an ultimate capacitance retention of 94.1%including the ability to light an LED for 18 s.Such findings recommend the developed a-MnO_(2) electrode to be a highly felicitous electrode for the field of energy storage.

Crystal Structures of Dy_2(WO_4)_3 and GdY(WO_4)_3

Two compounds, Dy_2(WO_4)_3 and GdY(WO_4)_3, were synthesized by using thestandard solid state reaction technique. The crystal structure was determined by powder X-raydiffraction and Rietveld refinement method. It is found that both compounds have Eu_2(WO_4)_3-typemonoclinic structure, with space group C 2/c, Z = 4. The unit cell parameters of Dy_2(WO_4)_3 are a= 0.75981(1) nm, b = 1.13220(1) nm, c = 1.13254(1) nm, and beta = 109.8001(3) deg, and those ofGdY(WO_4)_3 arc a = 0.76175(1) nm, b = 1.13543(1) nm, c = 1.13496(2) nm, and beta = 109.8015(13)deg. Each W atom has four oxygen nearest neighbors, while each rare-earth atom is surrounded byeight oxygen atoms. WO_4 tetrahedra share their four vertices with REO_8 (RE = Dy, Gd, or Y)trigondodecahedra and some REO_8 trigondodecahedra share an edge with each other. The phasetransition and the magnetic properties were investigated by differential thermal analysis (DTA) anddc superconducting quantum interference device (SQUID) magnetometer.

Synthesis and Analysis of Tm^(3+) Doped YF_3 Upconversion Luminescent Nano-materials

Upconversion （UC） phosphor Tm3＋ doped YF3 nano-erystals were prepared by hydrothermal method under different conditions and characterized by Field Transmission electron microscopy （TEM）, Scanning electron microscopy （SEM） and X-ray diffraction （XRD）. Their UC luminescence properties were studied by fluorescence spectrophotometer with 980 nm diode laser excitation, and impact of different grain sizes and morphology on the UC luminescence intensity was discussed. The fluorescence decay lifetime was calculated by Multi-exponential function fitting method. Results show that UC emission intensity was enhanced with the reduction of grain size, and the decay lifetime is 0.60 us.

Dielectric, piezoelectric, and ferroelectric properties of lanthanum-modified PZTFN ceramics

Specimens of Pb1-1.5xLax（Zr0.53 Ti0.47）1-y-zFeyNb2O3 （x = 0, 0.004, 0.008, 0.012, and 0.016, y = z = 0.01） （PZTFN） ceramics were synthesized by a semi-wet route. In the present study, the effect of La doping was investigated on the structural, microstructural, dielectric, piezoelectric, and ferroelectric properties of the ceramics. The results show that, the tetragonal （space group P4mm） and rhombohedral （space group R3c） phases are observed to coexist in the sample at x = 0.012. Microstructural investigations of all the samples reveal that La doping inhibits grain growth. Doping of La into PZTFN improves the dielectric, ferroelectric, and piezoelectric properties of the ceramics. The hys- teresis loops of all specimens exhibit nonlinear behavior. The dielectric, piezoelectric and ferroelectric properties show a maximum response atx 〉 0.012, which corresponds to the morphotropic phase boundary （MPB）.

A combined IR and XRD study of natural well crystalline goethites(α-FeOOH)

Goethite(a-FeOOH)is one of the most abundant minerals on the Earth surface,occurring in temperate,tropical and equatorial climates.Fe in goethite can be substituted by many cations such as Al,Ni for instance.A large amount of research has been conducted on the effect of varying elemental compositions(mainly Al-content)on the spectral features of goethites with most of the studies based on materials synthesized with different elemental ratios.The different elemental ratios,however,may not only affect the composition of the products but also their crystallinity and/or particle size and shape.Both parameters are known to affect results of both X-ray diffraction(XRD)and infrared spectroscopy(IR).These methods are predominantely used to characterize goethites.In the present study,therefore,a significant set of natural goethites was considered in order to investigate the effect of elemental composition on XRD and IR results.The focus was on crystallised samples which had a limited chemical variability but artefacts caused by the presence of admixtures could be excluded in most cases.First of all Rietveld refinement was optimized based on varying different parameters.A fairly good correlation of Rietveld derived crystallite sizes and specific surface area determined by N-adsorption(SSA)was found which proves the importance of considering the crystallite size parameters for Rietveld refinement and at the same times proves the quality of it.Using IR spectroscopy yet published relations of band position and Al-content could be confirmed despite the fact that the range of Al-contents was small.However,the band position of the Fe–O stretching,previously used as proxy for crystallinity assessment,was found to be least variable hence contradicting yet published results.Controversial results were also published for the effect of the Al-content on the position of the asymmetric FeOH stretching band at 450 cm.The goethites investigated in the present study indicate that the crystallite size determines the band position rather than the Al-content which is at least valid for the limited range of Al-contents.The results of the present study indicate that using synthetic sample sets bears the problem that more than one parameter might show systematic differences(e.g.crystallite size in a set of chemically varied goethites).The paper,therefore,provides IR reference data based on a set of natural well crystallised goethites.

X-Ray and Neutron Diffraction Studies on Thermal Parameters of Thalous Bromide

Thermal parameters of TIBr were determined using both X-ray and neutron diffraction techniques. The data was analysed by Rietveld profile refinement procedure. From the neutron diffraction data, due to weak odd-order reflections, it was not possible to determine the individual thermal parameters. TheX-ray diffraction measurements yielded BT1=0.296(5) nm2 and BBr=0.162(5) nm2. The overall isotropic value, B was 0.252(7) nm2 which is in good agreement with B=0.230(8) nm2 obtained from present neutron diffraction measurements. The present values are also in good agreement with theoretical estimates obtained from the shell models.

Pedogenically degenerated illite and chlorite lattices aid to palaeoclimatic reconstruction for chronologically constrained(8-130 ka) loess-palaeosols of Dilpur Formation,Kashmir,India

Chronologically well-constrained loess-palaeosols(recorded glacial and inter-glacial climate) revealed pedogenesis induced ionic substitutions,caused end-member compositional deviations in illite and chlorite,linked to widespread climatic changes occurred during Late Pleistocene.Further,micro-level climatic resolution is yet to be resolved.Thus,layer-wise X-ray diffraction analyses of clay separates,followed by Rietveld refinement revealed varied cell parameters and interatomic distances.Obtained values for detrital and pedogenic illite and chlorite when plotted against stratigraphic succession show notable changes in the crystallographic axes.The illite lattices associated with inadequately pedogenized palaeosols have been altered into illite/smectite mixed layers,but,the chlorite lattices represent expansion of a-,b-and contraction of c-axes with much greater amount of distortions,suggestive of warm-humid and acidic environment.The detrital 48,44 and 83,74 bonded illite and chlorite with2 sub-types each,when pedogenized retained 48,44 and 34;and 83 and 74 bonds(in their neo-formed 3 and 2 sub-types),respectively.The Al-O bond shows expansion,but,unchanged Si-O and decreased Si-K and K-O bonds show loss of Al and retention of Si and K ions in the illite lattices.The illite with 32 atoms and 48 bonds represent contraction of K-O,Si-K,Al-O and Si-O bonds caused bond reinforcement;however,loss of Al3+reflects all-out illite alteration.Owing to Al-O and K-O bond expansion,major K+ and Al3+ ionic loss occurred during the LGM,however,further ionic loss depends upon the magnitude of the loess-palaeosol weathering that they have suffered.The clilate sensitive Fe,Mg and Al ionic losses for Fe-O,Mg-O and Al11-O9 bond length expansions were recognized in the chlorite lattices.Such ionic losses are common,but,complete distortion is attributed to Al,Si,Fe and Mg ionic losses,followed by weakening of Al-O,Si-O,Fe-O and Mg-O bonds.Though,Si-O4 and Fe1-O4 bonds,and Si and Fe1 st ions remain intact.Thus,three major glacial episodes of ~5 ka each occurred under alkaline environment,but,intervened by two successive cycles of 55 ka each,encompassing three alternate warm and cold climatic sub-cycles of 12-15 ka.But,the coldness increases with each warm-cold sub-cycle that attained the glacial maxima.Further,these events correlate well with the deep-sea records of the North Atlantic(MIS-1 to MIS-5 e) and CLP loess-palaeosols(~127 ka).

Driving the sodium-oxygen battery chemistry towards the efficient formation of discharge products: The importance of sodium superoxide quantification

Sodium-oxygen batteries(SOBs) have the potential to provide energy densities higher than the state-ofthe-art Li-ion batteries. However, controlling the formation of sodium superoxide(NaO_(2)) as the sole discharge product on the cathode side is crucial to achieve durable and efficient SOBs. In this work, the discharge efficiency of two graphene-based cathodes was evaluated and compared with that of a commercial gas diffusion layer. The discharge products formed at the surface of these cathodes in a glyme-based electrolyte were carefully studied using a range of characterization techniques. NaO_(2) was detected as the main discharge product regardless of the specific cathode material while small amounts of Na_(2)O_(2).2H_(2)O and carbonate-like side-products were detected by X-ray diffraction as well as by Raman and infrared spectroscopies. This work leverages the use of X-ray diffraction to determine the actual yield of NaO_(2)which is usually overlooked in this type of batteries. Thus, the proper quantification of the superoxide formed on the cathode surface is widely underestimated;even though is crucial for determining the efficiency of the battery while eliminating the parasitic chemistry in SOBs. Here, we develop an ex-situ analysis method to determine the amount of NaO_(2) generated upon discharge in SOBs by transmission X-ray diffraction and quantitative Rietveld analysis. This work unveils that the yield of NaO_(2) depends on the depth of discharge where high capacities lead to very low discharge efficiency, regardless of the used cathode. We anticipate that the methodology developed herein will provide a convenient diagnosis tool in future efforts to optimize the performance of the different cell components in SOBs.