Least-squares refinement of biaxial stress components and unit-cell parameter in a 〈111〉 textured cubic TiN polycrystalline thin film by X-ray diffraction

2010 ◽  
Vol 25 (1) ◽  
pp. 25-30 ◽  
Author(s):  
Ryouichi Yokoyama ◽  
Jimpei Harada ◽  
Yoshiaki Akiniwa

Biaxial residual stress in a 〈111〉 textured cubic TiN polycrystalline thin film was analyzed by linear least-squares refinement using the method proposed by Yokoyama and Harada [J. Appl. Crystallogr. 42, 185–191 (2009)]. Values of the unstressed (or stress-free) unit-cell parameter a0=4.2332±0.0006 Å and the stress components of σ11=397(88), σ22=401(88), and σ12=−110(100) were obtained. The values of the in-plane stresses σ11 and σ22 presented in the TiN film are practically the same, while σ12 is relatively small. The results obtained in this study confirm that the above theoretical prediction by Yokoyama and Harada can be used to obtain reliable values of stress-free unit-cell parameter and three biaxial stress components of a textured cubic thin film.

1987 ◽  
Vol 2 (4) ◽  
pp. 225-226
Author(s):  
Peter Bayliss ◽  
Slade St. J. Warne

AbstractMagnesium-chlorophoenicite may be differentiated from the Mn-analogue chlorophoenicite, because for magnesium-chlorophoenicite at 7Å, whereas for chlorophoenicite.In a review of the literature for the Mineral Powder Diffraction File by Bayliss et al. (1980), powder X-ray diffraction data could not be found of the mineral species magnesium-chlorophoenicite, (Mg,Mn)3Zn2(AsO4)(OH,O)6. Dunn (1981) states that the powder X-ray diffraction data of magnesium-chlorophoenicite is essentially identical to that of chlorophoenicite (Mn analogue) and confirms that the minerals are isostructural.With the crystal structure parameters determined by Moore (1968) for a Harvard University specimen from New Jersey of chlorophoenicite, a powder X-ray diffraction pattern was calculated with the programme of Langhof, Physikalische Chemie Institute, Darmstadt. The calculated pattern was used to correct and complete the indexing of the powder X-ray diffraction data of chlorophoenicite specimen ROM M15667 from Franklin, Sussex County, New Jersey, U.S.A. by the Royal Ontario Museum (PDF 25-1159). With the correctly indexed data of ROM M15667, the unitcell parameters were refined by least-squares analysis and are listed in Table 1.The most magnesium-rich magnesium-chlorophoenicite found in the literature is a description of Harvard University specimen 92803 from Franklin, Sussex County, New Jersey, U.S.A. by Dunn (1981), where Mg is slightly greater than Mn. A 114.6 mm Debye-Schemer film taken of HU92803 with Cu radiation and a Ni filter (CuKα = 1.5418Å) was obtained from Dr. P. Dunn and measured visually. The unit-cell parameters, which were refined by least-squares analysis starting from the unit-cell parameters of PDF 25-1159 in space group C2/m(#12), are listed in Table 1, and give F28 = 4.1(0.050,136) by the method of Smith & Snyder (1979).The hkl, dcalulated, dobserved and relative intensities (I/I1) of HU92803 are presented in Table 2. With the atomic positions and temperature factors of chlorophoenicite determined by Moore (1968), the Mn atomic positions occupied by 50% Mg and 50% Mn, and the unit-cell parameters of HU92803, a powder X-ray diffraction pattern was calculated and Icalculated is recorded in Table 2. A third powder X-ray diffraction pattern was calculated with the Mn atomic positions fully occupied by Mg. Because the atomic scattering factor of Mn is more than twice greater than Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the calculated intensities of the first three reflections given in Table 3.Although the a, c and β unit-cell parameters of chlorphoenicite are similar to those of magnesium-chlorphoenicite, the b unit-cell parameter of chlorophoenicite is significantly greater than that of magnesium-chlorophoenicite (Table 1). The b unit-cell parameter represents the 0–0 distance of the Mn octahedra (Moore, 1968). Since the size of Mn is greater than that of Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the b unit-cell parameter given in Table 1.American Museum of Natural History (New York, N.Y., U.S.A.) specimen 28942 from Sterling Hill, Ogdensburg, New Jersey is composed of willemite, haidingerite and magnesian chlorophoenicite. A spectrographic analysis of the magnesian chlorophoenicite shows As, Mg, Mn and Zn. Powder X-ray diffraction data (PDF 34-190) of the magnesian chlorophoenicite was collected by diffractometer with Cu radiation and a graphite 0002 monochromator (Kα1 = 1.5405) at a scanning speed of 0.125° 2θ per minute. The unit-cell parameters, which were refined by leastsquares analysis starting from the unit-cell parameters of PDF 25-1159, are given in Table 1. Specimen AM 28942 is called chlorophoenicite, because of its large b unit-cell parameter (Table 1), and the I/I1 of 25 for reflection 001 and of 50 for reflection 201 compared to the Icalculated in Table 3.


1996 ◽  
Vol 11 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Nicole M. L. N. P. Closset ◽  
René H. E. van Doorn ◽  
Henk Kruidhof ◽  
Jaap Boeijsma

The crystal structure of La1−xSrxCoO3−δ (0≤x≤0.6) has been studied, using powder X-Ray diffraction. The crystal structure shows a transition from rhombohedral distorted perovskite for LaCoO3−δ into cubic perovskite for La0.4Sr0.6CoO3−δ. The cubic unit cell parameter is ac=3.8342(1) Å for La0.4Sr0.6CoO3−δ, the space group probably being Pm3m. Using a hexagonal setting, the cell parameters for La0.5Sr0.5CoO3−δ, are a=5.4300(3) Å, c=13.2516(10) Å; a=5.4375(1) Å, c=13.2313(4) Å for La0.6Sr0.4CoO3−δ; a=5.4437(1) Å, c=13.2085(5) Å for La0.7Sr0.3CoO3−δ; a=5.4497(2) Å, c=13.1781(6) Å for La0.8Sr0.2CoO3−δ and a=5.4445(2) Å, c=13.0936(6) Å for LaCoO3−δ with the space group probably being R3c.


1999 ◽  
Vol 14 (2) ◽  
pp. 456-459 ◽  
Author(s):  
V. Swamy ◽  
N. A. Dubrovinskaya ◽  
L. S. Dubrovinsky

Powder x-ray diffraction data of yttria (Y2O3) were obtained from room temperature to melting point with the thin wire resistance heating technique. A solid-state phase transition was observed at 2512 ± 25 K and melting of the high-uemperature phase at 2705 ± 25 K. Thermal expansion data for α–Y2O3 (C-type) are given for the range 298–2540 K. The unit cell parameter increases nonlinearly, especially just before the solid-state transition. The x-ray diffraction spectrum of the high-temperature phase is consistent with the fluorite-type structure (space group Fm3) with a refined unit cell parameter a = 5.3903(6) Å at 2530 K. The sample recrystallized rapidly above 2540 K, and above 2730 K, all the diffraction lines and spots disappeared from the x-ray diffraction spectrum that suggests complete melting.


2011 ◽  
Vol 26 (4) ◽  
pp. 331-334 ◽  
Author(s):  
F. Laufek ◽  
J. Návrátil

The RuSb2Te compound has been synthesized and structurally characterized from powder X-ray diffraction data. RuSb2Te has the skutterudite structure, Im3 symmetry, unit-cell parameter a = 9.2665(1) Å, V = 795.70(1) Å3, Z = 8, and Dc = 7.88 g/cm3. The Sb and Te atoms randomly occupy the crystallographic 24g position; no indications of ordering of Te and Sb atoms have been detected.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 325
Author(s):  
Sytle Antao

Synchrotron high-resolution powder X-ray diffraction (HRPXRD) and Rietveld structure refinements were used to examine the crystal structure of single phases and intergrowths (either two or three phases) in 13 samples of the helvine-group minerals, (Zn,Fe,Mn)8[Be6Si6O24]S2. The helvine structure was refined in the cubic space group P4¯3n. For the intergrowths, simultaneous refinements were carried out for each phase. The structural parameters for each phase in an intergrowth are only slightly different from each other. Each phase in an intergrowth has well-defined unit-cell and structural parameters that are significantly different from the three endmembers and these do not represent exsolution or immiscibility gaps in the ternary solid-solution series. The reason for the intergrowths in the helvine-group minerals is not clear considering the similar radii, identical charge, and diffusion among the interstitial M cations (Zn2+, Fe2+, and Mn2+) that are characteristic of elongated tetrahedral coordination. The difference between the radii of Zn2+ and Mn2+ cations is 10%. Depending on the availability of the M cations, intergrowths may occur as the temperature, pressure, fugacity fS2, and fluid composition change on crystallization. The Be–Si atoms are fully ordered. The Be–O and Si–O distances are nearly constant. Several structural parameters (Be–O–Si bridging angle, M–O, M–S, average <M–O/S>[4] distances, and TO4 rotational angles) vary linearly with the a unit-cell parameter across the series because of the size of the M cation.


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