Comments on determining X-ray diffraction-based volume fractions of retained austenite in steels

2001 ◽  
Vol 16 (4) ◽  
pp. 198-204 ◽  
Author(s):  
C. K. Lowe-Ma ◽  
W. T. Donlon ◽  
W. E. Dowling
Keyword(s):  
Retained Austenite ◽  
Volume Fraction ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
X Ray ◽  
Profile Fitting ◽  
Diffraction Peaks ◽  
Diffraction Patterns ◽  
Heat Treatment Regimes ◽  
Integrated Intensities

Retained austenite is an important characteristic of properly heat-treated steel components, particularly gears and shafts, that will be subjected to long-term use and wear. Normally, either X-ray diffraction or optical microscopy techniques are used to determine the volume percent of retained austenite present in steel components subjected to specific heat-treatment regimes. As described in the literature, a number of phenomenological, experimental, and calculation factors can influence the volume fraction of retained austenite determined from X-ray diffraction measurements. However, recent disagreement between metallurgical properties, microscopy, and service laboratory values for retained austenite led to a re-evaluation of possible reasons for the apparent discrepancies. Broad, distorted X-ray peaks from un-tempered martensite were found to yield unreliable integrated intensities whereas diffraction peaks from tempered samples were more amenable to profile fitting with standard shape functions, yielding reliable integrated intensities. Retained austenite values calculated from reliable integrated intensities were found to be consistent with values obtained by Rietveld refinement of the diffraction patterns. The experimental conditions used by service laboratories combined with a poor choice of diffraction peaks were found to be sources of retained austenite values containing significant bias.

Control of the phase composition of advanced calcium phosphates using an x-ray diffractometer with a curved position-sensitive detector

2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov
Keyword(s):  
Phase Composition ◽  
Calcium Phosphates ◽  
Position Sensitive Detector ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Impurity Phases ◽  
Position Sensitive ◽  
Diffraction Peaks ◽  
Diffraction Patterns

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.

A profile-fitting procedure for analysis of broadened X-ray diffraction peaks. I. Methodology. Erratum

1989 ◽  
Vol 22 (2) ◽  
pp. 184-184 ◽  
Author(s):  
S. Enzo ◽  
G. Fagherazzi ◽  
A. Benedetti ◽  
S. Polizzi
Keyword(s):  
X Ray Diffraction ◽  
Correct Equation ◽  
X Ray ◽  
Fitting Procedure ◽  
Profile Fitting ◽  
Diffraction Peaks

Equation (18) of the paper by Enzo, Fagherazzi, Benedetti & Polizzi [J. Appl. Cryst. (1988). 21, 536–542] is in error. The correct equation is: A(2θ) = exp [−a|(2θ − 2θ 0)/cot 2θ 0|].

Experimental Study of Precise Peak Determination in X-Ray Powder Diffraction

1983 ◽  
Vol 27 ◽  
pp. 53-60 ◽  
Author(s):  
T. C. Huang ◽  
W. Parrish ◽  
G. Lim
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Search Results ◽  
Profile Fitting ◽  
Derivative Method ◽  
Diffraction Peaks ◽  
Peak Search ◽  
Different Characteristics ◽  
Good Agreement ◽  
Statistical Noise

AbstractThe combined derivative method (accompanying paper) was tested with a large number of experimental patterns to illustrate its use in various difficult problems commonly arising in peak search analysis of X-ray diffraction data. Patterns obtained with various step sizes, resolution, counting statistical noise, and profile widths were used. The precision in 2θ determination and overlap resolution are in good agreement with those previously obtained from calculated profiles, raise identification of noise as diffraction peaks was eliminated by using a convolution range proportional to the full width at half maximum. Peak search results (both 2θ and intensity) were also compared to those obtained by profile fitting to illustrate the different characteristics of these two methods.

MAGNETIC AND TRANSPORT PROPERTIES OFPr0.7Sr0.3MnO3/La0.5Ca0.5MnO3/Pr0.7Sr0.3MnO3TRILAYERS

2012 ◽  
Vol 26 (23) ◽  
pp. 1250132 ◽  
Author(s):  
H. O. WANG ◽  
P. DAI ◽  
H. LIU ◽  
W. S. TAN ◽  
F. XU ◽  
...  
Keyword(s):  
Transport Properties ◽  
Exchange Bias ◽  
Volume Fraction ◽  
Magnetic Phase ◽  
X Ray Diffraction ◽  
High Crystalline Quality ◽  
Metal Insulator ◽  
X Ray ◽  
Diffraction Patterns ◽  
Oriented Single Crystal

All-manganites Pr0.7Sr0.3MnO3/ La0.5Ca0.5MnO3/ Pr0.7Sr0.3MnO3(PSMO/LCMO/PSMO) trilayers were deposited on (001)-oriented single crystal MgO by pulsed laser deposition. The thickness of both PSMO layers was 36 nm while the thickness of LCMO layer varied from 6 to 36 nm. High resolution X-ray diffraction patterns indicated that trilayers were well (001)-oriented grown with high crystalline quality, and that PSMO layers were fully-strain-relaxed while LCMO spacer was partially strained. Studies on transport and magnetic properties of trilayers indicated that metal-insulator transition temperature TMIincreased from 200 K to 260 K and the saturation magnetization was suppressed with decreasing thickness of LCMO spacer from 36 to 6 nm. Transport properties of trilayers are associated with enhancement of volume fraction of ferromagnetic clusters in charge ordered and magnetic phase separated LCMO spacer. Interestingly, exchange bias (EB) was not observed in PSMO/LCMO/PSMO trilayers. It was believed that preferential distribution of metallic ferromagnetic clusters in LCMO layer may result in disappearance of EB.

Structural properties of molecular beam epitaxy grown Ni/Pt superlattices

1997 ◽  
Vol 12 (1) ◽  
pp. 161-174 ◽  
Author(s):  
W. Staiger ◽  
A. Michel ◽  
V. Pierron-Bohnes ◽  
N. Hermann ◽  
M. C. Cadeville
Keyword(s):  
Molecular Beam ◽  
Growth Direction ◽  
Misfit Dislocations ◽  
X Ray Diffraction ◽  
Plan View ◽  
X Ray ◽  
Transmission Electron ◽  
Superlattice Peak ◽  
Diffraction Peaks ◽  
Diffraction Patterns

We find that the [Ni3.2nmPt1.6nm] × 15 and [Ni3.2nmPt0.8nm] × 15 multilayers are semicoherent and display a columnar morphology. From both the period of the moir’e fringes and the positions of the diffraction peaks in electronic (plan-view and crosssection geometries) and x-ray diffraction patterns, one deduces that the nickel is relaxed (at least in the error bars of all our measurements), whereas the platinum remains slightly strained (≈−1%). The interfaces are sharp; no intermixing takes place giving rise to neat contrasts in transmission electron microscopy (TEM) and to high intensities of the superlattice peaks in the growth direction in both diffraction techniques. The relaxation of the interfacial misfit occurs partially through misfit dislocations, partially through the strain of platinum. A quasiperiodic twinning occurs at the interfaces, the stacking fault which forms the twin being the most often located at the interface Pt/Ni, i.e., when a Pt layer begins to grow on the Ni layer. The simulation of the θ/2θ superlattice peak intensities takes into account the columnar microstructure. It shows that the roughness is predominantly at medium scale with a fluctuation of about 12.5% for Ni layers and negligible for Pt layers.

High Density Bulk Shape Rapid Consolidation of the Yba2Cu307-X Superconductor

1989 ◽  
Vol 169 ◽  
Author(s):  
S. V. Rele ◽  
R. V. Raman ◽  
H. S. Meeks ◽  
R. L. Anderson ◽  
R. N. Shelton ◽  
...  
Keyword(s):  
Volume Fraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Superconducting Volume Fraction ◽  
One Step ◽  
Hollow Cylinders ◽  
Diffraction Patterns ◽  
Set Up ◽  
Cylinders And Spheres ◽  
High Processing

AbstractA novel rapid densification technique for fabrication of bulk shape YBa2Cu307–xsuperconductor is presented. The Ceracon process is a one‐step, quasi‐isostatic consolidation route utilizing conventional P/M equipment and set‐up. The Ceracon technology has enabled successful fabrication of bulk, shapes such as discs, cylinders, hollow cylinders and spheres along with significant increases in the density up to 95‐98% of the theorertical. The superconducting volume fraction is preserved due to short hold times at the operating temperatures and avoidance of high processing temperatures. Results based on densities, microstructure, susceptibility measurements, X‐ray diffraction patterns and TGA measurements are discussed.

A Gaussian–Hermite polynomials function for X-ray diffraction profile fitting

1999 ◽  
Vol 32 (4) ◽  
pp. 730-735 ◽  
Author(s):  
F. Sánchez-Bajo ◽  
F. L. Cumbrera
Keyword(s):  
Hermite Polynomials ◽  
Gaussian Function ◽  
Shape Functions ◽  
X Ray Diffraction ◽  
Stabilized Zirconia ◽  
Profile Function ◽  
Diffraction Profile ◽  
X Ray ◽  
Profile Fitting ◽  
Diffraction Peaks

In recent years, several profile-shape functions have been successfully used in X-ray powder diffraction studies. Here, a new profile function for approximating the X-ray diffraction peaks is proposed. This model, based on a Gaussian function multiplied by a correction factor in the form of a series expansion in Hermite polynomials, can be employed in the cases where there are peak asymmetries. The function has been tested by using samples of α-Al2O3and 9-YSZ (yttria-stabilized zirconia), yielding generally satisfactory results.

A profile-fitting procedure for analysis of broadened X-ray diffraction peaks. I. Methodology

1988 ◽  
Vol 21 (5) ◽  
pp. 536-542 ◽  
Author(s):  
S. Enzo ◽  
G. Fagherazzi ◽  
A. Benedetti ◽  
S. Polizzi
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Fitting Procedure ◽  
Profile Fitting ◽  
Diffraction Peaks

scholarly journals X-ray diffraction evidence for the existence of 102.0- and 230.0-nm transverse periodicities in striated muscle.

1987 ◽  
Vol 105 (3) ◽  
pp. 1311-1318 ◽  
Author(s):  
J Bordas ◽  
G R Mant ◽  
G P Diakun ◽  
C Nave
Keyword(s):  
Electron Density ◽  
Striated Muscle ◽  
Diffraction Theory ◽  
Optical Microscope ◽  
Sartorius Muscle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Density Maps ◽  
Diffraction Patterns ◽  
Integrated Intensities

Synchrotron radiation techniques have enabled us to record meridional x-ray diffraction patterns from frog sartorius muscle at resolutions ranging from approximately 2,800 to 38 nm (i.e., overlapping with the optical microscope and the region normally accessible with low angle diffraction cameras). These diffraction patterns represent the transform of the low resolution structure of muscle projected on the sarcomere axis and sampled by its repeat. Altering the sarcomere length results in the sampling of different parts of this transform, which induces changes in the positions and the integrated intensities of the diffraction maxima. This effect has been used to determine the transform of the mass projection on the muscle axis in a quasicontinuous fashion. The results reveal the existence of maxima arising from long-range periodicities in the structure. Determination of the zeroes in the transforms has been used to obtain phase information from which electron density maps have been calculated. The x-ray diffraction diagrams and the resulting electron density maps show the existence of a series of mass bands, disposed transversely to the sarcomere axis and distributed at regular intervals. A set of these transverse structures is associated with thin filaments, and their 102.0-nm repeat suggests a close structural relationship with their known molecular components. A second set, spaced by approximately 230.0 nm, is also present; from diffraction theory one has to conclude that this repeat simultaneously exists in thick and thin filament regions.

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