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X-ray diffractometer
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X-ray diffractometer
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Series: ASM Desk Editions
Publisher: ASM International
Published: 01 December 1998
DOI: 10.31399/asm.hb.mhde2.a0003251
EISBN: 978-1-62708-199-3
... Debye-Scherrer camera and the X-ray diffractometer. The article also describes the uses of XRD analyses, such as the identification of phases or compounds in metals and ceramics; detection of order and disorder transformation; determination of lattice parameters and changes in lattice parameters due to...
Abstract
X-ray diffraction (XRD) is the most extensively used method for identifying and characterizing various aspects of metals related to the arrangements and spacings of their atoms for bulk structural analysis. XRD techniques are also applicable to ceramics, geologic materials, and most inorganic chemical compounds. This article describes the operating principles and types of XRD analyses, along with information about the threshold sensitivity and precision, limitations, sample requirements, and capabilities of related techniques. The necessary instrumentation for XRD analyses include the Debye-Scherrer camera and the X-ray diffractometer. The article also describes the uses of XRD analyses, such as the identification of phases or compounds in metals and ceramics; detection of order and disorder transformation; determination of lattice parameters and changes in lattice parameters due to alloying and temperature effects; measurement of residual stresses; characterization of crystallite size and perfection; characterization of preferred orientations; and determination of single crystal orientations.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006680
EISBN: 978-1-62708-213-6
.... The article ends with a few application examples of XRPD. X-ray powder diffraction diffractometers X-RAY POWDER DIFFRACTION (XRPD) techniques are used to characterize samples in the form of loose powders, aggregates of finely divided material or...
Abstract
X-ray powder diffraction (XRPD) techniques are used to characterize samples in the form of loose powders, aggregates of finely divided material or polycrystalline specimens. This article provides a detailed account of XRPD. It begins with a discussion on XRPD instrumentation and the techniques used to characterize samples. The article then describes the principles, advantages, and disadvantages of various types of powder diffractometers. A section on the Rietveld method of diffraction analysis is then presented. The article discusses various methods and procedures for qualifying and quantifying phase mixtures in powder samples. It provides information on typical sensitivity and experimental limits on precision of XRPD analysis and other systematic sources of errors that affect accuracy. Some of the factors pertinent to the estimation of crystallite size and defects are also presented. The article ends with a few application examples of XRPD.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006656
EISBN: 978-1-62708-213-6
... optics, a laser-guided microscope camera system for picking the analysis spot(s), a stage compatible with the sample type, and a detector, usually 1-D or 2-D, although scintillation detectors still are uncommonly used. Micro x-ray diffraction as a technique saw a decline in use as diffractometers...
Abstract
This article discusses various concepts of micro x-ray diffraction (XRD) used for the examination of materials in situ. The discussion covers the principles, equipment used, sample preparation procedure, considerations for calibrating a detector, steps for performing data analysis, and applications and interpretation of micro-XRD.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006631
EISBN: 978-1-62708-213-6
... viscous liquids (e.g., motor or Vaseline oil), which will not crystallize at low temperatures. Then the crystalline sample should be placed for data collection into a single-crystal x-ray diffractometer. Today there are several world-leading manufacturers of such equipment, which have distinct...
Abstract
This article provides a detailed account of the concepts of single-crystal x-ray diffraction (XRD). It begins with a historical review of XRD methods, followed by a description of the various factors involved in crystal symmetry. The article then focuses on the phase problem in x-ray structural analysis and validation of the structural model. Some of the factors to be considered for performing experimental procedure are provided. The article presents several examples of applications of single-crystal XRD. The following sections cover the crystallographic problem in terms of structural analysis, software programs for crystal structure solution and refinement, and visualization of crystal structures. The article ends with a discussion on various databases available for single-crystal XRD analysis.
Book Chapter
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006654
EISBN: 978-1-62708-213-6
... the tube. This fraction of x-rays is too divergent to be directly used for any diffraction measurements. Laboratory diffractometers have presample slits or optics to trim and collimate the radiation, which significantly reduces the flux of photons on the sample. Synchrotron x-rays, on the other hand...
Abstract
This article discusses the techniques and applications of synchrotron x-ray diffraction, providing information on x-ray generation, monochromation, and crystallography. X-ray diffraction techniques covered include single-crystal and powder diffraction. Some of the factors involved in the construction and development of macromolecular x-ray crystallography are also described.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006632
EISBN: 978-1-62708-213-6
... positioning precision of ±0.05 mm (±0.002 in.). The alignment of the diffractometers was established and checked using alloy or base metal powder incapable of supporting macroscopic residual stress, in accordance with ASTM E 915 (Ref 14). Revised from P.S. Prevey, X-Ray Diffraction...
Abstract
This article provides a detailed account of x-ray diffraction (XRD) residual-stress techniques. It begins by describing the principles of XRD stress measurement, followed by a discussion on the most common methods of XRD residual-stress measurement. Some of the procedures required for XRD residual-stress measurement are then presented. The article provides information on measurement of subsurface stress gradients and stress relaxation caused by layer removal. The article concludes with a section on examples of applications of XRD residual-stress measurement that are typical of industrial metallurgical, process development, and failure analysis investigations undertaken at Lambda Research.
Book Chapter
Series: ASM Desk Editions
Publisher: ASM International
Published: 01 November 1995
DOI: 10.31399/asm.hb.emde.a0003057
EISBN: 978-1-62708-200-6
... crystals or polycrystalline materials ( Ref 18 , 19 , 20 , 21 ). The single most useful instrument for phase identification or quantitative analysis of mixtures of phases, however, is the x-ray powder diffractometer. It provides for rapid acquisition of data useful for a number of purposes...
Abstract
This article describes testing and characterization methods of ceramics for chemical analysis, phase analysis, microstructural analysis, macroscopic property characterization, strength and proof testing, thermophysical property testing, and nondestructive evaluation techniques. Chemical analysis is carried out by X-ray fluorescence spectrometry, atomic absorption spectrophotometry, and plasma-emission spectrophotometry. Phase analysis is done by X-ray diffraction, spectroscopic methods, thermal analysis, and quantitative analysis. Techniques used for microstructural analysis include reflected light microscopy using polarized light, scanning electron microscopy, transmission electron microscopy, energy dispersive analysis of X-rays, and wavelength dispersive analysis of X-rays. Macroscopic property characterization involves measurement of porosity, density, and surface area. The article describes testing methods such as room and high-temperature strength test methods, proof testing, fracture toughness measurement, and hardness and wear testing. It also explains methods for determining thermal expansion, thermal conductivity, heat capacity, and emissivity of ceramics and glass and measurement of these properties as a function of temperature.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006643
EISBN: 978-1-62708-213-6
... world. Fig. 13 Single-crystal diffractometer. (a) Euler and (b) kappa geometries X-ray topography is a unique application of single-crystal analysis. It essentially is x-ray diffraction radiography in which a large area of a single crystal produces a single diffracted beam that creates a 1...
Abstract
This article describes the methods of X-ray diffraction analysis, the types of information that can be obtained, and its interpretation. The discussion covers the basic theories of X-rays and various types of diffraction experiments, namely single-crystal methods for polychromatic and monochromatic beams, powder diffraction methods, and the Rietveld method.
Book: Surface Engineering
Series: ASM Handbook
Volume: 5
Publisher: ASM International
Published: 01 January 1994
DOI: 10.31399/asm.hb.v05.a0001298
EISBN: 978-1-62708-170-2
... stress measurements. The Ω-and Ψ-diffractometers are defined on the basis of the sample axis for ψ tilt perpendicular or parallel to the plane of the incident and detected x-ray beam, respectively. A Ψ-diffractometer gives symmetric irradiated areas in −ψ and +ψ tilted angles at a given ( hkl...
Abstract
This article provides a useful guide for measuring residual macrostress on coatings. The most commonly used measurement methods are mechanical deflection, X-ray diffraction, and hole-drilling strain-gage. After a discussion on the origins of residual stress, the article describes the fundamental principles and presents examples of practical measurements for each method.
Book: Surface Engineering
Series: ASM Handbook
Volume: 5
Publisher: ASM International
Published: 01 January 1994
DOI: 10.31399/asm.hb.v05.a0001300
EISBN: 978-1-62708-170-2
... as by instrumental factors. A typical diffractometer will have an angular resolution of approximately 0.01°, which means that line broadening can be observed if the grain size D is lower than approximately 1 μm (40 μin.). This is easily achievable by various coating techniques, and x-ray...
Abstract
This article describes the structure of coatings produced by plasma spraying, vapor deposition, and electrodeposition processes. The main techniques used for microstructure assessment are introduced. The relationship between the microstructure and property is also discussed. The experimental techniques for microstructural characterization include metallographic technique, X-ray diffraction, electron, microscopies, and porosimetry.
Book: Surface Engineering
Series: ASM Handbook
Volume: 5
Publisher: ASM International
Published: 01 January 1994
DOI: 10.31399/asm.hb.v05.a0001238
EISBN: 978-1-62708-170-2
... for better quantification. For example, the percentage of retained austenite present at the surface of material can be measured by x-ray diffraction on the same diffractometer used for residual stress measurements. Reference 47 describes measurements of both residual stress and percentage of...
Abstract
The concept of surface integrity for grinding operations can be extended to encompass six different groups of key factors: visual, dimensional, residual stress, tribological, metallurgical, and others. This article discusses the importance of these factors in the performance and behavior of finishing methods in various manufactured parts. Special emphasis is given to residual stresses and their influence on the final mechanical properties of a manufactured part.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006667
EISBN: 978-1-62708-213-6
... structure form-factor measurements to be tracked. The crystal orientation, or face indexing, may also be determined by a laboratory single-crystal x-ray diffractometer before a neutron experiment. For powder neutron diffraction, sample sizes depend significantly on the instrument as well as on sample...
Abstract
This article provides a brief introduction to neutron diffraction as well as its state-of-the-art capabilities. The discussion covers the general principles of the neutron, neutron-scattering theory, generation of neutrons, types of incident radiation, and purposes of single-crystal neutron diffraction, powder diffraction, and pair distribution function analysis. The relationship between detector space and reciprocal space are presented. Various factors involved in sample preparation, calibration, and techniques used for analyzing diffraction data are described. The article also presents application examples and possible future developments in neutron diffraction.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006655
EISBN: 978-1-62708-213-6
... preference for some orientation can be beneficial. Two aspects of the microstructure are significant: the preferred orientation and the size of the columnar grains. The preferred orientation of a film can be ascertained using a standard x-ray diffractometer by comparing a θ-2θ scan to one from a powder...
Abstract
Low-energy electron diffraction (LEED) is a technique for investigating the crystallography of surfaces and overlayers adsorbed on surfaces. This article provides a brief account of LEED, covering the principles and measurements of diffraction from surfaces. Some of the processes involved in sample preparation are described. In addition, the article discusses the limitations of surface-sensitive electron diffraction and the applications of LEED with examples.
Series: ASM Handbook
Volume: 22A
Publisher: ASM International
Published: 01 December 2009
DOI: 10.31399/asm.hb.v22a.a0005418
EISBN: 978-1-62708-196-2
...-wavelength diffractometer, the principle is still the same, with the sample being rotated through every symmetric angle. The ODF is then reconstructed as for lab x-ray measurements but without the problem of ghosts. A more direct method is electron backscatter diffraction (EBSD). Here, the Kikuchi lines...
Abstract
Self-consistent models are a particular class of models in continuum micromechanics, that is, the field concerned with making predictions of the properties and evolution of aggregates whose single-crystal deformation behavior is known. This article provides information on the measurement and representation of textures as well as prediction of texture evolution in single-phase materials and two-phase aggregates.
Book Chapter
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006671
EISBN: 978-1-62708-213-6
...; AES, Auger electron spectroscopy; EPMA, electron probe x-ray microanalysis; FTIR, Fourier transform infrared spectroscopy; IA, image analysis; IC, ion chromatography; ICP-AES, inductively coupled plasma atomic emission spectroscopy; IR, infrared spectroscopy; LEISS, low-energy ion-scattering...
Abstract
The characterization, testing, and nondestructive evaluation of ceramics and glasses are vital to manufacturing control, property improvement, failure prevention, and quality assurance. This article provides a broad overview of characterization methods and their relationship to property control, both in the production and use of ceramics and glasses. Important aspects covered include the means for characterizing ceramics and glasses, the corresponding rationale behind them, and relationship of chemistry, phases, and microconstituents to engineering properties. The article also describes the effects that the structure of raw ceramic materials and green products and processing parameters have on the ultimate structure and properties of the processed piece. The effects that trace chemistry and processing parameters have on glass properties are discussed. The article describes mechanical tests and failure analysis techniques used for ceramics.
Book Chapter
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006757
EISBN: 978-1-62708-295-2
... by x-ray diffraction. The accuracy using a diffractometer is in the region of 0.5% for the range 1.5 to 38% of austenite by volume ( Ref 18 ). Fig. 33 Volume fraction of retained austenite in carbon steels fully austenitized and water quenched in water or brine at room temperature. Source...
Abstract
Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.
Series: ASM Handbook
Volume: 22A
Publisher: ASM International
Published: 01 December 2009
DOI: 10.31399/asm.hb.v22a.a0005424
EISBN: 978-1-62708-196-2
... confidence in the fidelity of simulation. This is true both when new methods are under development and when new applications emerge. Experiments involving in situ loading of specimens in facilities capable of x-ray and neutron diffraction measurements provide data at the scale of crystals. Elastic (lattice...
Abstract
This article provides an explanation on how crystal plasticity is implemented within finite element formulations by the use of physical length scales: crystal scale and continuum scale. It provides theoretical formulations for kinematic framework for deforming crystals and polycrystals, elastic and plastic behaviors of single crystals, refinements to the single-crystal constitutive, and crystal-scale finite-element. The article also presents examples that illustrate the capabilities of the formulations at the length scales.
Book Chapter
Series: ASM Desk Editions
Publisher: ASM International
Published: 01 November 1995
DOI: 10.31399/asm.hb.emde.a0003052
EISBN: 978-1-62708-200-6
Abstract
This article explains how ceramic powders are made. It begins by briefly describing the raw materials used in structural clay products, whitewares, refractories, and advanced ceramics. It then examines various additives that promote uniformity at different stages of the process. After a description of the comminution process (wet and dry milling methods), it discusses batching and mixing operations and granulation methods. The article also deals with the effect of process variables and the steps involved in chemical synthesis, including preparation from solution and gas-phase reactions, filtration and washing, and powder recovery techniques. It concludes with a discussion on characterization, centering on size distribution analysis, specific surface area, density, porosity chemical composition, phase, and surface composition.
Series: ASM Handbook
Volume: 4B
Publisher: ASM International
Published: 30 September 2014
DOI: 10.31399/asm.hb.v04b.a0005950
EISBN: 978-1-62708-166-5
... phenomena involved. Simulation results were commonly confirmed by microstructural analysis, hardness tests, and dimensional and x-ray diffraction (XRD) residual stress measurements. Although some results (such as prediction of temperature history, hardness distributions, and volume changes) were promising...
Abstract
This article describes the fundamental concepts of heat treatment simulation, including the physical events and their interactions, the heat treatment simulation software, and the commonly used simulation strategies. It summarizes material data needed for heat treatment simulations and discusses reliable data sources as well as experimental and computational methods for material data acquisition. The article provides information on the process data needed for accurate heat treatment simulation and the methods for their determination. Methods for validating heat treatment simulations are also discussed with an emphasis on the underlying philosophy for the selection and design of validation tests. The article also discusses the applications, capabilities, and limitations of heat treatment simulations via selected industrial case studies for a better understanding of the effect of microstructure, distortion, residual stress, and cracking in gears, shafts, and bearing rings.