Advances in X-Ray Analysis: Volume 32

665 Pages·1989·25.479 MB·English

by  John V. Gilfrich (auth.),  Charles S. Barrett,  John V. Gilfrich,  Ron Jenkins,  Ting C. Huang,  Paul K. Predecki (eds.)

ADVANCES IN
X-RAY ANALYSIS
Volume 32
Edited by
Charles S. Barrett
University of Denver
Denver, Colorado
John V. Gilfrich
Sachs/Freeman Associates
Washington, D.C.
Ron Jenkins
JCPDS-International Centre for Diffraction Data
Swarthmore, Pennsylvania
Ting C. Huang
IBM Almaden Research Center
San Jose, California
and
Paul K. Predecki
University of Denver
Denver, Colorado
Sponsored by
University of Denver Department of Engineering
and
JCPDS - International Centre for Diffraction Data
Springer Science+ Business Media, LLC
The LibraryofCongresscataloged the first volume ofthistitleas folIows:
Conferenceon Application of X-rayAnalysis.
Proceedings6th- 1957- [Denver)
v. illus. 24-28cm.annual.
No proceedings published for the first 5conferences.
Vols. for 1958- called also:Advancesin X-rayanalysis, v.2-
Proceedingsfor 1957issued bytheconferenceunderanearliername:Conferenceon
Industrial Applications of X-ray Analysis. Other slight variations in name of con
ference.
Vol. for 1957 published by the University of Denver, Denver Research Institute,
MetallurgyDivision.
Vois. for 1958- distributed byPlenum Press, NewYork.
ConferencessponsoredbyUniversityofDenver,DenverResearchInstitute.
I. X-rays-Industrial applications-Congresses. I. Denver University. Denver
Research Institute 11. Title: Advancesin X-ray analysis.
TA406.5.C6 58-35928
ISBN978-1-4757-9112-9 ISBN978-1-4757-9110-5(eBook)
DOI10.1007/978-1-4757-9110-5
Proceedingsofthe Thirty-seventh Annual Conferenceon ApplicationsofX-Ray Analysis,
held August 1-5, 1988,inSteamboat Springs, Colorado
© 1989SpringerScience+BusinessMediaNewYork
Originallypublishedby PlenumPress,NewYorkin1989.
Softcoverreprintofthehardcover1stedition 1989
All rightsreserved
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FOREWORD
The 37th Annual Denver Conference on Applications of X-Ray Analysis
was held August 1-5, 1988, at the Sheraton Steamboat Resort and Conference
Center, Steamboat Springs, Colorado. As usual, alternating with x-ray
diffraction, the emphasis this year was x-ray fluorescence, but as has been
the pattern for several occasions over the last few years, the Plenary
Session did not deal with that subject, specifically. In an attempt to
introduce the audience to one of the new developments in x-ray analysis,
the title of the session was "High Brilliance Sources/Applications," and
dealt exclusively with synchrotron radiation, a topic which has made a very
large impact on the x-ray community over the last decade. As the organizer
and co-chairman of the Plenary Session (with Paul Predecki), it is my
responsibility to report on that session here.
The Conference had the privilege of obtaining the services of some of
the preeminent practitioners of research using this remarkable x-ray
source; they presented the audience with unusually lucid descriptions of
the work which has been accomplished in the development and application of
the continuous, high intensity, tunable, polarized and collimated x-rays
available from no facility other than these specialized storage rings.
The opening lecture (and I use that term intentionally) was an
enthusiastic description of "What is Synchrotron Radiation?" by Professor
Boris Batterman of Cornell University and the Cornell High Energy
Synchrotron Sourc(! (CHESS). His many years of teaching and research were
obvious in the manner of his presentation, holding the attention of the
audience as he dealth with the sophisticated physics involved in the
production, extraction and manipulation of the x-ray beam for experimental
purposes. Dean Chapman, from the National Synchrotron Light Source (NSLS)
at Brookhaven, followed with a description of the general configuration of
the beamlines necessary to make use of the x-radiation. Such features as
shutters, vacuum, shielding and safety were discussed. Particular emphasis
was placed on the design of beamline optics, the monochromators and mirrors
required to provide focussed or collimated, monochromatic or continuous
spectrum beams, as well as the problems encountered due to the power
loading which those components must withstand because of the high intensity
of the radiation.
Following those two presentations, two talks were given describing
specific applications. John Newsam (with co-authors H. E. King, Jr., and
K. S. Liang), from Exxon Research and Engineering Company, narrated the
myriad ways in which x-ray diffraction could be conducted, using either
monochromatic or white radiation. Various single crystal experiments were
mentioned, including high resolution measurements, Laue techniques and
microcrystal analyses. Powder diffraction results addressed were high
resolution, energy-dispersion diffraction and anomalous scattering
measurements. I then had the privilege of presenting my thoughts on the
v
vi FOREWORD
present status of x-ray fluorescence analysis using synchrotron radiation,
polychromatic and monochromatic, as the excitation source. Research into
the capabilities of this technique is being conducted around the world, and
I took advantage of my personal knowledge of that effort to present a brief
review of the accomplishments, including the use of both energy- and
wavelength-dispersive detection.
I found the experience of organizing and participating in such a
Plenary Session very rewarding. Even though I have been associated with
work going on in the field for about seven years, I was surprised to
discover how little I knew about the wide variety of research being
conducted at the different facilities. It is even reasonable to assume, as
John Newsam said, that the next few years will witness a great increase in
the number of materials problems that are tackled using synchrotron
radiation techniques.
John V. Gilfrich
Washington, D.C.
January 1989
PREFACE
This volume constitutes the proceedings of the 1988 Denver Conference
on Applications of X-Ray Analysis and is the 32nd in the series. The
conference was held August 1-5, 1988, at the Sheraton Steamboat Resort &
Conference Center, Steamboat Springs, Colorado. The general chairmen were:
J. V. Gilfrich, Sachs/Freeman Associates, NRL; and P. K. Predecki,
University of Denver; with C. S. Barrett of the University of Denver as
honorary chairman. The conference advisory committee this year consisted
of: C. S. Barrett - University of Denver, J. V. Gilfrich - Sachs/Freeman
Associates, NRL, R. Jenkins - International Centre for Diffraction Data,
D. E. Leyden - Philip Morris USA, J. C. Russ - North Carolina State
University, C. O. Ruud - The Pennsylvania State University, and P. K.
Predecki - University of Denver. We take this opportunity to thank the
advisory committee for their active participation, tireless efforts and
able guidance which made this conference successful.
The conference plenary session was organized and chaired by
J. V. Gilfrich, Sachs/Freeman Associates/NRL, Washington, D.C., and was
entitled: "HIGH BRILLIANCE SOURCES/APPLICATIONS."
The invited papers on the program are listed below.
"What is Synchrotron Radiation?" B. W. Batterman
"Synchrotron Radiation Facilities," D. Chapman
"X-Ray Diffraction Using Synchrotron Radiation,"
J. M. Newsam, H. E. King, Jr., and K. S. Liang
"XRF Using Synchrotron Radiation," J. V. Gilfrich
"X-Ray Diffraction Analysis of High Tc Superconducting Thin Films,"
T. C. Huang, A. Segmuller, W. L. Lee, D. C. Bullock and R. Karimi
"Parallel Beam and Focusing Powder Diffractometry,"
W. Parrish and M. Hart
"Applications of Dual-Energy X-Ray Computed Tomography to Structural
Ceramics," W. A. Ellingson and M. W. Vannier
"X-Ray Microtomography,"
H. W. Deckman, B. F. Flannery, J. H. Dunsmuir and K. D'Amico
"Advances in Elemental and Chemical State Imaging in Two and Three
Dimensions Using Synchrotron Radiation,"
J. H. Kinney, M. C. Nichols, Q. C. Johnson, U. Bonse, R. A. Saroyan
and R. Nusshardt
vii
viii PREFACE
In addition to the Plenary Session, the following Special Sessions
were held:
o X-RAY TOMOGRAPHY, IMAGING, AND TOPOGRAPHY, chaired by P. Engler,
Standard Oil R&D; and N. Gurker, Technical University of Vienna,
Austria.
o APPLICATIONS OF DIGITIZED XRD PATTERNS, chaired by D. K. Smith,
Penn State University; and R. Jenkins, International Centre for
Diffraction Data.
o X-RAY STRESS ANALYSIS, chaired by A. Krawitz, University of
Missouri; and Y. Hirose, Kanazawa University, Japan.
o HANDLING TECHNIQUES IN QUALITATIVE AND QUANTITATVE ANALYSIS, chaired
by W. Schreiner, Philips Laboratories; and J. Nusinovici, Socabim,
Paris, France.
o THIN FILM APPLICATIONS OF XRD AND XRF, chaired by T. Huang, IBM
Almaden Research Center; and J. C. Russ, North Carolina State
University.
o ON-LINE X-RAY ANALYSIS: XRF AND XRD, chaired by A. Harding, Colorado
State University; and B. Cross, Kevex Corp.
Tutorial workshops on various XRF and XRD topics were held during
the first two days of the conference. These are listed below with the
names of the workshop organizers and instructors.
WFl XRF QUANTITATION FOR BEGINNERS I; G. R. Lachance, Geological Survey
of Canada (chair); and Michael Rokosz, Ford Motor Co.
WDl RANDOM AND SYSTEMATIC ERRORS IN XRO; G. J. McCarthy, North Dakota
State University (chair); T. G. Fawcett, Dow Chemical Co.;
G. P. Hamill, GTE Laboratories; R. Jenkins, International Centre for
Diffraction Data; and W. N. Schreiner, Philips Laboratories.
WF2 XRF QUANTITATION FOR BEGINNERS II; G. R. Lachance, Geological Survey
of Canada (chair); and Michael Rokosz, Ford Motor Co.
WD2 USE/ABUSE OF STANDARDS FOR XRD; C. R. Hubbard, Oak Ridge National
Lab (chair); D. Beard, Siemens Allis; W. Wong-Ng, National Bureau of
Standards; G. J. McCarthy, North Dakota State University; and
T. G. Fawcett, Dow Chemical Co.
WD3 MICRODENSITOMETER METHODS; Allan Brown, Studsvik Nuclear, Sweden
(chair); and C. M. Foris, E.I. duPont de Nemours (chair).
WF3 NEW X-RAY CHARACTERISTIC LINE NOMENCLATURE; R. Jenkins,
International Centre for Diffraction Data (chair).
WF4 XRF SAMPLE PREPARATION I; V. E. Buhrke, The Buhrke Co. (chair);
Vlad Kocman, Domtar Inc., Canada; Robert Wilson, Westinghouse
Hanford; Signa Fegley, Jessop Steel; Brad Wheeler, Link Analytical;
Alyssa Malen, Construction Tech Labs Div. Portland Cement; and
Fernand Claisse, Corporation Scientifique Claisse, Quebec.
WD4 DIFFRACTION PEAK BROADENING ANALYSIS; R. J. DeAngelis, University of
Kentucky (chair); and Ashok G. Dhere, E. I. duPont., Chattanooga, TN.
WFS XRF SAMPLE PREPARATION II; V. E. Buhrke, The Buhrke Co. (chair);
Vlad Kocman, Domtar Inc., Canada; Robert Wilson, Westinghouse
Hanford; Signa Fegley, Jessop Steel; Brad Wheeler, Link Analytical;
Alyssa Malen, Construction Tech Labs Div. Portland Cement; and
Fernand Claisse, Corporation Scientifique Claisse, Quebec.
WF6 INTERFACING XRF/XRD EQUIPMENT TO PC's; J. C. Russ, North Carolina
State University (chair); and Ted Satterfield, The Nucleus, Oak
Ridge, TN; D. C. Leepa, Brimrose Corp.; and Tom Baum, Kaufman, TX.
WDS MONOCHROMATIZATION TECHNIQUES; R. Jenkins, International Centre for
Diffraction Data (chair); Don Beard, Siemens Energy & Automation.
PREFACE ix
The total number registered for the conference was 413, over 260 of
whom registered for one or more workshops. We are particularly indebted
to the workshop organizers and instructors who gave unselfishly of their
time and experience to make the workshops an outstanding part of the
conference.
The conference dinner attendance was 185. A memorable evening of
entertainment was provided by "The Powdermen," after the dinner.
On behalf of the organ1z1ng committee, I would like to sincerely
thank the plenary session chairman, the invited speakers, the special
session chairmen, the contributed session chairmen (J. P. Willis, G. R.
Lachance, T. K. Smith, M. Rokosz, I. C. Noyan, G. M. Borgonovi, J. D.
Zahrt and R. Rousseau), the poster session chairmen (S. Piorek, Y. Gohshi,
C. S. Barrett and C. R. Hubbard) and the authors for their contributions.
The exceptional efforts of all these people made the sessions a great
success.
My special thanks to the Conference staff: Louise Carlson, Penny
Eucker, John Getty, Lucien Hehn, Jim Ludlam, Brenda Ziegler, and to the
Conference secretary, Lynne Bonno, all of whom worked long and unusual
hours to make the Conference successful.
Paul K. Predecki
for the Organizing Committee
January 1989
UNPUBLISHED PAPERS
The following papers were presented at the conference but are not
published here for various reasons.
"Quantitative Determination of Mineral Phases in Sand by X-Ray
Diffraction," R. M. Abu-Eid and 1. Abdul-Rahman, Kuwait Institute for
Scientific Research, Safat, Kuwait.
"Matrix Effect in X-Ray Fluorescence Analysis: A Practical Approach,"
R. M. Abu-Eid and I. Abdul-Rahman, Kuwait Institute for Scientific
Research, Safat, Kuwait.
"What is Synchrotron Radiation?" B. W. Batterman, Cornell University,
Ithaca, NY.
"Enhancement of L3 Subshell X-Ray Fluorescence Cross-Sections due to
Coster-Kronig Transitions," C. Bhan and B. Singh, Haryana Agricultural
University, Hisar, India; S. N. Chaturvedi and N. Nath, Kurukshetra
University, India.
"Quantitative Multicomponent Analysis by X-Ray Diffraction Using the
Rietveld Method," D. L. Bish, Los Alamos National Lab, NM; and S. A.
Howard, University of Missouri, Rolla, MO.
"Comparison of a Solid State Si Detector to a Conventional Scintillation
Detector-Monochromator System in X-Ray Diffraction Analysis of Geological
Materials," D. L. Bish and S. J. Chipera, Los Alamos National Laboratory,
NM.
"Development and Optimization of a Thin Film Attachment for a Standard
D500 Diffractometer," N. BroIl and M. Haase, Siemens AG, Karlsruhe, West
Germany.
x PREFACE
"Synchrotron Radiation Facilities," D. Chapman, Brookhaven National Lab,
Upton, NY.
"An Evaluation of the Rietveld Technique for Quantitative Analysis by
X-Ray Powder Diffraction," J. Cline, National Bureau of Standards,
Gaithersburg, MD.
"The Measurement of the Residual Strain in Polytetrafluoroethylene and
Polypropylene Pipe Liners Using X-Ray Diffraction," C. E. Crowder, Dow
Chemical Company, Midland, MI.
"Quantitative Phase Analysis through Digitized XRD Patterns,"
E. P. Farley, SRI International, Menlo Park, CA.
"Changes in Cu K-alpha Emission from YBa2Cu307_o Compounds,"
S. Fukushima and Y. Gohshi, Univ. of Tokyo, Japan; S. Kohiki, Matsushita
Technoresearch, Osaka, Japan; T. Wada, Matsushita Electric Industries,
Osaka, Japan.
"FDPP - An Interactive Program for the Processing of Digitized Fiber
Diffraction Patterns," K. H. Gardner and R. M. Hilmer, E. I. DuPont,
Wilmington, DE.
"Digital X-Ray Imaging of the Crystallinity in Polymers," R. W. Green,
M. F. Garbauskas and D. G. LeGrand, General Electric Co., Schenectady, NY.
"Computed Tomography Concepts in Micro XRF-Imaging, " N. Gurker, M.
Bavdaz, Technical University Vienna, Austria; A. Knochel and W. Peterson,
University Hamburg, Germany
"XRD Methods for Thin Film Analysis," E. Houtman, Philips I&E Division,
Almelo, The Netherlands
"Applications of X-Ray Thin Film Diffraction Method," M. Katayama and
M. Shimizu, Kawasaki Steel Corporation, Japan.
"Thickness Monitoring of Thin Composite Films Using DQM and X-Ray
Fluorescence Technique," D. K. Kaushik, Dayanand College, Hisar, India;
C. Bhan, Haryana Agricultural Univ., Hisar, India; S. K. Chattopadhyaya and
N. Nath, Kurukshetra Univ., India.
"Observation of Grain Growth during Secondary Recrystallization in
Grain-Oriented Silicon Steel with White X-Ray Topography by Synchrotron
Radiation," K. Kawasaki and M. Matsuo, Nippon Steel Corporation, Kawasaki,
Japan.
"X-Ray Diffraction Pattern Fitting Analysis of Phases in High
Temperature Superconducting Copper Oxides," M. Kimura and M. Matsuo,
Nippon Steel Corp., Kawasaki, Japan.
"Advances in Elemental and Chemical State Imaging in Two and Three
Dimensions using Synchrotron Radiation," J. H. Kinney, Q. C. Johnson and
R. A. Saroyan, Lawrence Livermore National Laboratory, Livermore, CA;
M. C. Nichols, Sandia National Laboratories, Livermore, CA; U. Bonse and
R. Nusshardt, University of Dortmund, W. Germany.
"Determination of Fillers in Paper by X-Ray Fluorescence Spectrometry
using Pulverized Samples," V. Kocman and L. M. Foley, Domtar Inc., Quebec.
"Application of Low-Cost XRF Technology to On-Line Analysis," S. R.
Little, ASOMA Instruments, Inc., Austin, TX
"Nondestructive Measurement of Layer Thicknesses in Double
Heterostructures by X-Ray Diffraction," A. T. Macrander, S. Lau, K. Strege
and S.N.G. Chu, AT&T Bell Laboratories, Murray Hill, NJ.
"X-Ray Microdiffraction using Dual Nickel-Coated Focusing Mirrors and a
Two Dimensional Position Sensitive Detector," T. F. McNulty, R. A. Larsen
and J. M. Quigley, Nicolet Instrument Corp., Madison, WI.
"Development of a High Resolution X-Ray Powder Diffractometer and its
Evaluation," S. Munekawa, Rigaku Corporation, Akishima, Japan; and
H. Toraya, Nagoya Institute of Technology, Tajimi, Japan.
"Flow Visualization in Heterogeneous Core Samples Using X-Ray Computed
Tomography," K. Narayanan, H. A. Deans, and W. F. Massell, University of
Houston, Houston, TX.
PREFACE xi
"A General Geometric Modelling Approach for the Monte Carlo Simulation
of Tomographic Systems," T. H. Prettyman, R. P. Gardner and K. Verghese,
North Carolina State University, Raleigh, NC.
"XRF Analysis of Tool Steel with Theoretical Alpha Correction,"
X. Ronghou, L. Jinsheng and L. Yun, Central Iron & Steel Research
Institute, Beijing, China.
"A Simple and Accurate Technique for Thin-Film X-Ray Fluorescence
Analysis of Geologic Samples," D. K. Smith, Lawrence Livermore National
Lab, Livermore, CA; and L. H. Cohen, University of California, Riverside,
CA.
"On-Line X-Ray Fluorescence Measurements," G. B. Ury, Amoco Research
Center, Naperville, IL.
"A Critical Comparison of X-Ray Diffraction and Barkhausen Noise
Measurement of Residual Stress in 4340M Steel," D. M. Walker, Boeing
Commercial Airplane Company, Seattle WA.
"Resolution of Practical Problems in the Residual Stress Analysis of CP
Titanium Welds," D. M. Walker, Boeing Commercial Airplane Company,
Seattle, WA.
"Criteria for Selecting a WD-XRF Spectrometer," P. L. Warren and A. E.
Smith, Wilton Materials Research Centre, Cleveland, England.
"Mathematical Correction Models in X-Ray Fluorescence Utilizing
Regression Analysis," B. D. Wheeler, LINK Analytical, Redwood City, CA
"Compton (Incoherent) Scattering of Sample Spectral Lines in XRFS (1):
Evidence for the Phenomenon and Resulting Analytical Errors," J. P.
Willis, University of Cape Town, Rondebosch, South Africa.
"Compton (Incoherent) Scattering of Sample Spectral Lines in XRFS (2):
Problems in the Accurate Determination of Net Spectral Line Intensities in
Samples of Low Mass Absorption Coefficient," J. P. Willis, University of
Cape Town, Rondebosch, South Africa.