m * The ORNL 10-m Small-Angle X-Ray Scattering Camera OAK RIDGE NATIONAL LABORATORY

170 Pages·2011·3.64 MB·English

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ORNL/TM-6342
OAK
RIDGE
NATIONAL
m*
LABORATORY
The ORNL 10-m Small-Angle
X-Ray Scattering Camera
R. W. Hendricks
n
OPERATED BY
UNION CARBIDE CORPORATION ;
FOR THE UNITED STATES
DEPARTMENT OF ENERGY
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Contract No. W-7405-eng-26
METALS AND CERAMICS DIVISION
THE ORNL 10-m SMALL-ANGLE X-RAV SCATTERING CAMERA
R. W. Hendricks
Date Published: December 1979
OAK RIDGE NATIONAL LABORATORY
Oak Ridge, Tennessee 3783O
operated by
UNION CARBIDE CORPORATION
for the
DEPARTMENT OF ENERGY
Printed in the United States of America. Available from
National Technical Information Service
U.S. Department of Commerce
5285 Port Royal Road, Springfield, Virginia 22161
NTIS price codes—Printed Copy: A11 Microfiche A01
This report was prepared as an account of work sponsored by an agency of the
United States Government. Neither the United States nor any agency thereof, nor
any of their employees, makes any warranty, expressed or implied, or assumes
any legal liability or responsibility 'ny third party's use or the results of sucli
use of any information, apparatus,, oduct or process disclosed in this report, or
represents that its use by such third party would not infringe privately owned
rights.
TABLE OF CONTENTS
Page
"V.I OVERVIEW
ABSTRACT 1-1
INTRODUCTION 1-1
GEOMETRICAL CONSIDERATIONS 1-4
THE CAMERA 1-8
THE DETECTOR 1-13
THE COMPUTER 1-17
THE INTERFACE 1-19
SOFTWARE 1-23
SYSTEM PERFORMANCE 1-27
APPLICATIONS . . 1"30
CONCLUSIONS . . 1-^0
V.2 X-RAY SOURCE
V. 3 CAMERA DESIGN
V.l» TWO-DIMENSIONAL POSITION-SENSITIVE DETECTOR
V.5 HIGH-SPEED DATA ACQUISITION INTERFACE HARDWARE
V.6 MOTOR INTERFACE HARDWARE
V.7 CAMAC INTERFACE
V.8 COMPUTER OPERATING SYSTEM AND SYSTEM GENERATION SOFTWARE
V.9 SYMBIONT DEVICES (OTI, E27, TEK, LPT, AND TIP)
V.10 ON-LINE GRAPHICS
*V.ll CAMERA CONTROL PROGRAMS (SAX, OVF, AND MOT)
ABSTRACT 11-1
INTRODUCTION 11-1
DATA STRUCTURES 11-2
PROGRAM OVF 11-8
PROGRAM MOT 11-8
PROGRAM SAX 11-9
SAX OPERATOR COMMANDS 11-13
SYSTEM PROGRAMMING NOTES 11-38
APPENDIX A - PROGRAM OVF SOURCE LISTING U-39
APPENDIX B - PROGRAM MOT SOURCE LISTING 11-43
APPENDIX C - PROGRAM SAX SOURCE LISTING 11-47
APPENDIX D - EXAMPLES OF THE USE OF PROGRAM SAX 11-67
APPENDIX E - PROCEDURES FOR COMPILING, LINK-EDITING, AND
CATALOGUING PROGRAM SAX 11-71
V.12 MICROPROCESSOR DATA TRANSFER SOFTWARE
if
Page
•V.13 FILE MANAGEMENT PROGRAMS (MANAGER, FETCH AND SAVE)
ABSTRACT 13~ 1
INTRODUCTION 13-1
DATA STRUCTURES 13~2
PROGRAM MANAGER 13-4
MANAGER OPERATOR COMMANDS 13~9
SUBROUTINE FETCH 13-25
SUBROUTINE SAVE 13-26
SYSTEM PROGRAMMING NOTES 13~27
APPENDIX A - SOURCE LISTING OF PROGRAM MANAGER 13-29
APPENDIX B - SOURCE LISTING OF SUBROUTINE FETCH 13~39
APPENDIX C - SOURCE LISTING OF SUBROUTINE SAVE 13-43
V. 11t DATA ANALYSIS SOFTWARE
V.15 IBM 360/91 BATCH DATA ANALYSIS PROGRAMS
V.16 PDP-10 TIME-SHARING DATA ANALYSIS PROGRAMS
V.17 SPECIAL SAMPLE HOLDERS
V.18 -DYNAMIC DEFORMATION DEVICE
V.19 CONSTRUCTION OF LABORATORY BUILDING
V.20 OPERATOR'S GUIDE
ACKNOWLEDGMENTS
The ORNL 10-m small-angle x-ray scattering camera is a unique,
state-of-the-art, computer-control led facility and represents an invest-
ment of approximately $500,000. It was developed by a team of approxi-
mately 30 engineers, programmers, technicians and craftsmen, all of whom
contributed significantly to its outstanding success. This report, in
which each chapter is authored by those individuals principally involved
in a specific aspect of the instrument, provides complete hardware and
software documentation for the facility. It is presented in a loose-
leaf format with the pages numbered by chapter. In this way each volume
may be updated from time to time as appropriate changes and/or enhance-
ments to the system are made. As updated pages are prepared, the
corrected text will be denoted by a solid b-->r in the left margin, as
illustrated here. In the following Table','of. Contents, an asterisk (~)
(left-hand side) indicates that the volunt as been published. The
remaining volumes will be published in the r»sar future. The Table of
Contents has been designed to serve as a subject index to the entire
report.
Special thanks must go to the following: J. E. Weidley and
R. H. Ward who designed the mechanical aspects of the camera and
H. N. Elmore, W. L. Hylton, T. F. Roberts, J. C. Ogle, J. Adams, and
D. E. Tumlin who constructed it; M. K. Kopp who designed the two-
dimensional position-sensitive detector, W. T. Clay who supervised Its
construction and testing, and C. E. Fowler, Jr. for his great skill in
assembling it; W. J. McClain, R. W. Napier, K/I T. Roseberry, and
J. W. Woody, Jr. for their role in specifying' and procuring the computer;
J. C. Twichell who conceived and designed the interface and motor driver
hardware, C. C. Johnson whose knowledge of the ModComp CPU was instru-
mental in successful installation of the interface, R. G. Upton who
supervised the construction and debugging of the interface components,
J. A. Ramsey and R. R. Bentz who did all of the assembly of the various
boards, M. Liccardo of Scientific Micro Systems.who provided invaluable
help with the microcontroller, and W. Strauss of Modular Computer Systems
who helped design, code, and prepare the custom ROMs for the communica-
tions processor; and R. L. Stephenson, N. A. Betz, J. S. Lin, R. D. Carlson,
and T. C. Tucker who wrote some of the special-purpose software. My ./
colleagues, B. S. Borie, R. D. Carlson, J. S. Lin, C. J. Sparks, and
H. L. Yakel provided continuous help through their discussions of geo-
metrical optics of the system, monochromator design, and general aspects
of the camera. Finally, such a project could not have been successful
without the continuous support and encouragement of H. L.^Yakel,
C. J. McHargue, J. R. Weir, and A. Zucker. I am grateful to all of
these individuals.
ORNL/TM-6342
INTERNAL DISTRIBUTION
1-2. Central Research Library 62-63. J. S. Lin
3. Document Reference Section 6k. C. J. McHargue
4-5. Laboratory Records Department 65. H. Postma
6. Laboratory Records, ORN. iRC 66. R. L. Stephenson
7. CRNL Patent Office 67. J. 0. Stiegler
8. H. R. Child 68. D. B. Trauger
9-58. R. W. Hendricks 69. J. R. Weir, Jr.
59. M. R. Hill 70. H. L. Yakel
60. S. P. King 71. A. Zucker
61. W. C. Koehler
EXTERNAL DISTRIBUTION
72-73. USDOE, Division of Material Sciences, Washington, DC 205*»5
L. C. lanniello
D. K. Stevens
Ik. USDOE, Oak Ridge Operations Office, P. 0. Box E, Oak Ridge,
TN 37830
Assistant Manager, Energy Research and Development
75—101. Technical Information Center, Office of Information Services,
P. 0. Box 62, Oak Ridge, TN 37830
A
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0RNL/TM-6342/V1
OAK
RIDGE
NATIONAL
LABORATORY
THE ORNL 10-m SMALL-ANGLE X-RAY SCATTERING CAMERA
Vol. 1. Overview
R. W. Hendricks
fL.
OPERATED BY f
UNION CARBIDE CORPORATION
FOB THE UNITED STATES '
DEPARTMENT OF ENERGY v
THE ORNL 10-m SMALL-ANGLE X-RAY SCATTERING CAMERA
1. OVERVIEW
ABSTRACT
A new small-angle x-ray scattering camera which utilizes
a rotating anode x-ray source, crystal monochromatization of
the incident beam, pinhole collimation, and a two-dimensional
position-sensitive proportional counter has been developed.
Because the sizos of the x-ray focal spot, the sample, and the
resolution element of the detector are each approximately
1 x 1 mm2,^ the camera was designed so that the focal spot-to-
sample and sample-to-detector distances may each be varied in
0.5~m increments up to 5 m to provide a system resolution in
the range 0.5-4.0 mrad. A large, general-purpose specimen
chamber has been provided into which a wide variety of special-
purpose specimen holders can be mounted. The detector has an
active area of 200 x 200 mm and has up to 200 x 200 resolution
elements. The data are recorded in the memory of a mini-
computer by a high-speed interface which uses a microprocessor
to map the position of an incident photon into an absolute
minicomputer memory address. With this interface, over 105
events/s can be recorded. The data recorded in the computer
memory can be processed on-line by a variety of programs
designed to enhance the user's interaction with the experi-
ment. Among these are routines for background and detector
sensitivity correction, contour and perspective plotting of
the two-dimensional data, a variety of averaging schemes for
determining circular averages and/or one-dimensional slices
of the data, file management programs to handle the large
quantity of data produced by a two-dimensional detector, and
an interactive package for communications with a central com-
puting facility via a dedicated hardwired link. At the highest
angular resolution (O.^f mrad), the flux incident on the speci-
men i s 1.0 x l G6 photons/s with the x-ray source operating
at 45 kV and 100 mA. The performance of the instrument is
demonstrated with several examples, among which are scattering
patterns from voids in neutron irradiated nickel, plastically
deformed polyethylene, and collagen fibrils. Results from a
kinetic study of the crystallization of polyethylene are also
reported. - i ^^
• W'
/ -'l. INTRODUCTION
/ ' • <
Small-angle x-ray scattering (SAXS) has long been used to study
microscopic levels of structures represented by fluctuations in electron
O &