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Influence of the Method of Measurement on the Optical Aniaotropy Factor OPTAF of Pyro- R.A.Rhan

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Influence of the Method of Measurement on the Optical Aniaotropy Factor OPTAF of Pyro- R.A.Rhan 2)#- /d 7J> 0 FORMAL REPORT GERHTR-T35- - UNITED STATES—GERMAN HIGH TEMPERATURE REACTOR RESEARCH EXCHANGE PROGRAM Original report number 082-RW____________________ Title Influence of the Method of Measurement on the Optical Aniaotropy Factor OPTAF of Pyro- r.a.rhan Author(si K. Koizlik et al. Originating Installation Kemforschungsanlage Julich. fiesellschaft mlt beachrankter Haftung Date of original report issuanoe. July IQjk ________ Reporting period covered________ —---------------------------- NOTICE--------------------------------- Translated from the original German This report was prepared as an account of work sponsored by the United States Government. Neither the United States nor the United States Energy This report, translated wholly or in part from the original Research and Development Administration, nor any of language, has been reproduced directly from copy pre­ their employees, nor any of their contractors, subcontractors, or their employees, makes any pared by the United States Mission to the European warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness Atomic Energy Community or usefulness of any information, apparatus, product or process disclosed, or represents that its use would not infringe privately owned rights. THIS REPORT MAY BE GIVEN UNLIMITED DISTRIBUTION I USERDA Technical Information Center, Oak Ridge, Tennessee NOTICE This rep (Visions of the %. MASTER arrangement and is subject to the terms thereof. DJ.SJMaiQlQM Q£ IMS DOCUMENT IS ilMMI DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. GEKHTR - 135 Distribution Category UC-77 KERNFORSCHUNGSANLAGE JULICH Gesellschaft mit beachrankter Haftttng Institute of Reactor Materials Influence of the Method of Measurement on the Optical Anisotropy Factor OPTAF of Pyrocarbon by K. Koizlik, K. TSuber, H. Nickel and H. Wasmund* Jul - 1082 - RW July 197% * E. Leitz GmbH, Wetzlar Printed as manuscript Oh the Influence of the Hethod of Bber den Einfluss des Hessverfahrens auf den Measurement on the Optical Anisotropy Factor Wert des optischen Anisotropiefaktors OPTAF OPTAF of Pyrocarbon von Pyrokohlenstoff by von K. Koizlik K. Koizlik K. TSuber K. TSuber H. Nickel . H- Nickel H. Wasmund ' H. Wasmund ' ABSTRACT KURZFASSUNG This study describes the development and installation of an auto­ Die vor1iegende Arbeit beschreibt die Entwicklung und Installation matic microscope photometer for the measurement of the optical eines automatischen Mikroskopphotometers zur Hessung des optischen anisotropy factor OPTAF on the pyrocarbon coatings of fuel parti­ Anisotropiefaktors OPTAF an den Pyrokohl enstof fhiil Is chichten von cles . After a short representation of the physical basis of this Brennstoffteilchen. Nach einer kurzen Einfiihrung in die physika 1 i- procedure the new microscope photometer is introduced. First meas­ schen Grundlagen des MeBverfahrens wird das MeBgerSt vorgestelIt. urements for the adaptation of the new instrument of the so far Erste Messungen zur Anpassung des neuen an das bisher verwendete used microscope photometer are discussed. By these measurements GerSt werden diskutiert. Anhand dieser Messungen wird der Einflufi the influence of the instrument on the value of OPTAF in the case des Mikroskopphotometers bei bestimmten MeBablSufen auf den OPTAF of some special ways of measuring are explained and the appearance erklSrt und die Erscheinung einer scheinbaren Anisotropic begrundet. of an apparent anisotropy is interpreted. + ) + ^ Fa. £. Leitz GmbH» Wetzlar Fa. E. Leitz GmbH, Wetzlar Table of Contents Page 1 Introduction 1. Introduction 2 The course of development of coated fuel particles for use in gas-cooled high temperature 2. Physical Principles of the Optical reactors (Kefs. 1 and 2), which is not yet Anisotropy Determination 5 complete even today, has necessitated all the time new and more accurate characterization 3* Microscope Photometer for Manual procedures. These procedures, which have Measurement 11 been devised in parallel with the continuous improvement in the production processes, Microscope Photometer for Automatic are aimed primarily at as complete as possible Measurement 17 a characterization of the coating material 4.1 Microscope Photometer 17 of the coated fuel particles, the pyrocarbon. Among the few, initially measurable material 4.2 Electronic Control 21 parameters particular importance was attached very early on to the anisotropy of the crystal­ 5* Calibration of the Automatic Measuring lographic orientation of the pyrocarbon in Microscope 24 regard to the use of the latter in the reactor 5.1 Apparent Orientation Anisotropy 26 (Ref. 3). In consequence of this the measurement of the orientation anisotropy became an 5.2 Apparent Orientation Anisotropy in essential part of the process of fuel particle Pyrocarbon Samples 31 characterization. 5*3 Influence of the Apparent Orientation Anisotropy on Measurement with the MPV XI 36 To permit investigations to be carried out 6. Summary 38 directly on the particle coatings, a new measuring technique had to be developed, since the classical X-ray method of structural determination was found at the time to be unsuitable, in particular as a result of the spherical symmetry of the orientation anisotropy of the particle coatings. Although an X-ray method (Ref. 4) is today available for this purpose, it is not as yet of far- reaching importance in view of the relatively complicated evaluation of the primary measurements. It has long been known, on the other hand, that pyrocarbon possessed the property, like graphite, of exhibiting the phenomenon of bireflection (Refs. 5 and 6). This property 1 2 - is manifested in qualitative terms by the appearance on suitably ground and polished pyrocarbon surfaces, exposed to vertical illumination with linearly polarized light using crossed polarizers, of a so-called "Maltese cross" (Ref, 7)• Fig, 1 shows the Maltese cross in diagrammatic form and on a particle micrograph. The Maltese cross becomes progressively clearer, the closer the alignment of the c-axes of the pyrocarbon crystallites parallel to the preferred direction, in other words the higher the value of the orientation anisotropy (Ref, 8) of the material. Although therefore there is a qualitative correlation between the intensity of the Maltese cross and the orientation anisotropy of pyrocarbon, no dear, quantitative relation between the Fig. 1 i Maltese cross on an equatorial section of a two can be established (Ref, 9)• coated particle, on the left in a photo­ graph and on the right in diagrammatic form However, the attempt to make use of miorophotometry (Refs, 10 and 11), which has been used for several decades, *.g., in mineralogy, as a key importance that it did a few years ago, new method of measurement of the orientation but is merely regarded as one, albeit important anisotropy proved successful. characteristic among other decisive material properties. This method, which is also based on the bireflection phenomenon, permits a quantitative In the last two years, however, a microscope determination to be made of the orientation photometer with the corresponding equipment anisotropy of pyrocarbon with a high local has been developed for a largely automatic resolution. The use of microphotometry measurement of the orientation anisotropy, which represents a considerable improvement in this field began after 1965 and led to the development of various technically dif­ on the original laboratory instrument. The reason for this is that orientation anisotropy ferent instruments (Refs, 12-1%). The development has established itself as a characterization of the method may today be regarded as in parameter which is simple to measure but principle complete (Refs. 15 and 16). The nevertheless, of great statement value. improved knowledge of the material pyrocarbon, This means that the number of samples for its material parameters and its irradiation analysis is correspondingly high, in particular behavior in the reactor have meant that in the case of highly radioactive coated orientation anisotropy no longer has the fuel particles from irradiation experiments, 3 - % _ In. addition orientation anisotropy is gaining a function of the angle between the direction new importance in the study of the separation of polarization and the c-axis of the crystal : mechanism of pyrocarbon from the gas phase. if the direction of polarization and the This frequently involves in particular the c-axis are parallel, the reflection capacity need for systematic serial measurements, reaches its minimum value at 8 %, whereas which involve t&» use of large* numbers of if they are perpendicular, the maximum personnely unless carried out by means of value will be reached at 28 %. No variation an automated procedure. in the reflection capacity occurs in the case of reflection in the (a,c) and (b,c) planes, since the a and b direction of The present paper is a report on the new the graphite monocrystal are optically method of measurement. Comparative measurements identical. Fig. 2 shows in diagrammatic are described between the old, physically form the bireflection effect. simple instrument and the new photometer, which enable the correlation which was previously obtained (Ref. 1?) between X-ray measurements In the case of polycrystalline pyrocarbon, and optical determinations of the orientation which is believed to be built up only from anisotropy, to be applied to the
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