Nuclear fuel technology - Sintered (U,Pu)O2 pellets - Guidance for ceramographic preparation for microstructure examination (ISO 22765:2016)

ISO 22765:2016 describes the ceramographic procedure used to prepare sintered (U,Pu)O2 pellets for qualitative and quantitative examination of the pellet microstructure.
The examinations are performed before and after thermal treatment or chemical etching.
They allow
-      observation of any cracks, intra- and intergranular pores or inclusions, and
-      measurement of the grain size, porosity and plutonium homogeneity distribution.
The mean grain diameter is measured by one of the classic methods: counting (intercept method), comparison with standard grids or typical images, etc.[2] The measurement of individual grain sizes requires uniform development of the microstructure over the entire specimen.
The plutonium cluster and pore distribution and localization are generally analysed by automatic image analysis systems. The plutonium distribution is usually revealed by chemical etching but alpha-autoradiography can also be used. The first technique avoids the tendency for autoradiography to exaggerate the size of plutonium-rich clusters due to the distance the alpha particles travel away from the source.

Kernbrennstofftechnologie - Gesinterte (U,Pu)O2-Pellets - Leitfaden für die keramographische Herstellung der Proben zur Untersuchung des Feingefüges (ISO 22765:2016)

Dieses Dokument beschreibt das keramographische Verfahren zur Vorbereitung von gesinterten (U,Pu)O2 Pellets für die qualitative und quantitative Untersuchung der Pellet Mikrostruktur.
Die Untersuchungen werden vor und nach der Wärmebehandlung oder dem chemischen Ätzen durch-geführt.
Sie ermöglichen
   die Beobachtung von jeglichen Rissen, von Poren im und zwischen dem Granulat oder von Einschlüssen und
   die Messung der Korngröße, Porosität und Homogenitätsverteilung des Plutoniums.
Der mittlere Korndurchmesser wird nach einem der klassischen Verfahren gemessen: Zählen (Intercept-Verfahren), Vergleich mit Standardrastern oder typischen Bildern usw. [2]. Die Messung einzelner Korn-größen erfordert die gleichmäßige Entwicklung der Mikrostruktur über die gesamte Probe.
Die Verteilung der Plutonium Cluster und -Poren und deren Lokalisierung werden in der Regel mit auto-matischen Bildanalysesystemen analysiert. Die Plutoniumverteilung wird in der Regel durch chemisches Ätzen festgestellt, es kann aber auch die Alpha Autoradiographie verwendet werden. Die erste Technik vermeidet die Tendenz der Autoradiographie, die Größe plutoniumreicher Cluster aufgrund des Abstandes, den die Alpha Partikel von der Quelle zurücklegen, als zu groß wiederzugeben.

Technologie du combustible nucléaire - Pastilles (U,Pu)O2 frittées - Préconisations relatives à la préparation céramographique pour examen de la microstructure (ISO 22765:2016)

ISO 18610:2016 décrit la procédure céramographique utilisée pour préparer des pastilles de (U,Pu)O2 frittées afin de réaliser des examens qualitatifs et quantitatifs de leur microstructure.
Ces examens sont réalisés avant et après un traitement thermique ou une attaque chimique.
Ils permettent:
-      l'observation d'éventuels fissures, pores inter- et intragranulaires ou inclusions; et
-      le mesurage des tailles de grains, de la porosité et de l'homogénéité de la distribution du plutonium.
Le diamètre de grain moyen est mesuré par l'une des méthodes classiques suivantes: comptage (méthode par interception), comparaison à des grilles normalisées ou des images types, etc[2]. Le mesurage des dimensions du grain requiert la révélation uniforme de la microstructure sur l'ensemble de l'échantillon.
La localisation et la distribution des pores et des agglomérats de plutonium sont en général analysées par des systèmes automatiques d'analyse des images. La distribution du plutonium est, en règle générale, mise en évidence par une attaque chimique mais il est également possible d'utiliser l'autoradiographie alpha. La première technique évite la tendance propre à l'autoradiographie, d'exagérer la taille des agglomérats riches en plutonium en raison de la distance parcourue par les particules alpha depuis la source.

Tehnologija jedrskih goriv - Sintrani peleti (U,Pu)O2 - Navodilo za pripravo keramografske preiskave mikrostrukture (ISO 22765:2016)

Keramografski postopek, ki se uporabi za pripravo sintranih peletov (U,Pu)O2 za kvalitativno in kvantitativno preiskavo mikrostrukture peletov.
Preiskave se izvedejo pred in po toplotni obdelavi ali kemičnem jedkanju.
Omogočajo:
– opažanje morebitnih razpok, intra- in intergranularnih por ali vključkov ter
– meritve velikosti zrna, poroznosti in homogenosti porazdelitve plutonija.
Povprečni premer zrna je izmerjen z eno od klasičnih metod: štetje (metoda preseka), primerjava s standardnimi mrežami ali značilnimi slikami itd.[2] Izmera velikosti posameznega zrna zahteva poenoten razvoj mikrostrukture v celotnem primerku.
Skupki plutonija in razporeditev ter lokalizacija por so običajno analizirani s samodejnimi sistemi slikovne analize. Razporeditev plutonija se običajno razkrije s kemičnim jedkanjem, lahko pa se uporabi tudi alfa avtoradiografija. S prvo tehniko se izognemo težnji avtoradiografije, da poda preveliko velikost skupkov, bogatih s plutonijem, zaradi razdalje, ki jo delci alfa prepotujejo od vira.

General Information

Status
Published
Publication Date
11-Jun-2019
Withdrawal Date
30-Dec-2019
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
12-Jun-2019
Due Date
28-Nov-2020
Completion Date
12-Jun-2019

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SLOVENSKI STANDARD
01-september-2019
Tehnologija jedrskih goriv - Sintrani peleti (U,Pu)O2 - Navodilo za pripravo
keramografske preiskave mikrostrukture (ISO 22765:2016)
Nuclear fuel technology - Sintered (U,Pu)O2 pellets - Guidance for ceramographic
preparation for microstructure examination (ISO 22765:2016)
Kernbrennstofftechnologie - Gesinterte (U,Pu)O2-Pellets - Leitfaden für die
keramographische Herstellung der Proben zur Untersuchung des Feingefüges (ISO
22765:2016)
Technologie du combustible nucléaire - Pastilles (U,Pu)O2 frittées - Préconisations
relatives à la préparation céramographique pour examen de la microstructure (ISO
22765:2016)
Ta slovenski standard je istoveten z: EN ISO 22765:2019
ICS:
27.120.30 Cepljivi materiali in jedrska Fissile materials and nuclear
gorivna tehnologija fuel technology
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 22765
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 27.120.30
English Version
Nuclear fuel technology - Sintered (U,Pu)O2 pellets -
Guidance for ceramographic preparation for
microstructure examination (ISO 22765:2016)
Technologie du combustible nucléaire - Pastilles Kernbrennstofftechnologie - Gesinterte (U,Pu)O2-
(U,Pu)O2 frittées - Préconisations relatives à la Pellets - Leitfaden für die keramographische
préparation céramographique pour examen de la Herstellung der Proben zur Untersuchung des
microstructure (ISO 22765:2016) Feingefüges (ISO 22765:2016)
This European Standard was approved by CEN on 8 March 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22765:2019 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
The text of ISO 22765:2016 has been prepared by Technical Committee ISO/TC 85 "Nuclear energy,
nuclear technologies, and radiological protection” of the International Organization for Standardization
(ISO) and has been taken over as EN ISO 22765:2019 by Technical Committee CEN/TC 430 “Nuclear
energy, nuclear technologies, and radiological protection” the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 22765:2016 has been approved by CEN as EN ISO 22765:2019 without any modification.

INTERNATIONAL ISO
STANDARD 22765
First edition
2016-12-15
Nuclear fuel technology — Sintered
(U,Pu)O pellets — Guidance for
ceramographic preparation for
microstructure examination
Technologie du combustible nucléaire — Pastilles (U,Pu)O frittées
— Préconisations relatives à la préparation céramographique pour
examen de la microstructure
Reference number
ISO 22765:2016(E)
©
ISO 2016
ISO 22765:2016(E)
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
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Tel. +41 22 749 01 11
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copyright@iso.org
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ii © ISO 2016 – All rights reserved

ISO 22765:2016(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Description . 2
6 Equipment . 2
7 Reagents and resin . 2
8 Operating procedure . 3
8.1 Specimen cutting . 3
8.2 Resin embedding . 3
8.3 Rough polishing . 3
8.4 Final polishing . 3
9 Structure development . 4
9.1 General . 4
9.2 Development by thermal treatment . 4
9.3 Development by chemical etching . 4
9.4 Development by ion etching . 5
Bibliography . 7
ISO 22765:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directives
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received. www.iso.org/patents
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assessment, as well as information about ISO’s adherence to the World Trade Organization (WTO)
principles in the Technical Barriers to Trade (TBT), see the following URL: http://www.iso.org/iso/
foreword.html
The committee responsible for this document is ISO/TC 85, Nuclear energy, nuclear technologies, and
radiological protection, Subcommittee SC 5, Nuclear installations, processes and technologies.
iv © ISO 2016 – All rights reserved

INTERNATIONAL STANDARD ISO 22765:2016(E)
Nuclear fuel technology — Sintered (U,Pu)O pellets
— Guidance for ceramographic preparation for
microstructure examination
1 Scope
This document describes the ceramographic procedure used to prepare sintered (U,Pu)O pellets for
qualitative and quantitative examination of the pellet microstructure.
The examinations are performed before and after thermal treatment or chemical etching.
They allow
— observation of any cracks, intra- and intergranular pores or inclusions, and
— measurement of the grain size, porosity and plutonium homogeneity distribution.
The mean grain diameter is measured by one of the classic methods: counting (intercept method),
[2]
comparison with standard grids or typical images, etc. The measurement of individual grain sizes
requires uniform development of the microstructure over the entire specimen.
The plutonium cluster and pore distribution and localization are generally analysed by automatic
image analysis systems. The plutonium distribution is usually revealed by chemical etching but alpha-
autoradiography can also be used. The first technique avoids the tendency for autoradiography to
exaggerate the size of plutonium-rich clusters due to the distance the alpha particles travel away from
the source.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
The ceramographic preparation of (U,Pu)O pellets involves two steps:
— specimen polishing, after embedding or not the specimen in a specific resin;
— thermal treatment or chemical etching to reveal the specimen microstructure.
ISO 22
...

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