Microbeam analysis -- Electron probe microanalysis -- Quantitative analysis of Mn dendritic segregation in continuously cast steel product

This document specifies procedures for quantitative analysis of Mn dendritic segregation in steel billets, blooms, slabs using electron probe microanalysis (EPMA). This document is mainly applicable to continuously cast products with Mn content more than 0,01Â % by mass. It can also be used for steel ingots and steel products, such as cast iron and cast steel. The minimum size of analysable dendrites is totally dependent on the resolution of microscope of EPMA and beam size of filament used for quantitative analysis.

Analyse par microfaisceaux -- Analyse par microsonde de Castaing -- Analyse quantitative de la ségrégation dendritique du manganèse dans un produit en acier coulé en continu

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Status
Published
Publication Date
08-Apr-2021
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
03-Mar-2021
Completion Date
02-Mar-2021
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INTERNATIONAL ISO
STANDARD 23692
First edition
2021-04
Microbeam analysis — Electron
probe microanalysis — Quantitative
analysis of Mn dendritic segregation in
continuously cast steel product
Analyse par microfaisceaux — Analyse par microsonde de Castaing
— Analyse quantitative de la ségrégation dendritique du manganèse
dans un produit en acier coulé en continu
Reference number
ISO 23692:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 23692:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 23692:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Selection of reference material ............................................................................................................................................................. 2

6 Sampling and specimen preparation .............................................................................................................................................. 2

6.1 Sampling ....................................................................................................................................................................................................... 2

6.2 Specimen preparation ...................................................................................................................................................................... 2

7 Calibration of the instrument ................................................................................................................................................................. 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Prepare the instrument ................................................................................................................................................................... 3

8.2 Set up the experiment parameters ........................................................................................................................................ 3

8.3 Perform the analysis........................................................................................................................................................................... 4

8.4 Process the data ..................................................................................................................................................................................... 4

9 Uncertainty ................................................................................................................................................................................................................. 5

10 Report .............................................................................................................................................................................................................................. 5

Annex A (informative) Example of quantitative mapping analysis of dendritic segregation ....................6

Annex B (informative) Example of quantitative line analysis of dendritic segregation ..................................9

Bibliography .............................................................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 23692:2021(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

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

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 (see 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 (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 202, Microbeam analysis, Subcommittee

SC 2, Electron probe microanalysis.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 23692:2021(E)
Introduction

Electron probe X-ray microanalysis (EPMA) is a modern technique used to qualitatively determine and

quantitatively measure the elemental composition of solid materials, including metal alloys, ceramics,

glasses, minerals, polymers, powders, etc., on a spatial scale of approximately one micrometer laterally

and in depth. EPMA is based on the physical mechanism of electron-stimulated X-ray emission and

X-ray spectrometry (see ISO 23833).

The dendritic segregation rich in Mn is unavoidable during steel solidification, which is the direct cause

of banded structure in steel product formed in the hot rolling process. The toughness and strength of

steel are greatly affected by the banded structure. The quantification of the dendritic segregation can

facilitate steel maker to optimize steel-making process parameters, and therefore control the banded

structure in the final product.

It is a new method to quantify the dendritic segregation through EPMA by measuring inhomogeneity

of Mn with EPMA. In order to obtain comparative and repeatable results it is necessary to standardize

this method. These enable products to be compared and evaluated for the purpose of quality control.

© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 23692:2021(E)
Microbeam analysis — Electron probe microanalysis
— Quantitative analysis of Mn dendritic segregation in
continuously cast steel product
1 Scope

This document specifies procedures for quantitative analysis of Mn dendritic segregation in steel

billets, blooms, slabs using electron probe microanalysis (EPMA).

This document is mainly applicable to continuously cast products with Mn content more than 0,01 % by

mass. It can also be used for steel ingots and steel products, such as cast iron and cast steel.

The minimum size of analysable dendrites is totally dependent on the resolution of microscope of EPMA

and beam size of filament used for quantitative analysis.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 11938, Microbeam analysis — Electron probe microanalysis — Methods for elemental-mapping

analysis using wavelength-dispersive spectroscopy

ISO 14594, Microbeam analysis — Electron probe microanalysis — Guidelines for the determination of

experimental parameters for wavelength dispersive spectroscopy

ISO 14595, Microbeam analysis — Electron probe microanalysis — Guidelines for the specification of

certified reference materials (CRMs)

ISO 22489, Microbeam analysis — Electron probe microanalysis — Quantitative point analysis for bulk

specimens using wavelength dispersive X-ray spectroscopy
ISO 23833, Microbeam analysis — Electron probe microanalysis (EPMA) — Vocabulary
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 23833 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at www .iso .org/ obp
— IEC Electropedia: available at www .electropedia .org
3.1
dendritic segregation

phenomenon that element content differs in the first-crystallized dendrite arms and post-crystallized

inter-dendritic spaces during alloy solidification in a dendritic pattern
3.2
mapping analysis

method of analysing element in EPMA, through which element distribution in an area can be obtained

© ISO 2021 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 23692:2021(E)
3.3
line analysis

method of analysing element in EPMA, through which element distribution in a specified direction can

be obtained
3.4
ratio of dendritic segregation

ratio of the maximum content in the inter-dendritic spaces and the minimum content in the dendrite

arms of the selected element in the dendritic zone of a specimen
4 Principle

Mapping analysis or line analysis is firstly performed to display the dendritic segregation of Mn

element in a certain area of steel billet. The map or line of X-ray counts can thus be obtained from the

above analysis. The calibration curve generated from a series of Mn reference
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 23692
ISO/TC 202/SC 2
Microbeam analysis - Electron probe
Secretariat: SAC
microanalysis - Quantitative analysis
Voting begins on:
2021­01­05 of Mn dendritic segregation in
continuously cast steel product
Voting terminates on:
2021­03­02
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
ISO/FDIS 23692:2021(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN­
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2021
---------------------- Page: 1 ----------------------
ISO/FDIS 23692:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH­1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 23692:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Selection of reference material ............................................................................................................................................................. 2

6 Sampling and specimen preparation .............................................................................................................................................. 2

6.1 Sampling ....................................................................................................................................................................................................... 2

6.2 Specimen preparation ...................................................................................................................................................................... 2

7 Calibration of the instrument ................................................................................................................................................................. 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Prepare the instrument ................................................................................................................................................................... 3

8.2 Set up the experiment parameters ........................................................................................................................................ 3

8.3 Perform the analysis........................................................................................................................................................................... 4

8.4 Process the data ..................................................................................................................................................................................... 4

9 Uncertainty ................................................................................................................................................................................................................. 5

10 Report .............................................................................................................................................................................................................................. 5

Annex A (informative) Example of quantitative mapping analysis of dendritic segregation ....................6

Annex B (informative) Example of quantitative line analysis of dendritic segregation ..................................9

Bibliography .............................................................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 23692:2021(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

organizations, governmental and non­governmental, in liaison with ISO, also take part in the work.

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 (see 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 (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 202, Microbeam analysis, Subcommittee

SC 2, Electron probe microanalysis.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/FDIS 23692:2021(E)
Introduction

Electron probe X-ray microanalysis (EPMA) is a modern technique used to qualitatively determine and

quantitatively measure the elemental composition of solid materials, including metal alloys, ceramics,

glasses, minerals, polymers, powders, etc., on a spatial scale of approximately one micrometer laterally

and in depth. EPMA is based on the physical mechanism of electron-stimulated X-ray emission and

X-ray spectrometry (see ISO 23833).

The dendritic segregation rich in Mn is unavoidable during steel solidification, which is the direct cause

of banded structure in steel product formed in the hot rolling process. The toughness and strength of

steel are greatly affected by the banded structure. The quantification of the dendritic segregation can

facilitate steel maker to optimize steel­making process parameters, and therefore control the banded

structure in the final product.

It is a new method to quantify the dendritic segregation through EPMA by measuring inhomogeneity

of Mn with EPMA. In order to obtain comparative and repeatable results it is necessary to standardize

this method. These enable products to be compared and evaluated for the purpose of quality control.

© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 23692:2021(E)
Microbeam analysis - Electron probe microanalysis -
Quantitative analysis of Mn dendritic segregation in
continuously cast steel product
1 Scope

This document specifies procedures for quantitative analysis of Mn dendritic segregation in steel

billets. blooms, slabs using electron probe microanalysis (EPMA).

This document is mainly applied in continuously cast product with Mn content more than 0,01 % by

mass. This method can also be used in steel ingots and steel products, such as cast iron and cast steel.

The minimum size of analysable dendrites is totally dependent on the resolution of microscope of EPMA

and beam size of filament used for quantitative analysis.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 11938, Microbeam analysis — Electron probe microanalysis — Methods for elemental-mapping

analysis using wavelength-dispersive spectroscopy

ISO 14594, Microbeam analysis — Electron probe microanalysis — Guidelines for the determination of

experimental parameters for wavelength dispersive spectroscopy

ISO 14595, Microbeam analysis — Electron probe microanalysis — Guidelines for the specification of

certified reference materials (CRMs)

ISO 22489, Microbeam analysis — Electron probe microanalysis — Quantitative point analysis for bulk

specimens using wavelength dispersive X-ray spectroscopy
ISO 23833, Microbeam analysis — Electron probe microanalysis (EPMA) — Vocabulary
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 23833 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at www .iso .org/ obp
— IEC Electropedia: available at www .electropedia .org
3.1
dendritic segregation

phenomenon that element content differs in the first-crystallized dendrite arms and post-crystallized

inter-dendritic spaces during alloy solidification in a dendritic pattern
3.2
mapping analysis

method of analysing element in EPMA, through which element distribution in an area can be obtained

© ISO 2021 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/FDIS 23692:2021(E)
3.3
line analysis

method of analysing element in EPMA, through which element distribution in a specified direction can

be obtained
3.4
ratio of dendritic segregation (SR)

ratio of the maximum content in the inter-dendritic spaces and the minimum content in the dendrite

arms of
...

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