ISO 5803:2023

Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for determination of monoclinic phase in zirconia

This document specifies a method for the qualitative and quantitative determination of the monoclinic phase present in yttria tetragonal zirconia polycrystal (Y-TZP) powders with an yttria content ≤ 6 mol% using X-ray powder diffraction. This method is also applicable for determining the monoclinic phase content in monolithic Y-TZP ceramics with an yttria content of ≤ 6 mol%. NOTE For quantitative determination of the monoclinic phase present in zirconia with a higher content of yttria or another stabilizer (e.g. MgO, CaO), this document can be referenced.

Titre manque

General Information

• Status: Published
• Publication Date: 30-Jan-2023
• ICS: 81.060.30 - Advanced ceramics
• Technical Committee: ISO/TC 206 - Fine ceramics
• Drafting Committee: ISO/TC 206 - Fine ceramics
• Current Stage: 6060 - International Standard published
• Start Date: 31-Jan-2023
• Due Date: 08-Jan-2024
• Completion Date: 31-Jan-2023

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 5803
First edition
2023-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Test method for determination of
monoclinic phase in zirconia
Reference number
ISO 5803:2023(E)
© ISO 2023

---------------------- Page: 1 ----------------------
ISO 5803:2023(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii
  © ISO 2023 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 5803:2023(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Sample preparation .2
7 Test procedure .2
7.1 Qualitative analysis . 2
7.2 Quantitative analysis . 3
8 Qualitative and quantitative analysis . 3
8.1 Qualitative analysis . 3
8.2 Quantitative analysis . 3
8.3 Limitations of the quantitative analysis . 4
9 Test report . 4
Annex A (informative) Recommended P values in different systems . 5
Bibliography . 7
iii
© ISO 2023 – All rights reserved

---------------------- Page: 3 ----------------------
ISO 5803:2023(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 206, Fine ceramics.
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 2023 – All rights reserved

---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 5803:2023(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Test method for determination of monoclinic
phase in zirconia
1 Scope
This document specifies a method for the qualitative and quantitative determination of the monoclinic
phase present in yttria tetragonal zirconia polycrystal (Y-TZP) powders with an yttria content ≤ 6 mol%
using X-ray powder diffraction. This method is also applicable for determining the monoclinic phase
content in monolithic Y-TZP ceramics with an yttria content of ≤ 6 mol%.
NOTE For quantitative determination of the monoclinic phase present in zirconia with a higher content of
yttria or another stabilizer (e.g. MgO, CaO), this document can be referenced.
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/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 20203, Carbonaceous materials used in the production of aluminium — Calcined coke — Determination
of crystallite size of calcined petroleum coke by X-ray diffraction
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The qualitative and quantitative determination of the monoclinic phase in Y-TZP powders or Y-TZP
ceramics is derived from the X-ray diffraction analysis of a representative sample of this powder or
ceramic.
The qualitative analysis is based on a comparison of the recorded spectrum with available reference
data (ICDD PDF database).
[1–4]
The quantitative analysis is based on the polymorph method. The polymorph method provides
phase analysis from a small number of integrated intensities in an X-ray diffraction scan. It is adapted
[2,5–7]
for the determination of the monoclinic phase in zirconia powders or zirconia ceramics. For
a full analysis, including the quantitative determination of all the phases, the full pattern method as
[1]
mentioned in EVN 14273:2002 or the Rietveld method are recommended.
1
© ISO 2023 – All rights reserved

---------------------- Page: 5 ----------------------
ISO 5803:2023(E)
5 Apparatus
The usual laboratory apparatus and, in particular, the following shall be used:
5.1 X-ray diffractometer, equipped with a copper X-ray tube, a monochromator or filter for
restricting the wavelength range, a sample holder, a radiation detector, a signal processor and readout.
The following experimental settings are recommended:
— precise goniometer (2θ error ≤ 0,5°);
— primary soller slit with a divergence ≤ 2,5°;
— divergence slit ≤ 1°;
— receiving slit ≤ 2 mm;
— scatter slit ≤ 1°;
— continuous scanning rate at ≤ 2°/min or step scanning at ≤ 0,05°/step.
5.2 Sample h
...

ISO/PRF 5803:2022(E)
2022-10-01
ISO/TC 206/WG 2
Secretariat: JISC
Date: 2022-12-13
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Test method for determination of monoclinic phase
in zirconia
FDIS stage
© ISO 2022 – All rights reserved

---------------------- Page: 1 ----------------------
ISO/PRF 5803:2022(E)
© ISO 2022
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
EmailE-mail: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2022 – All rights reserved

---------------------- Page: 2 ----------------------
ISO/PRF 5803:2022(E)
Contents
Foreword . iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 1
6 Sample preparation . 2
7 Test procedure . 2
7.1 Qualitative analysis . 2
7.2 Quantitative analysis . 2
8 Qualitative and quantitative analysis . 3
8.1 Qualitative analysis . 3
8.2 Quantitative analysis . 3
8.3 Limitations of the quantitative analysis . 4
9 Test report . 4
Annex A (informative) Recommended P values in different systems . 5
Bibliography . 7

© ISO 2022 – All rights reserved iii

---------------------- Page: 3 ----------------------
ISO/PRF 5803:2022(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).
Field Code Changed
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.
Field Code Changed
This document was prepared by Technical Committee ISO/TC 206, Fine Ceramicsceramics.
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.
Field Code Changed
iv © ISO 2022 – All rights reserved

---------------------- Page: 4 ----------------------
ISO/PRF 5803:2022(E)
Fine ceramics (advanced ceramics, advanced technical ceramics)
— — Test method for determination of monoclinic phase in
zirconia
1 Scope
This document specifies a method for the qualitative and quantitative determination of the monoclinic
phase present in yttria tetragonal zirconia polycrystal (Y-TZP) powders with an yttria content ≤ ≤ 6 mol%
using X-ray powder diffraction. This method is also applicable to determinefor determining the
monoclinic phase content in monolithic Y-TZP ceramics with an yttria content of ≤ ≤ 6 mol%.
NOTE For quantitative determination of the monoclinic phase present in zirconia with a higher content of
yttria or otheranother stabilizer (e.g. MgO, CaO, etc.),), this document can be referenced.
2 Normative references
The following document isdocuments 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/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 20203, Carbonaceous materials used in the production of aluminium — Calcined coke — Determination
of crystallite size of calcined petroleum coke by X-ray diffraction
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— — ISO Online browsing platform: available at https://www.iso.org/obp
— — IEC Electropedia: available at https://www.electropedia.org/
4 Principle
The qualitative and quantitative determination of the monoclinic phase in Y-TZP powder or Y-TZP
ceramics is derived from the X-ray diffraction analysis of a representative sample of this powder or
ceramic.
The qualitative analysis is based on a comparison of the recorded spectrum with available reference data
(ICDD PDF data bank).
[1–4[1-4] ]
The quantitative analysis is based on the polymorph method. . The polymorph method provides
phase analysis from a small number of integrated intensities in an X-ray diffraction scan. It is adapted for
[2,5–7[2,5-7] ]
the determination of the monoclinic phase in zirconia powders or zirconia ceramics. . For a full
analysis, including the quantitative determination of all the phases, the full pattern method as mentioned
[1[1]]
in EVN 14273:2002 or the Rietveld method isare recommended.
5 Apparatus
The usual laboratory apparatus and, in particular, the following shall be used:
5.1 5.1X-ray diffractometer
The X-ray diffractometer shall be, equipped with a copper X-ray tube, a monochromator or filter for
restricting the wavelength range, a sample holder, a radiation detector, a signal processor and readout.
The following experimental settings are recommended:
© ISO 2022 – All rights reserved 1

---------------------- Page: 5 ----------------------
ISO/PRF 5803:2022(E)
— — precise goniometer (2θ error ≤ ≤ 0,5º);5°);
— — primary soller slit with a divergence ≤ ≤ 2,5º;5°;
— — divergence slit ≤1º; ≤ 1°;
— — receiving slit ≤ ≤ 2 mm;
— — scatter slit ≤1º; ≤ 1°;
— — continuous scanning rate at ≤2º/ ≤ 2°/min or step scanning at ≤ ≤ 0,05º/05°/step.
5.2 5.2Sample holder
The, the dimensions of the sample holderwhich shall be such that X-ray irradiation outside of the sample
volume can be avoided. The sample holders enable packing of a pulverized sample of sufficient height to
expose a level, smooth surface to the X-ray beam.
6 Sample preparation
The powder to be analysed shall have a homogeneous grain size, in order to avoid primary extinction and
assureensure good statistics. The recommended grain size is less than 40 μm. The packing techniques for
the X-ray diffraction specimen holder shall be according toin accordance with ISO 20203. A
representative test sample of this powder is filled and pressed into the cavity of the sample holder. Use
the backfill pressing technique to obtain a flat and smooth sample surface and to reduce pr
...

INTERNATIONAL ISO
STANDARD 5803
First edition
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Test method for determination of
monoclinic phase in zirconia
PROOF/ÉPREUVE
Reference number
ISO 5803:2022(E)
© ISO 2022

---------------------- Page: 1 ----------------------
ISO 5803:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii
PROOF/ÉPREUVE © ISO 2022 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 5803:2022(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Sample preparation .2
7 Test procedure .2
7.1 Qualitative analysis . 2
7.2 Quantitative analysis . 3
8 Qualitative and quantitative analysis . 3
8.1 Qualitative analysis . 3
8.2 Quantitative analysis . 3
8.3 Limitations of the quantitative analysis . 4
9 Test report . 4
Annex A (informative) Recommended P values in different systems . 5
Bibliography . 7
iii
© ISO 2022 – All rights reserved PROOF/ÉPREUVE

---------------------- Page: 3 ----------------------
ISO 5803:2022(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 206, Fine ceramics.
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
PROOF/ÉPREUVE © ISO 2022 – All rights reserved

---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 5803:2022(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Test method for determination of monoclinic
phase in zirconia
1 Scope
This document specifies a method for the qualitative and quantitative determination of the monoclinic
phase present in yttria tetragonal zirconia polycrystal (Y-TZP) powders with an yttria content ≤ 6 mol%
using X-ray powder diffraction. This method is also applicable for determining the monoclinic phase
content in monolithic Y-TZP ceramics with an yttria content of ≤ 6 mol%.
NOTE For quantitative determination of the monoclinic phase present in zirconia with a higher content of
yttria or another stabilizer (e.g. MgO, CaO), this document can be referenced.
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/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 20203, Carbonaceous materials used in the production of aluminium — Calcined coke — Determination
of crystallite size of calcined petroleum coke by X-ray diffraction
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The qualitative and quantitative determination of the monoclinic phase in Y-TZP powder or Y-TZP
ceramics is derived from the X-ray diffraction analysis of a representative sample of this powder or
ceramic.
The qualitative analysis is based on a comparison of the recorded spectrum with available reference
data (ICDD PDF data bank).
[1–4]
The quantitative analysis is based on the polymorph method. The polymorph method provides
phase analysis from a small number of integrated intensities in an X-ray diffraction scan. It is adapted
[2,5–7]
for the determination of the monoclinic phase in zirconia powders or zirconia ceramics. For
a full analysis, including the quantitative determination of all the phases, the full pattern method as
[1]
mentioned in EVN 14273:2002 or the Rietveld method are recommended.
1
© ISO 2022 – All rights reserved PROOF/ÉPREUVE

---------------------- Page: 5 ----------------------
ISO 5803:2022(E)
5 Apparatus
The usual laboratory apparatus and, in particular, the following shall be used:
5.1 X-ray diffractometer, equipped with a copper X-ray tube, a monochromator or filter for
restricting the wavelength range, a sample holder, a radiation detector, a signal processor and readout.
The following experimental settings are recommended:
— precise goniometer (2θ error ≤ 0,5°);
— primary soller slit with a divergence ≤ 2,5°;
— divergence slit ≤ 1°;
— receiving slit ≤ 2 mm;
— scatter slit ≤ 1°;
— continuous scanning rate at ≤ 2°/min or step scanning at ≤ 0,05°/step.
5.2 Sample holder, the dimen
...