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.

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General Information

Status
Published
Publication Date
30-Jan-2023
Technical Committee
Drafting Committee
Current Stage
6060 - International Standard published
Start Date
31-Jan-2023
Due Date
08-Jan-2024
Completion Date
31-Jan-2023
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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 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
ii
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
Foreword
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described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
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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
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.
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
...

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