SIST EN ISO 13356:2015
(Main)Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
This International Standard specifies the requirements and corresponding test methods for a
biocompatible and biostable ceramic bone-substitute material based on yttria-stabilized tetragonal
zirconia (yttria tetragonal zirconia polycrystal, Y-TZP) for use as a material for surgical implants.
Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem Zirkon (Y-TZP) (ISO 13356:2015)
Diese Internationale Norm legt die Anforderungen und die dazugehörigen Prüfverfahren für ein biokompatibles und biostabiles keramisches Knochenersatzmaterial auf der Grundlage von yttriumstabi-lisiertem tetragonalem Zirkon (mit Yttrium polykristallines, tetragonales Zirkoniumdioxid, Y-TZP) fest, das für chirurgische Implantate verwendet wird.
Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisée à l'yttrium (Y-TZP) (ISO 13356:2015)
L'ISO 13356:2015 spécifie les exigences et les méthodes d'essai correspondantes applicables aux matériaux de substitution osseuse, biocompatibles et biostables, à base de zircone tétragonale stabilisée à l'oxyde d'yttrium (polycristaux de zircone tétragonale stabilisée à l'yttrium, Y-TZP), utilisés en tant que matériaux constitutifs d'implants chirurgicaux.
Vsadki (implantati) za kirurgijo - Keramični materiali na osnovi tetragonalnega cirkonija, stabiliziranega z itrijem (Y-TZP) (ISO 13356:2015)
Ta mednarodni standard določa zahteve biozdružljivega in biostabilnega keramičnega materiala za kostne nadomestke na osnovi tetragonalnega cirkonija, stabiliziranega z itrijem, (z itrijem stabilizirani polikristal tetragonalnega cirkonija, Y-TZP) za uporabo kot material za kirurške vsadke ter ustrezne preskusne metode zanj.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 13356:2015
01-december-2015
1DGRPHãþD
SIST EN ISO 13356:2013
9VDGNL LPSODQWDWL ]DNLUXUJLMR.HUDPLþQLPDWHULDOLQDRVQRYLWHWUDJRQDOQHJD
FLUNRQLMDVWDELOL]LUDQHJD]LWULMHP <7=3 ,62
Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-
TZP) (ISO 13356:2015)
Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem
Zirkon (Y-TZP) (ISO 13356:2015)
Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisée à
l'yttrium (Y-TZP) (ISO 13356:2015)
Ta slovenski standard je istoveten z: EN ISO 13356:2015
ICS:
11.040.40 Implantanti za kirurgijo, Implants for surgery,
protetiko in ortetiko prosthetics and orthotics
SIST EN ISO 13356:2015 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 13356:2015
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SIST EN ISO 13356:2015
EN ISO 13356
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2015
EUROPÄISCHE NORM
ICS 11.040.40 Supersedes EN ISO 13356:2013
English Version
Implants for surgery - Ceramic materials based on yttria-
stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
Implants chirurgicaux - Produits céramiques à base de Chirurgische Implantate - Keramische Werkstoffe aus
zircone tétragonal stabilisée à l'yttrium (Y-TZP) (ISO yttriumstabilisiertem tetragonalem Zirkonium (Y-TZP)
13356:2015) (ISO 13356:2015)
This European Standard was approved by CEN on 22 August 2015.
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, 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: Avenue Marnix 17, B-1000 Brussels
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13356:2015 E
worldwide for CEN national Members.
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SIST EN ISO 13356:2015
EN ISO 13356:2015 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 13356:2015
EN ISO 13356:2015 (E)
European foreword
This document (EN ISO 13356:2015) has been prepared by Technical Committee
ISO/TC 106 “Dentistry” in collaboration with Technical Committee CEN/TC 55 “Dentistry” the
secretariat of which is held by DIN.
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 March 2016, and conflicting national standards shall
be withdrawn at the latest by March 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document supersedes EN ISO 13356:2013.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 13356:2015 has been approved by CEN as EN ISO 13356:2015 without any modification.
3
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SIST EN ISO 13356:2015
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SIST EN ISO 13356:2015
INTERNATIONAL ISO
STANDARD 13356
Third edition
2015-09-15
Implants for surgery — Ceramic
materials based on yttria-stabilized
tetragonal zirconia (Y-TZP)
Implants chirurgicaux — Produits céramiques à base de zircone
tétragonal stabilisée à l’yttrium (Y-TZP)
Reference number
ISO 13356:2015(E)
©
ISO 2015
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, 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
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Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Physical and chemical properties . 2
3.1 Test category . 2
3.1.1 General. 2
3.1.2 Category 1 . 2
3.1.3 Category 2 . 2
4 Test methods . 4
4.1 General . 4
4.2 Bulk density . 4
4.3 Chemical composition . 4
4.4 Microstructure . 4
4.4.1 Principle . 4
4.4.2 Test report . 5
4.4.3 Amount of monoclinic phase . 5
4.5 Biaxial flexural strength . 6
4.5.1 Principle . 6
4.5.2 Apparatus . 6
4.5.3 Preparation of test specimens . 6
4.5.4 Procedure . 7
4.5.5 Calculation of results . 8
4.5.6 Test report . 8
4.6 Four-point bending strength . 8
4.7 Weibull modulus . 9
4.8 Young’s modulus . 9
4.9 Hardness . 9
4.10 Cyclic fatigue . 9
4.10.1 Principle . 9
4.10.2 Apparatus . 9
4.10.3 Sample size and preparation of test specimens . 9
4.10.4 Procedure and sample requirement . 9
4.10.5 Test Report .10
4.11 Radioactivity .10
4.11.1 Principle .10
4.11.2 Apparatus .10
4.11.3 Sample preparation .11
4.11.4 Isotope identification - Energy calibration .11
4.11.5 Quantitative analysis .11
4.11.6 Expression of results .12
4.11.7 Test report .12
4.12 Accelerated aging test .12
4.12.1 General.12
4.12.2 Procedure .12
4.12.3 Evaluation of accelerated aging outcome .12
Bibliography .13
© ISO 2015 – All rights reserved iii
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SIST EN ISO 13356:2015
ISO 13356:2015(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 on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary Information
The committee responsible for this document is ISO/TC 150, Implants for surgery, Subcommittee
SC 1, Materials.
This third edition cancels and replaces the second edition (ISO 13356:2008), which has been
technically revised.
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
Introduction
No known surgical implant material has ever been found to cause absolutely no adverse reactions in
the human body. However, long-term clinical experience regarding the use of the material referred to in
this International Standard has shown that an acceptable level of biological response can be expected if
the material will be used in appropriate applications.
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SIST EN ISO 13356:2015
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SIST EN ISO 13356:2015
INTERNATIONAL STANDARD ISO 13356:2015(E)
Implants for surgery — Ceramic materials based on yttria-
stabilized tetragonal zirconia (Y-TZP)
1 Scope
This International Standard specifies the requirements and corresponding test methods for a
biocompatible and biostable ceramic bone-substitute material based on yttria-stabilized tetragonal
zirconia (yttria tetragonal zirconia polycrystal, Y-TZP) for use as a material for surgical implants.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
ISO 3611, Geometrical product specifications (GPS) — Dimensional measuring equipment: Micrometers for
external measurements — Design and metrological characteristics
ISO 7500-1, Metallic materials — Verification of static uniaxial testing machines — Part 1:
Tension/compression testing machines — Verification and calibration of the force-measuring system
ISO 13383-1, Fine ceramics (advanced ceramics, advanced technical ceramics) — Microstructural
characterization — Part 1: Determination of grain size and size distribution
ISO 14704, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for flexural
strength of monolithic ceramics at room temperature
ISO 14705, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for hardness of
monolithic ceramics at room temperature
ISO 17561, Fine ceramics (advanced ceramics, advanced technical ceramics) - Test method for elastic moduli
of monolithic ceramics at room temperature by sonic resonance
ISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) — Determination of density
and apparent porosity
ISO 20501, Fine ceramics (advanced ceramics, advanced technical ceramics) — Weibull statistics for
strength data
ISO 22214, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for cyclic
bending fatigue of monolithic ceramics at room temperature
EN 623-2, Advanced technical ceramics — Monolithic ceramics — General and textural properties —
Part 2: Determination of density and porosity
EN 843-2, Advanced technical ceramics — Mechanical properties of monolithic ceramics at room
temperature — Part 2: Determination of Young’s modulus, shear modulus and Poisson’s ratio
EN 843-4, Advanced technical ceramics — Mechanical properties of monolithic ceramics at room
temperature — Part 4: Vickers, Knoop and Rockwell superficial hardness
EN 843-5, Advanced technical ceramics — Mechanical properties of monolithic ceramics at room
temperature — Part 5: Statistical analysis
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
ASTM C1161, Standard Test Method for Flexural Strength of Advanced Ceramics at Ambient Temperature
ASTM C1198, Standard Test Method for Dynamic Young’s Modulus, Shear Modulus, and Poisson’s Ratio for
Advanced Ceramics by Sonic Resonance
ASTM C1239, Standard Practice for Reporting Uniaxial Strength Data and Estimating Weibull Distribution
Parameters for Advanced Ceramics
ASTM C1259, Standard Test method for Dynamic Young’s Modulus. Shear Modulus, and Poisson’s Ratio for
Advanced Ceramics by Impulse Excitation of Vibration
ASTM C1327, Standard Test Method for Vickers Indentation Hardness of Advanced Ceramics
ASTM C1331, Standard Test Method for Measuring Ultrasonic Velocity in Advanced Ceramics with
Broadband Pulse-Echo Cross-Correlation Method
ASTM E112, Standard Test Method for Determining Average Grain Size
3 Physical and chemical properties
The physical and chemical properties, when tested as specified in Clause 4, shall comply with the values
specified in Table 1.
3.1 Test category
3.1.1 General
The required tests are divided into two categories.
3.1.2 Category 1
The following test shall be performed for periodical production control:
a) bulk density;
b) chemical composition;
c) microstructure;
d) strength (including Weibull modulus);
e) accelerated aging (monoclinic fraction).
3.1.3 Category 2
The manufacturer shall define the general materials specification. In addition to all tests in 3.1.2, the
following tests shall be performed to demonstrate compliance with the material specification:
a) hardness;
b) Young’s modulus;
c) fatigue strength;
d) accelerated aging (strength);
e) quantity of monoclinic phase;
f) radioactivity.
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
Table 1 — Limits for material properties
Test
Property Unit Requirement Reference Subclause
category
ISO 18754
3
Bulk density g/cm 1 ≥ 6,00 4.2
EN 623–2
Chemical composition 4.3
a
ZrO +HfO +Y O ≥ 99,0
2 2 2 3
Y O > 4,5 to ≤ 6,0
2 3
% mass
HfO 1 ≤ 5
2
fraction
Al O ≤ 0,5
2 3
Other oxides ≤ 0,5
Microstructure 4.4
Intercept distance ≤ 0,4
ISO 13383-1
Grain size μm 1
ASTM E112
Standard deviation < 0,2
% molar
Amount of monoclinic phase 2 ≤ 20 See 4.4.3
fraction
Strength: alternative of 1)
or 2)
a
1a) Biaxial flexure 1 ≥ 500 ASTM C1499 4.5
ISO 20501
1b) Weibull modulus 1 ≥ 8 EN 843–5 4.7
ASTM C1239
ISO 14704
MPa
a
2a) 4-point bending 1 ≥ 800 EN 843–1 4.6
ASTM C1161
ISO 20501
2b) Weibull modulus 1 ≥ 8 EN 843–5 4.7
ASTM C 1239
ISO 17561
EN 843–2
ASTM C1198
Young’s modulus GPa 2 ≥ 200 4.8
ASTM C1259
ASTM C1331
ISO 14705
Hardness GPa 2 ≥ 11,8 EN 843–4 4.9
ASTM C1327
Cyclic fatigue limit stress
MPa 2 ≥ 320 ISO 22214 4.10
6
at 10 cycles
b
Radioactivity Bq/kg 2 ≤ 200 — 4.11
Accelerated aging 4.12
NOTE The number of fractional digits given for each limit value in this table indicates the appropriate number of fractional
digits which should be given for the respective measured values.
a
Measured on a minimum of 10 test specimens.
b 238 226 232
The radioactivity, defined as the sum of the mass activity of U , Ra , Th , and determined by gamma
spectroscopy on the ready-to-use powder should be equal or less than 200 Bq/kg. This value will be reviewed at the next
revision of this International Standard and will be based upon the radioactivity data from implant ceramic manufacturers.
All naturally occurring gamma emitters are to be analysed.
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
Table 1 (continued)
Test
Property Unit Requirement Reference Subclause
category
Maximum amount of mon-
% molar
oclinic phase after acceler- 1 ≤ 25 See 4.4.3
fraction
ated aging
Residual biaxial flexure
≥ 500, and decrease not
strength after accelerated 2 See 4.5
more than 20 %
aging
MPa
Residual 4-point bending
≥ 800, and decrease not
strength after accelerated 2 See 4.6
more than 20 %
aging
NOTE The number of fractional digits given for each limit value in this table indicates the appropriate number of fractional
digits which should be given for the respective measured values.
a
Measured on a minimum of 10 test specimens.
b 238 226 232
The radioactivity, defined as the sum of the mass activity of U , Ra , Th , and determined by gamma
spectroscopy on the ready-to-use powder should be equal or less than 200 Bq/kg. This value will be reviewed at the next
revision of this International Standard and will be based upon the radioactivity data from implant ceramic manufacturers.
All naturally occurring gamma emitters are to be analysed.
4 Test methods
4.1 General
All test specimens shall be prepared using the same production methods as regular implant components,
including, but not limited to: the precursor powder; pressing technique; pressure; and firing conditions,
unless justified by the manufacturer.
Where the requirements for the test report are not explicitly specified in this standard, the test report
for a given property shall be written according to the referenced standard described in the subclause of
this property and shall include a reference to this International Standard, i.e. ISO 13356:2015.
4.2 Bulk density
The bulk density shall be determined and reported in accordance with ISO 18754 or EN 623-2.
4.3 Chemical composition
The chemical compositions shall be determined by ICP-OES (Inductively Coupled Plasma – Optical
[1]
Emission Spectrometry), X-ray fluorescence, or atomic absorption spectrum analysis methods.
4.4 Microstructure
4.4.1 Principle
To describe the microstructure, the average grain size is determined by measuring the linear intercept
size in accordance with ISO 13383-1 or ASTM E112.
Five test specimens shall be used for the determination of microstructure.
NOTE The linear intercept method results in a nominal average grain size for the selected position of
micrograph, not the distribution of the size of individual grains.
For selection, preparation, and evaluation of the specimens, the following guidelines shall be followed:
a) the use of final device components as specimens for microstructure evaluation is recommended;
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SIST EN ISO 13356:2015
ISO 13356:2015(E)
b) the wall thickness of the specimens shall represent the maximum and minimum of the
manufacturer’s device components;
c) Four micrographs on each surface shall be taken; the positions of which shall include regions in the
bulk as well as at the edges of the specimen;
d) the specimen selection shall reflect the possibility of temperature deviation in the furnace;
e) the requirement for mean linear intercept grain size given in Table 1 shall be met at each selected
position of the micrographs;
f) the standard deviation of the mean linear intercept grain size shall be determined from the data of
all selected micrographs; the standard deviation shall meet the requirement given in Table 1.
The determination of mean linear intercept grain size shall be organized such that consistency of
regular production can be assessed to a sufficient statistical relevance. The manufacturer shall
justify the procedure implemented for grain size determination for its specific manufacturing
process. It is recommended that the manufacturer analyse the reliability, repeatability, and
maintenance of the manufacturing process with respect to microstructure (e.g. validation) and
utilize this information to implement the regular routine production control. If this detailed analysis
is successfully completed, regular control of the microstructure can be controlled with a reduced
number of specimens and micrographs.
For improved contrast and grain boundary detection, it is recommended to use a scanning electron
microscope (SEM) at a high acceleration voltage in conjunction with secondary electron detection
capabilities.
4.4.2 Test report
The test report shall be prepared in accordance with ISO 13383-1 or ASTM E112 whichever is applicable.
The test report shall contain at least the following information:
a) identity of the ceramic material, details of batch number or other codes sufficient to identify the
test specimens uniquely;
b) method of preparation of the test specimens, including details of the grinding and polishing
procedure employed to prepare the test surfaces, as well as the etching procedure;
c) mean linear intercept size and its standard deviation shall be expressed in micrometres;
d) at least one micrograph from the specimen taken to show the microstructure after the thermal
etch;
...
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