《ISO-13356-2008.pdf》由会员分享，可在线阅读，更多相关《ISO-13356-2008.pdf（20页珍藏版）》请在三一文库上搜索。
1、 Reference number ISO 13356:2008(E) ISO 2008 INTERNATIONAL STANDARD ISO 13356 Second edition 2008-06-01 Implants for surgery Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) Implants chirurgicaux Produits cramiques base de zircone ttragonal stabilis loxyde dyttrium (Y-TZP) Co
2、pyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) PDF disclaimer This PDF file may contain embedde
3、d typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not
4、 infringing Adobes licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters wer
5、e optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reser
6、ved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the request
7、er. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Lic
8、ensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) ISO 2008 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope 1 2 Normative references1 3 Physical and chemical properties2 4
9、 Test methods3 4.1 Bulk density3 4.2 Chemical composition 3 4.3 Microstructure3 4.4 Biaxial flexural strength6 4.5 Four-point bending strength 9 4.6 Cyclic fatigue9 4.7 Radioactivity.10 4.8 Accelerated Aging Test.12 Bibliography13 Copyright International Organization for Standardization Provided by
10、IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide fe
11、deration 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 com
12、mittee. 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. International Standards are drafted in accord
13、ance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard require
14、s approval by at least 75 % of the member bodies casting a vote. 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. ISO 13356 was prepared by Technical
15、Committee ISO/TC 150, Implants for surgery, Subcommittee SC 1, Materials. This second edition cancels and replaces the first edition (ISO 13356:1997) which has been technically revised. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co
16、/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) ISO 2008 All rights reserved v Introduction No known surgical implant material has ever been shown to cause absolutely no adverse reactions in the human body. H
17、owever, long-term clinical experience of the use of the material referred to in this International Standard has shown that an acceptable level of biological response can be expected when the material is used in appropriate applications. Copyright International Organization for Standardization Provid
18、ed by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 N
19、ot for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 13356:2008(E) ISO 2008 All rights reserved 1 Implants for surgery Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) 1 Scope This Internationa
20、l Standard specifies the characteristics of, 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 material for surgical implants. 2 Normative refere
21、nces The following referenced documents are indispensable for the application 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 3611, Micrometer callipers for external
22、measurement ISO 7500-1:2004, Metallic materials Verification of static uniaxial testing machines Part 1: Tension/compression testing machines Verification and calibration of the force-measuring system ISO 14704, Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for flexural
23、strength of monolithic ceramics at room temperature ISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of density and apparent porosity EN 623-2, Advanced technical ceramics Monolithic ceramics General and textural properties Part 2: Determination of density and
24、porosity EN 623-3, Advanced technical ceramics Monolithic ceramics General and textural properties Part 3: Determination of grain size and size distribution (characterized by the Linear Intercept Method) ASTM C1499, Standard Test Method for Monotonic Equibiaxial Flexural Strength of Advanced Ceramic
25、s at Ambient Temperature ASTM E112-96, Standard Test Methods for Determining Average Grain Size ASTM G136-03, Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction ASTM F1873-98 1), Standard Specification for High-Purity Dense Yttria Tetragonal Zi
26、rconium Oxide Polycrystal (Y-TZP) for Surgical Implant Applications 1) Standard since withdrawn. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitte
27、d without license from IHS -,-,- ISO 13356:2008(E) 2 ISO 2008 All rights reserved 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. Table 1 Limits for material properties Property Unit Req
28、uirement Test method according to subclause Bulk density g/cm3 W 6,00 4.1 Chemical composition: ZrO2 + HfO2 + Y2O3 Y2O3 HfO2 Al2O3 Other oxides percent mass fraction W 99,0 4,5 to u 6,0 u 5 u 0,5 u 0,5 4.2 Microstructure: grain size m Intercept distance u 0,4 4.3 Microstructure: amount of monoclinic
29、 phase Standard deviation HV 500 or HRC 40) in order to minimize damage or roughness caused by fracture of the test pieces. In order to accommodate slight departures from surface flatness of the test pieces, a (0,6 0,1) mm thick rubber plate with a Shore hardness of 60 5 shall be placed between the
30、support ring and the test piece, and a piece of paper shall be placed between the test piece and the loading ring. 4.4.2.3 Micrometer, in accordance with ISO 3611, capable of measuring to an accuracy of 0,01 mm. Copyright International Organization for Standardization Provided by IHS under license w
31、ith ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) ISO 2008 All rights reserved 7 4.4.3 Preparation of test piece Prepare billets or discs of the zirconia ceramic using methods represen
32、tative of the method of production of parts for surgery, using the same precursor powder, pressing technique and pressure and firing conditions. Test pieces (see Figure 2) shall be circular plates of diameter (36,0 1,0) mm and thickness (2,0 0,1) mm and shall be flat on the test face to closer than
33、0,3 mm. The surface to be tested shall be in the as-fired state. At least 10 test pieces shall be prepared for determination of mean strength, or at least 30 test pieces if a Weibull statistical analysis is required. Key 1 loading ring 3 support ring 5 specimen 2 paper 4 rubber plate Figure 2 Schema
34、tic diagram of the biaxial flexure testing device employing concentric loading and support rings Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitte
35、d without license from IHS -,-,- ISO 13356:2008(E) 8 ISO 2008 All rights reserved 4.4.4 Procedure 4.4.4.1 Measure the diameter of the test piece to the nearest 0,1 mm and the thickness to the nearest 0,01 mm, each in at least three random positions. Calculate the mean diameter and mean thickness. 4.
36、4.4.2 Place the rubber sheet on the support ring of the test jig. Place the test piece on the rubber sheet, with the surface to be tested in contact with the rubber, and centre it. Place a paper disc on the top of the test piece, place the loading ring on the paper and centre it relative to the test
37、 piece and support ring. 4.4.4.3 Apply a steadily increasing compressive force, F, to the jig at a loading rate of (500 100) N/s until the test piece fractures. Record the load at fracture and its location. 4.4.4.4 Inspect the fragments for evidence of the failure origin. If this is more than 0,5 mm
38、 outside the inner loading ring, note this fact in the test report (see 4.4.6). For the purposes of calculation of the fracture stress, assume failure within the inner loading ring. Do not discard the result in calculating the mean strength of the test batch. 4.4.4.5 Repeat the procedure for each te
39、st piece in the batch. 4.4.5 Calculation of results For each test piece, calculate the nominal fracture stress, s, in megapascals, as: ()() 22 22 ss l 3 1ln1 22 l DDDF D tD =+ where F is the force applied at fracture, in newtons; t is the mean test piece thickness, in millimetres; Dl is the support
40、ring mean (contact) diameter in millimetres; Ds is the loading ring mean (contact) diameter, in millimetres; D is the test piece diameter, in millimetres; is Poissons ratio for zirconia (assume to be 0,3). Calculate the mean fracture stress and the standard deviation for the batch of test pieces. 4.
41、4.6 Test report The test report shall contain at least the following information. a) The identity of the ceramic material, details of batch number or other codes sufficient to uniquely identify the test pieces. b) Method of preparing the test pieces. c) Mean value and standard deviation of the fract
42、ure stresses. If appropriate, the individual fracture stresses of the series of test pieces as well as Weibull statistical data may be given. The position of failure of test pieces shall be reported if this appears to fall outside the loading ring diameter (see 4.4.4). d) Reference to this Internati
43、onal Standard, i.e. ISO 13356:2008. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 02:25:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13356:2008(E) ISO 2008 A
44、ll rights reserved 9 4.5 Four-point bending strength The four-point bending strength shall be determined in accordance with ISO 14704 using 4-point (20 40) mm spans. Calculate the individual nominal flexural strengths, the mean value and the standard deviation. The test pieces shall be 45 mm in leng
45、th (4,0 0,2) mm in width and (3,0 0,2) mm in thickness. The test piece is supported by two parallel rollers of diameter (5,0 0,2) mm. The two rollers shall be positioned symmetrically with respect to the length of the test piece with their centres (40 0,5) mm apart (outer span). The two loading roll
46、ers shall be symmetrically located with respect to the outer roller and shall have a span of (20 0,2) mm. The surface to be tested shall be in contact with the outer rollers. 4.6 Cyclic fatigue 4.6.1 Principle The cyclic fatigue shall be determined by a four-point bend cycling fatigue test under sim
47、ulated physiological conditions. 4.6.2 Apparatus 4.6.2.1 Mechanical testing machine, suitable for applying a cycling sinusoidal load. The testing machine shall be in accordance with ISO 7500-1:2004, Class 1 with an accuracy of 1 % of the maximum load or better. The machine shall have instrumentation to monitor the maximum and minimum loads, and to record the number of cycles or the elapsed time of the test. 4.6.2.2 Testing jig, in accordance with ISO 14704. The test piece is supported by two parallel rollers. Each roller shall be positioned symmetrically with respect to the length of