1、BRITISH STANDARD BS ISO 13779-4:2002 Implants for surgery Hydroxyapatite Part 4: Determination of coating adhesion strength ICS 11.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 13779-4:2002 This British Standard, having been prepared under the direction of the H
2、ealth and Environment Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 18 June 2002 BSI 18 June 2002 ISBN 0 580 39867 6 National foreword This British Standard reproduces verbatim ISO 13779-4:2002 and implements it as the UK na
3、tional standard. The UK participation in its preparation was entrusted to Technical Committee CH/150/1, Materials (for surgical implants), which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British
4、Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or British Standards Online. This publicati
5、on does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/E
6、uropean committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page
7、, pages ii to iv, pages 1 to 7, and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 13779-4:2002(E)INTERNATIONAL STANDARD ISO 13779-4 First edition 2002-05-01
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13、22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.c h Web ww.wiso.ch Prnietdi nS wztierland ii ISO 2002 Allr ithgsr ese devrISO 13779-4:2002(E) I SO 2002 All irthgs ersedevr iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (I
14、SO 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, gov
15、ernmental 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 accordance with the rules given in the ISO/IEC
16、 Directives, Part 3. 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 requires approval by at least 75 % of the membe
17、r bodies casting a vote. Attention is drawn to the possibility that some of the elements of this part of ISO 13779 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 13779-4 was prepared by Technical Commit
18、tee ISO/TC 150, Implants for surgery, Subcommittee SC 1, Materials. ISO 13779 consists of the following parts, under the general title Implants for surgery Hydroxyapatite: Part 1: Ceramic hydroxyapatite Part 2: Coatings of hydroxyapatite Part 3: Chemical analysis and characterization of cristallinit
19、y and phase purity Part 4: Determination of coating adhesion strength Future parts will deal with other relevant aspects of implant material based on hydroxyapatite. ISO 13779-4:2002(E) iv I SO 2002 All irthgs ersedevr Introduction No known surgical implant material has ever been shown to cause abso
20、lutely no adverse reactions in the human body. However, long-term clinical experience of the use of the material referred to in this part of ISO 13779 has shown that an acceptable level of biological response can be expected, if the material is used in appropriate applications. The biological respon
21、se to hydroxyapatite ceramic has been demonstrated by a history of clinical use and by laboratory studies. See the Bibliography for further information. INTERNATIONAL STANDARD ISO 13779-4:2002(E)I SO 2002 All irthgs ersedevr 1Implants for surgery Hydroxyapatite Part 4: Determination of coating adhes
22、ion strength 1 Scope This part of ISO 13779 specifies test methods for measurement of the adhesion strength of hydroxyapatite coatings intended for use on components of surgical implants. 2 Normative reference The following normative document contains provisions which, through reference in this text
23、, constitute provisions of this part of ISO 13779. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 13779 are encouraged to investigate the possibility of applying the most recent edition
24、 of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 7500-1:1999, Metallic materials Verification of static uniaxial testing mach
25、ines Part 1: Tension/compression testing machines Verification and calibration of the force-measuring system 3 Terms and definitions For the purposes of this part of ISO 13779, the following terms and definitions apply. 3.1 ceramic hydroxyapatite hydroxyapatite which has been sintered into a coheren
26、t crystalline mass by subjecting it to conditions at which the crystals in the powder fuse together ISO 13779-1 3.2 coating distinct layer of material deposited onto the surface of a metallic or non-metallic substrate by either a thermal, vapour or aqueous route 3.3 hydroxyapatite chemical compound
27、with a crystallographic structure characterized by the powder diffraction file PDF 9-432 of the International Committee for Diffraction Data ICDD, Newton Square, Pennsylvania, USA NOTE The chemical formula is Ca 5 (OH)(PO 4 ) 3 . ISO 13779-1 ISO 13779-4:2002(E) 2 I SO 2002 All irthgs ersedevr 3.4 si
28、ntering process for production of ceramics in which the application of heat causes a significant reduction of particle surface area and bulk volume to achieve densification and consequent increase in mechanical properties ISO 13779-1 4 Determination of hydroxyapatite coating adhesion strength 4.1 Pr
29、inciple Coating adhesion strength is determined by applying a uniaxial tensile load to a cylindrical test assembly composed of one hydroxyapatite-coated specimen bonded to an uncoated component. 4.2 Apparatus 4.2.1 Mechanical testing machine, of load capacity not less than 30 kN and accuracy 2 % of
30、full scale reading. The tensile load shall be applied normal to the plane of the coating. Verification and calibration of the force-measuring system shall be in accordance with ISO 7500-1. 4.2.2 Loading assembly, used to transmit the load from the testing machine to the test assembly. The loading as
31、sembly shall ensure that the axis of the test assembly does not deviate from that of the testing machine by more than 1 and 0,1 mm, in order that the coating test plane is perpendicular to the axial load. Eccentric loading of the test assembly shall invalidate the result. The yoke and dowel pin asse
32、mbly illustrated in Figure 1 is an example of a loading assembly which meets these requirements The coated specimen and uncoated component are each secured by two perpendicular pins which minimize off-axis loading. The dimensions of the loading assembly, as specified in Table 1, are suitable for the
33、 testing of coatings with a maximum predicted adhesion or cohesion strength of 50 MPa. Key 1 Test assembly 2 Pins 3 Yoke 4 Adhesive 5 Tested coating Figure 1 Illustration of loading assembly which minimizes off-axis loading ISO 13779-4:2002(E) I SO 2002 All irthgs ersedevr 3Table 1 Jig and specimen
34、dimensions for testing of coatings with adhesion/cohesion strengths of less than 50 MPa Dimensions mm Figure 2 symbol Test component/jig Ti6Al4V alloy 316 stainless steel Stepped test component 25 0,05 25 0,05 ts Test surface diameter Straight test component 0,02 0,041 25 0,02 0,041 25 a Sample hold
35、er step diameter 0,02 0,041 20 0,02 0,041 18 b Pin hole diameter 0,015 0 9 +0,015 0 8 +c Sample hole depth 14 0,1 12 0,1 d Pin diameter 0,005 0,041 9 0,005 0,041 8 e Pin length 55 0,1 50 0,1 Stepped test component 0,033 0 20 +0,033 0 18 +f Yoke internal width Straight test component 0,033 0 25 +0,03
36、3 0 25 +Stepped test component 40 0,1 35 0,1 g Yoke external diameter Straight test component 45 0,1 45 0,1 h Yoke hole depth 14 0,1 12 0,1 k Yoke internal depth 40 0,1 40 0,1 4.2.3 Test assembly. The parts of the test assembly (coated specimen and uncoated component) are bonded together by the use
37、of a polymeric adhesive. The uncoated component shall be fabricated from the same material as the substrate of the coated specimen. Recommended materials are listed in Table 1. The dimensions of the uncoated component shall be the same as those of the coated specimen, with dimensions and tolerances
38、as in Table 1. Loading and test components are illustrated in Figure 2. The dimensions of the components specified are suitable for the testing of coatings with a maximum predicted adhesion or cohesion strength of 50 MPa. NOTE 1 The accuracy of this test method is highly sensitive to preparation of
39、the coated specimen, application of the polymeric adhesive and proper alignment of the coated specimen and uncoated component. Improper alignment will result in eccentric loading and the application of bending stresses on the assembly, leading to an invalid result. NOTE 2 The bond surface of the unc
40、oated component may be roughened in order to aid bonding with the polymeric adhesive. 4.2.4 Polymeric adhesive, having a minimum adhesive bond strength at least 5 MPa greater than either the adhesion or cohesion strength of the coating, or 30 MPa, whichever is greater. The polymeric adhesive used sh
41、all be identified in any test report. Where porosity extends to the coating/substrate interface, it shall be ensured that, by careful application to the coating and selection of a sufficiently viscous polymeric adhesive, the polymeric adhesive will not penetrate through the coating to the substrate.
42、 Penetration of the adhesive through the coating shall invalidate the result. The penetration of the adhesive shall be assessed by examining cross-sections of a trial test piece. ISO 13779-4:2002(E) 4 I SO 2002 All irthgs ersedevr 4.3 Preparation of coated specimen Exercise care in the preparation o
43、f the coated specimen. Inspect all specimens prior to both assembly and testing. Reject any found to be non-representative of the particular coating under test. Test specimens shall not be machined after the hydroxyapatite coating has been applied. The area of coating to be tested shall be nominally
44、 circular with a diameter of 25 mm and tolerances as in Table 1, or shall possess an equivalent cross-sectional area. Measure and record the cross-sectional area and the coated specimen dimensions. If specimens of other dimensions or cross-sectional area are used, the data shall be demonstrated to b
45、e equivalent to that obtained for a nominally circular specimen with a diameter of 25 mm. a) Yoke b) Pin c) Stepped test component d) Straight test component Key 1 Hydroxyapatite coating surface (when applicable) See Table 1 for meaning of symbols and dimensions. Figure 2 Dimensions of loading and t
46、est components ISO 13779-4:2002(E) I SO 2002 All irthgs ersedevr 54.4 Application of polymeric adhesive and alignment of test assembly Apply the polymeric adhesive, in a single action, to the axial centre of the coating. Regulate the amount of adhesive applied and the force used to bring the parts t
47、ogether so as to ensure that excess adhesive does not form a collar around the coated specimen/uncoated component joint. Remove any excess adhesive after curing has occurred, in a manner which does not compromise the integrity of the test assembly. Bring the uncoated component into contact with the
48、adhesive/coated specimen so as to ensure a plane parallel, uniform thickness of adhesive over the cross-sectional area to be tested. In order to ensure uniaxial alignment of the test assembly, use a device to rigidly hold the parts of the assembly in position during the curing of the polymeric adhes
49、ive. This device shall enable a constant axial tension (typically, 0,2 MPa) to be applied to the assembly during curing, in order to compensate for any shrinkage of the adhesive. 4.5 Test procedure Place the test assembly in the grips of the tensile testing machine, so that the long axis of the test assembly coincides with the direction of applied tensile loading. Apply the tensile load at a constant cross-head velocity of (1,0 0,01) mm/min until
