1、Designation: F1160 05 (Reapproved 2011)1Standard Test Method forShear and Bending Fatigue Testing of Calcium Phosphateand Metallic Medical and Composite Calcium Phosphate/Metallic Coatings1This standard is issued under the fixed designation F1160; the number immediately following the designation ind
2、icates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEUnits information was editorially corrected in J
3、anuary 2012.1. Scope1.1 This test method covers the procedure for determiningthe shear and bending fatigue performance of calcium phos-phate coatings and of porous and nonporous metallic coatingsand for determining the bending fatigue performance ofmetallic coatings oversprayed with calcium phosphat
4、e. Thistest method has been established based on plasma-sprayedtitanium and plasma-sprayed hydroxylapatite coatings. Theefficacy of this test method for other coatings has not beenestablished. In the shear fatigue mode, this test methodevaluates the adhesive and cohesive properties of the coatingon
5、a metallic substrate. In the bending fatigue mode, this testmethod evaluates both the adhesion of the coating as well asthe effects that the coating may have on the substrate material.These methods are limited to testing in air at ambient tempera-ture. These test methods are not intended for applica
6、tion infatigue tests of components or devices; however, the testmethod which most closely replicates the actual loadingconfiguration is preferred.1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact eq
7、uivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user
8、 of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E6 Terminology Relating to Methods of Mechanical TestingE206 Definitions of Terms Relating to Fatigue Testing and
9、the Statistical Analysis of Fatigue Data; Replaced byE 11503E466 Practice for Conducting Force Controlled ConstantAmplitude Axial Fatigue Tests of Metallic MaterialsE467 Practice for Verification of Constant Amplitude Dy-namic Forces in an Axial Fatigue Testing SystemE468 Practice for Presentation o
10、f Constant Amplitude Fa-tigue Test Results for Metallic MaterialsE1012 Practice for Verification of Test Frame and SpecimenAlignment Under Tensile and Compressive Axial ForceApplication3. Definitions3.1 The definitions of terms relating to shear and fatiguetesting appearing in Terminology E6 shall b
11、e considered asapplying to the terms used in this test method.4. Summary of Test Method4.1 Shear Fatigue Testing:4.1.1 The intent of the shear fatigue test is to determine theadhesive or cohesive strength, or both, of the coating.4.1.2 This test method is designed to allow the coating tofail at eith
12、er the coating/substrate interface, within the coating,or at the glue/coating interface between the coating and theadhesive bonding agent used to transmit the load to the coating.4.2 Bending Fatigue Testing:1This test method is under the jurisdiction of ASTM Committee F04 on Medicaland Surgical Mate
13、rials and Devices and is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Oct. 1, 2011. Published January 2012. Originallyapproved in 1991. Last previous edition approved in 2005 as F1160 05. DOI:10.1520/F1160-05R11E01.2For referenced ASTM standards,
14、visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.or
15、g.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2.1 The primary intent of the bending fatigue test is toquantify the effect that the coating has on the substrate it isapplied to. Secondarily, it may be used to provide a subjectiv
16、eevaluation of coating adhesion, (that is, spalling resistance,cracking resistance, and so forth).4.2.2 This test method is designed to first provide a substratefatigue strength to serve as a baseline to assess the effects of thecoating on the resulting fatigue strength of the system.5. Significance
17、 and Use5.1 The shear and bending fatigue tests are used to deter-mine the effect of variations in material, geometry, surfacecondition, stress, and so forth, on the fatigue resistance ofcoated metallic materials subjected to direct stress for up to 107cycles. These tests may be used as a relative g
18、uide to theselection of coated materials for service under condition ofrepeated stress.5.2 In order that such basic fatigue data be comparable,reproducible, and can be correlated among laboratories, it isessential that uniform fatigue practices be established.5.3 The results of the fatigue test may
19、be used for basicmaterial property design. Actual components should not betested using these test methods.6. Equipment Characteristics6.1 Equipment characteristics shall be in accordance withPractice E466, Section 7. See also Practices E467 and E1012and Definitions E206.6.2 Shear Fatigue Test Grips:
20、6.2.1 GeneralVarious types of grips may be used totransmit the load to the specimens by the testing machine. Toensure axial shear stress, it is important that the specimen axiscoincide with the centerline of the heads of the testing machineand that the coating test plane be parallel to the axial loa
21、d. Anydeparture from this requirement (that is, any eccentric loading)will introduce bending stresses that are not included in theusual stress calculation (force/cross-sectional area).6.2.2 A drawing of a typical gripping device for the testassembly is shown in Fig. 1.6.2.3 Fig. 2 shows a drawing of
22、 the adaptor to mate theshear fixture to the tensile machine6.2.4 Figs. 3 and 4 show a schematics of the test setup.6.3 Bending Fatigue Test GripsThere are a variety oftesting machines that may be employed for this test (that is,rotating beam fatigue machines and axial fatigue machines).The gripping
23、 method for each type of equipment shall bedetermined by either the manufacturer of that equipment(rotating beam machines) or the user.7. Adhesive Bonding Materials7.1 Adhesive Bonding AgentA polymeric adhesive bond-ing agent in film form, or filled viscous adhesive cement, shallbe identified and sh
24、all meet the following requirements.7.1.1 The bonding agent shall be capable of bonding thecoating on the test specimen components with an adhesiveshear strength that is at least 34.5 MPa 5000 psi or as great asthe minimum required adhesion or cohesion strength of thecoating, whichever is greater.7.
25、1.2 In instances where coating porosity extends to thecoating/substrate interface, the bonding agent shall be suffi-ciently viscous and application to the coating sufficientlydetailed, to ensure that it will not penetrate through the coatingFIG. 1 Gripping Device for Shear TestingFIG. 2 Adaptor to M
26、ate the Gripping Device to the TensileMachineFIG. 3 Schematic of the Shear Test SetupF1160 05 (2011)12to the substrate. The FM 1000 Adhesive Film4with a thicknessof 0.25 mm 0.01 in. has proven satisfactory for this testmethod.7.1.3 If a material other than FM 1000 is used, or thecondition of the FM
27、1000 is unknown, it must be tested toestablish its equivalence to fresh FM 1000. Testing should beperformed without the presence of the coating to establish theperformance of the adhesive.8. Test Specimen8.1 Shear Fatigue Specimen for Calcium Phosphate andMetallic Coatings Only:8.1.1 The recommended
28、 shear test specimen and setup isillustrated in Figs. 3 and 4, respectively. A complete assembledtest assembly consists of two solid pieces, one with a coatedsurface and the other with an uncoated surface. The uncoatedsurface may be roughened to aid in the adhesion of theadhesive bonding agent.8.1.2
29、 The cross-sectional area of the substrate upon whichthe coating is applied shall be a nominal 2.85 cm20.44 in.2.When specimens of another cross-sectional area are used, thedata must be demonstrated to be equivalent to the resultsproduced using the 2.85-cm2standard cross-sectional area andthe specim
30、en size should be reported.8.2 Bending Fatigue Specimen for Calcium Phosphate,Metallic, and Calcium Phosphate-Metallic Composite Coat-ings:8.2.1 The type of specimen used will depend upon theobjective of the test program, the type of equipment, theequipment capacity, and the form in which the materi
31、al isavailable. However, the design must meet certain generalcriteria as follows:8.2.1.1 The design of the specimen should be such that ifspecimen failure should occur, it should occur in the testsection (reduced area as shown in Figs. 5-8).8.2.1.2 Specimens using a flat tapered beam configurationsh
32、ould be designed such that a constant surface stress exists inthe test section when the specimen is constrained at one endand point loaded perpendicular to the beam axis at the otherend (that is, cantilever loading).8.2.1.3 Rotating beam specimens may have unique dimen-sions, depending upon the type
33、 of machine used. Appropriatemanufacturers specifications for these specimens should beused.8.3 Specimen Coating Preparation:8.3.1 Coatings may be applied by any one of a number oftechniques. All test specimens for coating characterizationshall be prepared from indicative coating lots, using product
34、ionfeedstock lots and be coated on the same equipment used foractual implants. The coating should consist of a layer which ismechanically or chemically attached and covers the surface.8.3.2 Coatings should be applied as follows:8.3.2.1 For the shear fatigue specimens, the coating shouldbe applied to
35、 the 19.05-mm 0.75-in. diameter face only (seeFig. 3).8.3.2.2 For the bending fatigue specimens, the coatingshould be applied to the reduced section only, with theexception of the constant stress specimen which should havecoating in the entire region of constant stress (see Figs. 5-9).8.3.3 All ther
36、mal treatments normally performed on thedevices should be performed on the test specimens.8.3.4 If used, passivation and sterilization techniques shouldbe consistent with those used for actual devices.8.3.5 InspectionBefore testing, visual inspections shouldbe performed on 100 % of the test specimen
37、s. Non-uniformcoating density shall be cause for specimen rejection. For theshear fatigue specimen, lack of coating on the coated face shallbe cause for specimen rejection. For the bending fatiguespecimen, lack of coating in highly stressed regions shall because for specimen rejection.9. Procedure9.
38、1 The number of specimens required for testing, as well asthe test methods in which the fatigue data may be interpreted,can vary. Several test methods are referenced in this testmethod.5,6,74The sole source of supply of the apparatus known to the committee at this timeis Cytec Engineered Materials,
39、Inc., 1300 Revolution St., Havre de Grace, MD21078. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.5Collins, J.A.
40、, Failure of Materials in Mechanical Design, John Wiley composite coatings; fatigue testing;hydroxylapatite; metallic coatings; plasma-sprayed coatings;porous coatings; tribasic calcium phosphateF1160 05 (2011)15FIG.10hValuesF1160 05 (2011)16FIG. 11 k ValuesTABLE 1 ASTM F1160 Round Robin, Cycles to
41、FailureSourceA12345683 300 78 000 run out 64 700 64 200 71 90053 500 62 300 26 800 78 800 136 300 51 00080 400 92 200 16 900 137 200 57 000 88 10067 900 36 300 28 700 175 100 48 700 51 20064 900 73 400 17 900 116 400 32 100 58 20089 400 98 200 70 700 211 100 61 300 42 40051 000 49 100 52 900 183 100
42、 45 100 58 40072 500 63 600 22 500 200 500 77 900 84 20046 600 118 200 23 300 161 200 40 000 64 60054 800 40 700 38 000 111 100 55 400 44 80048 100 82 800 36 800 277 500 38 100 73 30097 700 72 700 . . . 183 100 56 800 66 400Average 67 517 6 17 277 72 292 6 22 009 33 450 6 11 622 158 317 6 60 157 59
43、408 6 27 312 62 875 6 14 653A1 = Biomet.2 = Osteonics.3 = Wright Medical.4 = EML.5 = Zimmer.6 = Howmedica.TABLE 2 Precision StatisticsXASxBSrCSRDrERF75 643 42 706 30 269 51 611 84 753 144 511AX = average of the cell averages.BSx= standard deviation of cell averages.CSR= reproducibility standard devi
44、ation.DSr= repeatability standard deviation.Er = 95 % repeatability limit.FR = 95 % reproducibility limit.F1160 05 (2011)17APPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 This test method is needed to aid in the developmentof a high-quality material for use in load-bearing implantapplications. T
45、he influence of coatings on the resulting fatiguebehavior of the system must be viewed as a combination of thesurface-roughening treatments required to apply the coating,the thermal effects of the coating process, and any othersecondary treatments used. The purpose of this test method isto provide t
46、he following information: (1) the influence of thepreceding processing steps and (2) the integrity of the coatingand the coating/substrate interface.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
47、 of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every f
48、ive years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
49、 committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm
