1、Designation: F1160 14 (Reapproved 2017)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.1NOTEEditorial changes were made throughout in Decemb
3、er 2017.1. 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 over sprayed with calcium phosphate.
4、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 a m
5、etallic 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 applicatio
6、n 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 equiv
7、alents; 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 of
8、 this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the
9、Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2E6 Terminology Relating to Methods of Mechanical TestingE466 Practice for Con
10、ducting 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 of Constant Amplitude Fa-tigue Test Results for Metallic MaterialsE1012 Practice f
11、or Verification of Testing Frame and Speci-men Alignment Under Tensile and Compressive AxialForce ApplicationE1832 Practice for Describing and Specifying a DirectCurrent Plasma Atomic Emission Spectrometer3. Terminology3.1 The definitions of terms relating to shear and fatiguetesting appearing in Te
12、rminology E6 shall be considered asapplying to the terms used in this test method.3.2 loading points, nobjects in contact with the test beamor bar used to apply force to the beam or bar, usually radiusedto concentrate the force on a point or a line.4. Summary of Test Method4.1 Shear Fatigue Testing:
13、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 either the coating/substrate interface, within the coating,1This test method is under the jurisdiction of ASTM Commit
14、tee F04 on Medicaland Surgical Materials and Devices and is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Dec. 1, 2017. Published January 2018. Originallyapproved in 1991. Last previous edition approved in 2014 as F1160 14. DOI:10.1520/F1160-14R17E
15、01.2For referenced ASTM standards, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
16、x C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by t
17、he World Trade Organization Technical Barriers to Trade (TBT) Committee.1or at the interface between the coating and the adhesivebonding agent used to transmit the force to the coating.4.2 Bending Fatigue Testing:4.2.1 The primary intent of the bending fatigue test is toquantify the effect that the
18、coating has on the substrate it isapplied to. Secondarily, it may be used to provide a subjectiveevaluation 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
19、assess the effects of thecoating on the resulting fatigue strength of the system.5. Significance 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 m
20、aterials subjected to direct stress for up to 107cycles. These tests may be used as a relative guide 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 is
21、essential that uniform fatigue practices be established.5.3 The results of the fatigue test may 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
22、, Section 7. See also Practices E467, E1012, andE1832.6.2 Shear Fatigue Test Grips: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
23、 of the testing machineand that the coating test plane be parallel to the axial force.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 grip
24、ping device for the testassembly is shown in Fig. 1.6.2.3 Fig. 2 shows a drawing of the adaptor to mate theshear fixture to the tensile machine6.2.4 Figs. 3 and 4 show schematics of the test setup.6.3 Bending Fatigue Test GripsThere are a variety oftesting machines that may be employed for this test
25、 (that is,rotating beam fatigue machines and axial fatigue machines).The gripping method for each type of equipment shall bedetermined by either the manufacturer of that equipment or theuser.7. Adhesive Bonding Materials7.1 Adhesive Bonding AgentA polymeric adhesive bond-ing agent in film form, or v
26、iscous adhesive cement, shall beidentified and shall 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 cohesio
27、n strength of theFIG. 1 Gripping Device for Shear TestingNOTE 1(2 PL) indicates the top and bottom adapters are identical.FIG. 2 Adaptor to Mate the Gripping Device to the Tensile Ma-chineFIG. 3 Schematic of the Shear Test SetupF1160 14 (2017)12coating, whichever is greater. The 34.5 MPa bonding str
28、engthis the static strength of the adhesive. The fatigue strength of theadhesive is usually less than that value. In fatigue the coatingunder test is often stronger than the adhesive causing thefracture to occur at the adhesive interface. If it is desirable tocontinue a fatigue test after fracture t
29、hrough the adhesive, thetest sample may be rebonded and testing.7.1.2 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
30、coatingto the substrate. The FM 1000 Adhesive Film3with 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 1000 is unknown, it must be tested toestablish its equivalence to fresh FM 1000. Testing should
31、 beperformed without the presence of the coating to establish theperformance of the adhesive. Two alternative adhesives thathave been used successfully are HYSOL 9514 (also known asLOCTITE EA 9514 and LOCTITE 9514) and 3M 2214non-metallic filled. Validation data on Hysol 9514 from In-dolab GmbH is p
32、resented in Appendix X2. These adhesivesmay not be suitable for HA coatings because they couldpenetrate the HA.8. Test Specimen8.1 Shear Fatigue Specimen for Calcium Phosphate andMetallic Coatings Only:8.1.1 The recommended shear test specimen and setup isillustrated in Figs. 3 and 4, respectively.
33、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 The cross-sectional area of the substrate upon whichthe coating is applied s
34、hall 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 specimen size should be reported.8.2 Bending Fatigue Specimen for Calcium Phosphate
35、,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 material isavailable. The R ratio for bending fatigue tests shall be 0.1 orless exc
36、luding rotating beam samples. For rotating beamsamples the R ratio shall be -1.0. However, the design shallmeet certain general criteria as follows:8.2.1.1 The design of the specimen shall be such that ifspecimen failure should occur, it occurs in the test section(reduced area as shown in Figs. 5-8)
37、.8.2.1.2 Specimens using a flat tapered beam configurationshould be designed such that a tapered gauge section with aconstant surface stress exists when the specimen is constrainedat one end and force applied through loading points perpen-dicular to and centered on the beam axis at the other end (th
38、atis, cantilever loading, usually a tapered cantilever beam asshown in Fig. 9).8.2.1.3 Four-point bend specimens consisting of straightbars of constant, usually rectangular, cross section loaded infour-point bending also produce a region of constant surfacestress in the center span between the two c
39、enter loading points.The distance between the two external loading points shallalways be identical (see Fig. 10).8.2.1.4 Rotating beam specimens may have uniquedimensions, depending upon the type of machine used. Appro-priate manufacturersspecifications for these specimens shouldbe used.8.2.1.5 The
40、tensile surface edges of the flat tapered cantile-ver beam specimen and the four point bend specimen may bebroken to a small non zero radius to avoid stress concentrationsat the edge.8.3 Specimen Coating Preparation:8.3.1 Coatings may be applied by any one of a number oftechniques. All test specimen
41、s for coating characterization3The sole source of supply of the apparatus known to the committee at this timeis Cytec Engineered Materials, Inc., 1300 Revolution St., Havre de Grace, MD21078. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters
42、. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.FIG. 4 Drawing of the Recommended Shear Test Specimen As-semblyFIG. 5 Bending Fatigue Specimen With Tangentially BlendingFillets Between the Test Section and the Ends for Rot
43、ating Beamor Axial LoadingF1160 14 (2017)13shall be prepared from indicative coating lots, using productionfeedstock 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 Coatin
44、gs should be applied as follows:8.3.2.1 For the shear fatigue specimens, the coating shouldbe applied to the 19.05-mm 0.75-in. diameter face only (seeFig. 3).8.3.2.2 For the rotating beam and axial fatigue test speci-mens the coating shall be applied all around and extend slightlybeyond the reduced
45、sections (see Figs. 5-8). For the tension-tension bending fatigue specimens, the coating shall be appliedto the side that will be loaded in tension only. The coating shallextend well beyond the tapered gauge area to keep stressconcentrations at the transition from coated surface to uncoatedsurface o
46、ut of the high stress regions (Fig. 9). On the four-pointbend test sample the coating shall be extended outside of theinner loading points to keep a possible stress concentration atthe transition from coated surface to uncoated surface outsidethe maximum stress center region.).8.3.3 All thermal trea
47、tments 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 specimens. Non-u
48、niformcoating 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. Procedure9.1 The nu
49、mber 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.4,5,69.2 The type of specimen used will depend upon theobjective of the test program, the type of equipment available,the equipment capacity, and the form in which the material isavailable. The specimen chosen should come as close tomatching the intended application as possible.9.3 The test frequency used shall not exceed 50 Hz forrotating beam tests and 30 Hz for bending fatigue tests.
