1、Designation: F1147 05 (Reapproved 2017)1Standard Test Method forTension Testing of Calcium Phosphate and MetallicCoatings1This standard is issued under the fixed designation F1147; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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 corrections were made throughout in June 2017.1. Scope1.1 This test method covers tension testing of calc
3、iumphosphate and metallic porous coatings adhering to densemetal substrates at ambient temperatures. It assesses the degreeof adhesion of coatings to substrates, or the internal cohesionof a coating in tension normal to the surface plane.1.2 The values stated in inch-pound units are to be regardedas
4、 standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered 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 th
5、is standard to establish appro-priate safety and health practices and determine the applica-bility 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 Decision on Princip
6、les 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:2E4 Practices for Force Verification of Testing MachinesE6 Terminology Relating to Methods of Mec
7、hanical TestingE8 Test Methods for Tension Testing of Metallic MaterialsF1501 Test Method for Tension Testing of Calcium Phos-phate Coatings (Withdrawn 2000)33. Terminology3.1 The definitions of terms relating to tension testingappearing in Terminology E6 shall be considered as applyingto the terms
8、used in this test method.4. Summary of Test Method4.1 The tensile test method consists of subjecting a speci-men assembly composed of one coated and one uncoatedcomponent to a tensile load. In the case of the calciumphosphate coatings, the components to be tested must bebonded together by use of a p
9、olymeric adhesive. In the case ofthe metallic coatings, the components may either be bondedwith the adhesive, or sintered together. The adhesive may be infilm form or bulk form, but it must have a minimum bulktensile strength of 34.5 MPa (5000 psi) or as great as theminimum required adhesion or cohe
10、sion strength of thecoating, whichever is greater.4.2 The tensile load must be applied normal to the plane ofthe coating utilizing a tension machine which is capable ofdetermining the maximum strength of the coating or coatingattachment to the substrate interface.5. Significance and Use5.1 The tensi
11、le test method is recommended for tensiontesting of calcium phosphate/substrate or porous metal coating/substrate combinations and can provide information on theadhesive or cohesive strength of coatings under (uniaxial)tensile stress.5.2 The test method may be useful for comparative evalu-ation of a
12、dhesive or cohesive strengths of a variety of types ofcoatings. Coatings may be applied using a variety of methods,including, but not limited to, plasma-spraying and sintering.Information developed using this test method may be useful forcertain quality control and design purposes.5.3 The test shoul
13、d not be considered to provide an intrinsicvalue for utilization directly in making calculations such asdetermining the ability of a coating to withstand specifiedenvironmental stresses.1This test method is under the jurisdiction of ASTM Committee F04 on Medicaland Surgical Materials and Devices and
14、 is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved May 1, 2017. Published June 2017. Originallyapproved in 1988. Last previous edition approved in 2011 as F1147 05 (2011).DOI: 10.1520/F1147-05R17.2For referenced ASTM standards, visit the ASTM websit
15、e, 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,
16、100 Barr Harbor Drive, PO Box 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
17、 Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.4 Processing variables such as substrate preparation priorto coating, surface texture, coating technique variables orpostcoating heat treatment variables may introduce a signifi-cant effect on the
18、results of the tension test. The specimenbeing evaluated must be representative of the actual end-usecoating.6. Apparatus6.1 Testing MachinesMachines used for testing shall con-form to the requirements of Practices E4. The loads used indetermining tensile strength and yield strength shall be withint
19、he loading range of the testing machine as defined in PracticesE4. See also Test Methods E8.6.2 Gripping Devices:6.2.1 GeneralVarious types of grips may be used totransmit the load applied to the specimens by the testingmachine. To ensure axial tensile stress, it is important that thespecimen axis c
20、oincide with the centerline of the heads of thetesting machine and that the coating test plane be perpendicularto the axial load. Any departure from this requirement (that is,any eccentric loading) will introduce bending stresses that arenot included in the usual stress calculation (force/cross-sect
21、ional area).6.2.2 Yoke and Dowel Pin GripsA schematic diagram of atypical gripping device for specimens with holes drilled for pinloading is illustrated in Fig. 1. There should be two perpen-dicular pins in order to maximize off-axis loading.7. Materials7.1 Adhesive Bonding AgentA polymeric adhesive
22、 bond-ing agent in film form, or filled viscous adhesive cement, whenused, shall be identified and shall meet the following require-ments.7.1.1 The bonding agent shall be capable of bonding thecoating on the test specimen components with a tensile strengththat is at least 34.5 MPa (5000 psi) or as g
23、reat as the minimumrequired adhesion or cohesion strength of the coating.7.1.2 In instances where porosity extends to the coatingsubstrate interface, the bonding agent shall be sufficientlyviscous and application to the coating sufficiently careful toassure that it will not penetrate through the coa
24、ting to thesubstrate. The FM 1000 Adhesive Film4with a thickness of0.25 mm (0.01 in.) has proven satisfactory for this test. If amaterial other than FM 1000 is used, or the condition of theFM 1000 is unknown, it must be tested to establish itsequivalence fresh FM 1000. Testing should be performedwit
25、hout the presence of the coating to establish the perfor-mance of the adhesive.8. Test Specimens8.1 General:8.1.1 In order to ensure precision and accuracy in testresults, it is important that care be exercised in the preparationof specimens, both in machining and in the case of multi-partspecimens,
26、 in the assembly. Specimen components must beproperly aligned in order that generated stresses be purelyaxial, that is, normal to the coated surface.8.1.2 Tensile-Type SpecimensThree general types of testspecimens are illustrated in Figs. 2 and 3. A complete,assembled test assembly consists either o
27、f two solid pieces; onewith a coated surface and the other with an uncoated surface orthree solid pieces; two with uncoated surfaces and one with acoating applied on one side. The uncoated surface may beroughened to aid in the bonding of the adhesive.8.1.3 The cross-sectional area of the substrate u
28、pon whichthe coating is applied shall be nominal 5.07 cm2(0.78 in.2).When specimens of another cross-sectional area are used, thedata must be demonstrated to be equivalent to a 5.07 cm2standard cross-sectional area, and the specimen size should bereported.8.1.4 All test specimens for coating charact
29、erization shall beprepared from indicative coating lots, using production feed-stock lots and be coated on the same equipment used for actualimplants.8.2 Specimen Coating Preparation:8.2.1 Coatings may be applied by any one of a number oftechniques. The coating should consist of a layer which ismech
30、anically or chemically attached and covers the surface.4The 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 I
31、nternational Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.FIG. 1 Yoke and Dowel Pin Grips for Tensile Testing Porous Sur-facesF1147 05 (2017)128.2.2 All thermal treatments normally performed on thedevices sh
32、ould be performed on the test specimens.8.2.3 If employed, passivation and sterilization techniquesshould be consistent with those used for actual devices.8.2.3.1 If the passivation and sterilization processes can beshown not to influence the tensile strength, these steps may beeliminated.8.2.4 Insp
33、ectionBefore testing, visual inspections shouldbe performed on 100 % of the test specimens. Lack of coatingin highly stressed regions, as well as non-uniform coatingappearance, shall be cause for specimen rejection.9. Procedure9.1 Specimens tested with FM 1000 adhesive shall beprepared as follows:9.
34、1.1 Curing the AdhesiveThe test results achieved aregreatly dependent upon the adhesive used and the way in whichit is cured. One suggested adhesive commonly used withcalcium phosphate coatings is FM 1000 having a thickness of0.25 mm (0.01 in.). This material has successfully been curedusing the fol
35、lowing cycle: Where testing porous coatings, morethan one layer of glue may need to be employed.NOTE 1In the case of porous coatings, care must be taken to guaranteethat the adhesive does not bond to the substrate.9.1.2 Align the adhesive with the surface of the coating,taking precautions to align t
36、he adhesive in the center of thecoating.9.1.3 Apply a constant force using a calibrated high tem-perature spring, resulting in a stress of 0.138 MPa (20 psi)between the coating and the opposing device that will test thecoating.9.1.3.1 Care must be taken to maintain alignment of thecoating and the ma
37、tching counterface during the curing of theadhesive.9.1.4 Place the assembly in an oven and heat at 176C(350F) for 23 h.9.1.4.1 The exact amount of time necessary to cure theadhesive will need to be determined by each user, as oventemperature may vary with load size and oven type. It issuggested tha
38、t the curing cycle be optimized without thecoating present, first.9.1.5 Remove the cured assembly from the oven and allowit to cool to room temperature.9.1.6 Remove all excess glue which has protruded from thecoated surface. This process must not compromise the integrityof the sample.9.2 Place the s
39、pecimen assembly in the grips so that the longaxis of the specimen coincides with the direction of appliedtensile load through the centerline of the grip assembly.9.3 Apply a tensile load to each test specimen at a constantrate of cross-head speed of 0.25 cm/min (0.10 in. min). TheFIG. 2 Tensile Spe
40、cimens for Testing Porous SurfacesFIG. 3 Smooth Tensile SpecimensF1147 05 (2017)13test should be continued until complete separation of thecomponents has been achieved. Record the maximum loadapplied.10. Calculation10.1 Calculate the substrate area upon which the coating isapplied to the nearest 0.0
41、06 cm2(0.001 in.2). Record peak(failure) load and calculate failing stress in MPa (psi) ofadhesive bond area as follows:S 5 F/A (1)where:S = adhesion or cohesion strength,F = maximum load to failure, andA = cross-sectional area.11. Report11.1 The report shall include the following information:11.1.1
42、 Identification of the materials used in the specimen,including the bonding agent if used.11.1.2 Identification of methods used to apply the coating,including the coating method, heat-treatment, and other data ifavailable, including date, cycle number, and time and tempera-ture of the run.11.1.3 Dim
43、ensional data including the bond cross-sectionalarea and the thickness of the porous or other coated layer.11.1.4 Number of specimens tested.11.1.5 Report all values for the failure load, includingmaximum, minimum, and mean.11.1.6 The mode of failure (for example, cohesive versusadhesive) for each t
44、est specimen.12. Precision and Bias12.1 Precision (beaded F75)The precision of this testmethod was established by an interlaboratory comparisonamong six (6) laboratories. The specimens tested weresintered-bead coatings of F75 (cobalt-chromium-molybdenum)alloy on F75 substrates. The population mean t
45、ensile strengthwas 4325 lbf/in.2(29.8 MPa) for all samples tested by alllaboratories.12.1.1 RepeatabilityFor replicate results obtained by thesame operator on nominally identical test materials, the repeat-ability standard deviation (Sr) was 613 lbf/in.2(4.23 MPa).Anytwo such results (would be expec
46、ted to differ by more than)1715 lbf/in.2(11.8 MPa) only 1 time in 20.12.1.2 ReproducibilityFor independent results obtainedby different operators working in different laboratories onnominally identical test materials, the reproducibility standarddeviation (SR) was 772 lbf/in.2(5.32 MPa). Any two suc
47、hresults (would be expected to differ by more than) 2160 lbf/in.2(14.8 MPa) only 1 time in 20.NOTE 2The precision study under 12.1 was conducted using couponswhich had a one square inch area (1.13 in. diameter). The bead tensilestrength was intentionally lowered for this round robin comparison topro
48、duce coating fractures rather than glue failures in the coupons.12.2 Precision (HA Coating)The precision of this testmethod was established by an interlaboratory comparisonamong seven (7) laboratories. The substrate of the specimenstested was titanium-6aluminum-4vanadium, which washydroxylapatite-co
49、ated. The mean tensile strength was 8405lbf/in.2(58.0) MPa for all samples tested by all laboratories.12.2.1 RepeatabilityFor replicate results obtained by thesame operator on nominally-identical test materials, the repeat-ability standard deviation Srwas 1016 lbf/in.2(7.0 MPa). Anytwo such results (would be expected to differ by more than)2845 lbf/in.2(19.6 MPa) only one time in 20.12.2.2 ReproducibilityFor independent results obtainedby different operators working in different laboratories onnominally-identical test materials, the reproducibility standard
