ASTM F1160-14(2017)e1
(Test Method)Standard Test Method for Shear and Bending Fatigue Testing of Calcium Phosphate and Metallic Medical and Composite Calcium Phosphate/Metallic Coatings
Standard Test Method for Shear and Bending Fatigue Testing of Calcium Phosphate and Metallic Medical and Composite Calcium Phosphate/Metallic Coatings
SIGNIFICANCE AND USE
5.1 The shear and bending fatigue tests are used to determine the effect of variations in material, geometry, surface condition, stress, and so forth, on the fatigue resistance of coated metallic materials subjected to direct stress for up to 107 cycles. These tests may be used as a relative guide to the selection of coated materials for service under condition of repeated stress.
5.2 In order that such basic fatigue data be comparable, reproducible, and can be correlated among laboratories, it is essential that uniform fatigue practices be established.
5.3 The results of the fatigue test may be used for basic material property design. Actual components should not be tested using these test methods.
SCOPE
1.1 This test method covers the procedure for determining the shear and bending fatigue performance of calcium phosphate coatings and of porous and nonporous metallic coatings and for determining the bending fatigue performance of metallic coatings over sprayed with calcium phosphate. This test method has been established based on plasma-sprayed titanium and plasma-sprayed hydroxylapatite coatings. The efficacy of this test method for other coatings has not been established. In the shear fatigue mode, this test method evaluates the adhesive and cohesive properties of the coating on a metallic substrate. In the bending fatigue mode, this test method evaluates both the adhesion of the coating as well as the effects that the coating may have on the substrate material. These methods are limited to testing in air at ambient temperature. These test methods are not intended for application in fatigue tests of components or devices; however, the test method which most closely replicates the actual loading configuration is preferred.
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: F1160 − 14 (Reapproved 2017)
Standard Test Method for
Shear and Bending Fatigue Testing of Calcium Phosphate
and Metallic Medical and Composite Calcium Phosphate/
Metallic Coatings
This standard is issued under the fixed designation F1160; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial changes were made throughout in December 2017.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers the procedure for determining
mendations issued by the World Trade Organization Technical
the shear and bending fatigue performance of calcium phos-
Barriers to Trade (TBT) Committee.
phate coatings and of porous and nonporous metallic coatings
and for determining the bending fatigue performance of
2. Referenced Documents
metallic coatings over sprayed with calcium phosphate. This
2.1 ASTM Standards:
test method has been established based on plasma-sprayed
E6 Terminology Relating to Methods of Mechanical Testing
titanium and plasma-sprayed hydroxylapatite coatings. The
E466 Practice for Conducting Force Controlled Constant
efficacy of this test method for other coatings has not been
Amplitude Axial Fatigue Tests of Metallic Materials
established. In the shear fatigue mode, this test method
E467 Practice for Verification of Constant Amplitude Dy-
evaluates the adhesive and cohesive properties of the coating
namic Forces in an Axial Fatigue Testing System
on a metallic substrate. In the bending fatigue mode, this test
E468 Practice for Presentation of Constant Amplitude Fa-
method evaluates both the adhesion of the coating as well as
tigue Test Results for Metallic Materials
the effects that the coating may have on the substrate material.
E1012 Practice for Verification of Testing Frame and Speci-
These methods are limited to testing in air at ambient tempera-
men Alignment Under Tensile and Compressive Axial
ture. These test methods are not intended for application in
Force Application
fatigue tests of components or devices; however, the test
E1832 Practice for Describing and Specifying a Direct
method which most closely replicates the actual loading
Current Plasma Atomic Emission Spectrometer
configuration is preferred.
1.2 The values stated in either SI units or inch-pound units
3. Terminology
are to be regarded separately as standard. The values stated in
3.1 The definitions of terms relating to shear and fatigue
each system may not be exact equivalents; therefore, each
testing appearing in Terminology E6 shall be considered as
system shall be used independently of the other. Combining
applying to the terms used in this test method.
values from the two systems may result in non-conformance
3.2 loading points, n—objects in contact with the test beam
with the standard.
or bar used to apply force to the beam or bar, usually radiused
1.3 This standard does not purport to address all of the
to concentrate the force on a point or a line.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety, health, and environmental practices and deter-
4.1 Shear Fatigue Testing:
mine the applicability of regulatory limitations prior to use.
4.1.1 The intent of the shear fatigue test is to determine the
1.4 This international standard was developed in accor-
adhesive or cohesive strength, or both, of the coating.
dance with internationally recognized principles on standard-
4.1.2 This test method is designed to allow the coating to
fail at either the coating/substrate interface, within the coating,
This test method is under the jurisdiction ofASTM Committee F04 on Medical
and Surgical Materials and Devices and is the direct responsibility of Subcommittee
F04.15 on Material Test Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2017. Published January 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1991. Last previous edition approved in 2014 as F1160 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/F1160-14R17E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F1160 − 14 (2017)
or at the interface between the coating and the adhesive
bonding 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 to
quantify the effect that the coating has on the substrate it is
applied to. Secondarily, it may be used to provide a subjective
evaluation of coating adhesion, (that is, spalling resistance,
cracking resistance, and so forth).
4.2.2 Thistestmethodisdesignedtofirstprovideasubstrate
fatiguestrengthtoserveasabaselinetoassesstheeffectsofthe
coating on the resulting fatigue strength of the system.
5. Significance and Use
5.1 The shear and bending fatigue tests are used to deter-
mine the effect of variations in material, geometry, surface
condition, stress, and so forth, on the fatigue resistance of
FIG. 1 Gripping Device for Shear Testing
coatedmetallicmaterialssubjectedtodirectstressforupto10
cycles. These tests may be used as a relative guide to the
selection of coated materials for service under condition of
repeated stress.
5.2 In order that such basic fatigue data be comparable,
reproducible, and can be correlated among laboratories, it is
essential that uniform fatigue practices be established.
5.3 The results of the fatigue test may be used for basic
material property design. Actual components should not be
tested using these test methods.
6. Equipment Characteristics
6.1 Equipment characteristics shall be in accordance with
Practice E466, Section 7. See also Practices E467, E1012, and
E1832.
6.2 Shear Fatigue Test Grips:
6.2.1 General—Various types of grips may be used to
transmit the load to the specimens by the testing machine. To
ensure axial shear stress, it is important that the specimen axis
coincide with the centerline of the heads of the testing machine
andthatthecoatingtestplanebeparalleltotheaxialforce.Any
departure from this requirement (that is, any eccentric loading)
NOTE 1—(2 PL) indicates the top and bottom adapters are identical.
will introduce bending stresses that are not included in the
FIG. 2 Adaptor to Mate the Gripping Device to the Tensile Ma-
usual stress calculation (force/cross-sectional area).
chine
6.2.2 A drawing of a typical gripping device for the test
assembly is shown in Fig. 1.
6.2.3 Fig. 2 shows a drawing of the adaptor to mate the
shear fixture to the tensile machine
6.2.4 Figs. 3 and 4 show schematics of the test setup.
6.3 Bending Fatigue Test Grips—There are a variety of
testing machines that may be employed for this test (that is,
rotating beam fatigue machines and axial fatigue machines).
The gripping method for each type of equipment shall be
determined by either the manufacturer of that equipment or the
FIG. 3 Schematic of the Shear Test Setup
user.
7. Adhesive Bonding Materials
7.1.1 The bonding agent shall be capable of bonding the
7.1 Adhesive Bonding Agent—A polymeric adhesive bond- coating on the test specimen components with an adhesive
ing agent in film form, or viscous adhesive cement, shall be shear strength that is at least 34.5 MPa [5000 psi] or as great as
identified and shall meet the following requirements. the minimum required adhesion or cohesion strength of the
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F1160 − 14 (2017)
8.1.1 The recommended shear test specimen and setup is
illustrated in Figs. 3 and 4, respectively.Acomplete assembled
test assembly consists of two solid pieces, one with a coated
surface and the other with an uncoated surface. The uncoated
surface may be roughened to aid in the adhesion of the
adhesive bonding agent.
8.1.2 The cross-sectional area of the substrate upon which
2 2
the coating is applied shall be a nominal 2.85 cm [0.44 in. ].
When specimens of another cross-sectional area are used, the
data must be demonstrated to be equivalent to the results
produced using the 2.85-cm standard cross-sectional area and
the specimen 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 the
objective of the test program, the type of equipment, the
equipment capacity, and the form in which the material is
available. The R ratio for bending fatigue tests shall be 0.1 or
FIG. 4 Drawing of the Recommended Shear Test Specimen As- less excluding rotating beam samples. For rotating beam
sembly
samples the R ratio shall be -1.0. However, the design shall
meet certain general criteria as follows:
8.2.1.1 The design of the specimen shall be such that if
specimen failure should occur, it occurs in the test section
coating, whichever is greater. The 34.5 MPa bonding strength
(reduced area as shown in Figs. 5-8).
isthestaticstrengthoftheadhesive.Thefatiguestrengthofthe
8.2.1.2 Specimens using a flat tapered beam configuration
adhesive is usually less than that value. In fatigue the coating
should be designed such that a tapered gauge section with a
under test is often stronger than the adhesive causing the
constant surface stress exists when the specimen is constrained
fracture to occur at the adhesive interface. If it is desirable to
at one end and force applied through loading points perpen-
continue a fatigue test after fracture through the adhesive, the
dicular to and centered on the beam axis at the other end (that
test sample may be rebonded and testing.
is, cantilever loading, usually a tapered cantilever beam as
7.1.2 In instances where coating porosity extends to the
shown in Fig. 9).
coating/substrate interface, the bonding agent shall be suffi-
8.2.1.3 Four-point bend specimens consisting of straight
ciently viscous and application to the coating sufficiently
bars of constant, usually rectangular, cross section loaded in
detailed, to ensure that it will not penetrate through the coating
four-point bending also produce a region of constant surface
to the substrate.The FM 1000Adhesive Film with a thickness
stress in the center span between the two center loading points.
of 0.25 mm [0.01 in.] has proven satisfactory for this test
The distance between the two external loading points shall
method.
always be identical (see Fig. 10).
7.1.3 If a material other than FM 1000 is used, or the
8.2.1.4 Rotating beam specimens may have unique
condition of the FM 1000 is unknown, it must be tested to
dimensions, depending upon the type of machine used.Appro-
establish its equivalence to fresh FM 1000. Testing should be
priate manufacturers’specifications for these specimens should
performed without the presence of the coating to establish the
be used.
performance of the adhesive. Two alternative adhesives that
8.2.1.5 The tensile surface edges of the flat tapered cantile-
have been used successfully are HYSOL 9514 (also known as
ver beam specimen and the four point bend specimen may be
LOCTITE EA 9514 and LOCTITE 9514) and 3M 2214
brokentoasmallnonzeroradiustoavoidstressconcentrations
non-metallic filled. Validation data on Hysol 9514 from In-
at the edge.
dolab GmbH is presented in Appendix X2. These adhesives
may not be suitable for HA coatings because they could
8.3 Specimen Coating Preparation:
penetrate the HA.
8.3.1 Coatings may be applied by any one of a number of
techniques. All test specimens for coating characterization
8. Test Specimen
8.1 Shear Fatigue Specimen for Calcium Phosphate and
Metallic Coatings Only:
The sole source of supply of the apparatus known to the committee at this time
is Cytec Engineered Materials, Inc., 1300 Revolution St., Havre de Grace, MD
FIG. 5 Bending Fatigue Specimen With Tangentially Blending
21078. If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider- Fillets Between the Test Section and the Ends for Rotating Beam
ation at a meeting of the responsible technical committee, which you may attend. or Axial Loading
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F1160 − 14 (2017)
8.3.2.2 For the rotating beam and axial fatigue test speci-
mensthecoatingshallbeappliedallaroundandextendslightly
beyond the reduced sections (see Figs. 5-8). For the tension-
tension bending fatigue specimens, the coating shall be applied
to the side that will be loaded in tension only.The coating shall
FIG. 6 Specimens With a Continuous Radius Between the Ends
for Rotating Beam or Axial loading extend well beyond the tapered gauge area to keep stress
concentrationsatthetransitionfromcoatedsurfacetouncoated
surfaceoutofthehighstressregions(Fig.9).Onthefour-point
bend test sample the coating shall be extended outside of the
inner loading points to keep a possible stress concentration at
the transition from coated surface to uncoated surface outside
the maximum stress center region.).
8.3.3 All thermal treatments normally performed on the
FIG. 7 Specimens With Tangentially Blending Fillets Between the
Uniform Test Section and the Ends for Axial Loading
devices should be performed on the test specimens.
8.3.4 Ifused,passivationandsterilizationtechniquesshould
be consistent with those used for actual devices.
8.3.5 Inspection—Before testing, visual inspections should
be performed on 100 % of the test specimens. Non-uniform
coating density shall be cause for specimen rejection. For the
shear fatigue specimen, lack of coating on the coated face shall
FIG. 8 Specimens With a Continuous Radius Between the Ends
be cause for specimen rejection. For the bending fatigue
for Axial Loading
specimen, lack of coating in highly stressed regions shall be
cause for specimen rejection.
9. Procedure
9.1 Thenumberofspecimensrequiredfortesting,aswellas
the test methods in which the fatigue data may be interpreted,
can vary. Several test methods are referenced in this test
4,5,6
method.
9.2 The type of specimen used will depend upon the
FIG. 9 Tapered Beam Configuration for Bend Testing
objective of the test program, the type of equipment avail
...
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