ASTM F1147-05(2017)e1
(Test Method)Standard Test Method for Tension Testing of Calcium Phosphate and Metallic Coatings
Standard Test Method for Tension Testing of Calcium Phosphate and Metallic Coatings
SIGNIFICANCE AND USE
5.1 The tensile test method is recommended for tension testing of calcium phosphate/substrate or porous metal coating/substrate combinations and can provide information on the adhesive or cohesive strength of coatings under (uniaxial) tensile stress.
5.2 The test method may be useful for comparative evaluation of adhesive or cohesive strengths of a variety of types of coatings. 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 for certain quality control and design purposes.
5.3 The test should not be considered to provide an intrinsic value for utilization directly in making calculations such as determining the ability of a coating to withstand specified environmental stresses.
5.4 Processing variables such as substrate preparation prior to coating, surface texture, coating technique variables or postcoating heat treatment variables may introduce a significant effect on the results of the tension test. The specimen being evaluated must be representative of the actual end-use coating.
SCOPE
1.1 This test method covers tension testing of calcium phosphate and metallic porous coatings adhering to dense metal substrates at ambient temperatures. It assesses the degree of adhesion of coatings to substrates, or the internal cohesion of a coating in tension normal to the surface plane.
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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 and health 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
Relations
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: F1147 − 05 (Reapproved 2017)
Standard Test Method for
Tension Testing of Calcium Phosphate and Metallic
Coatings
This standard is issued under the fixed designation F1147; 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 corrections were made throughout in June 2017.
1. Scope phate Coatings (Withdrawn 2000)
1.1 This test method covers tension testing of calcium
3. Terminology
phosphate and metallic porous coatings adhering to dense
3.1 The definitions of terms relating to tension testing
metal substrates at ambient temperatures. It assesses the degree
appearing in Terminology E6 shall be considered as applying
of adhesion of coatings to substrates, or the internal cohesion
to the terms used in this test method.
of a coating in tension normal to the surface plane.
1.2 The values stated in inch-pound units are to be regarded
4. Summary of Test Method
as standard. The values given in parentheses are mathematical
4.1 The tensile test method consists of subjecting a speci-
conversions to SI units that are provided for information only
men assembly composed of one coated and one uncoated
and are not considered standard.
component to a tensile load. In the case of the calcium
1.3 This standard does not purport to address all of the
phosphate coatings, the components to be tested must be
safety concerns, if any, associated with its use. It is the
bonded together by use of a polymeric adhesive. In the case of
responsibility of the user of this standard to establish appro-
the metallic coatings, the components may either be bonded
priate safety and health practices and determine the applica-
with the adhesive, or sintered together.The adhesive may be in
bility of regulatory limitations prior to use.
film form or bulk form, but it must have a minimum bulk
1.4 This international standard was developed in accor-
tensile strength of 34.5 MPa (5000 psi) or as great as the
dance with internationally recognized principles on standard-
minimum required adhesion or cohesion strength of the
ization established in the Decision on Principles for the
coating, whichever is greater.
Development of International Standards, Guides and Recom-
4.2 The tensile load must be applied normal to the plane of
mendations issued by the World Trade Organization Technical
the coating utilizing a tension machine which is capable of
Barriers to Trade (TBT) Committee.
determining the maximum strength of the coating or coating
2. Referenced Documents attachment to the substrate interface.
2.1 ASTM Standards:
5. Significance and Use
E4 Practices for Force Calibration and Verification of Test-
5.1 The tensile test method is recommended for tension
ing Machines
testingofcalciumphosphate/substrateorporousmetalcoating/
E6 Terminology Relating to Methods of Mechanical Testing
substrate combinations and can provide information on the
E8/E8M Test Methods for Tension Testing of Metallic Ma-
adhesive or cohesive strength of coatings under (uniaxial)
terials
tensile stress.
F1501 Test Method for Tension Testing of Calcium Phos-
5.2 The test method may be useful for comparative evalu-
ation of adhesive or cohesive strengths of a variety of types of
This test method is under the jurisdiction ofASTM Committee F04 on Medical
coatings. Coatings may be applied using a variety of methods,
and Surgical Materials and Devices and is the direct responsibility of Subcommittee
including, but not limited to, plasma-spraying and sintering.
F04.15 on Material Test Methods.
Current edition approved May 1, 2017. Published June 2017. Originally Informationdevelopedusingthistestmethodmaybeusefulfor
approved in 1988. Last previous edition approved in 2011 as F1147 – 05 (2011).
certain quality control and design purposes.
DOI: 10.1520/F1147-05R17E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F1147 − 05 (2017)
5.3 The test should not be considered to provide an intrinsic
value for utilization directly in making calculations such as
determining the ability of a coating to withstand specified
environmental stresses.
5.4 Processing variables such as substrate preparation prior
to coating, surface texture, coating technique variables or
postcoating heat treatment variables may introduce a signifi-
cant effect on the results of the tension test. The specimen
being evaluated must be representative of the actual end-use
coating.
6. Apparatus
6.1 Testing Machines—Machines used for testing shall con-
form to the requirements of Practices E4. The loads used in
determining tensile strength and yield strength shall be within
the loading range of the testing machine as defined in Practices
E4. See also Test Methods E8/E8M.
6.2 Gripping Devices:
6.2.1 General—Various types of grips may be used to
transmit the load applied to the specimens by the testing
machine. To ensure axial tensile stress, it is important that the
specimen axis coincide with the centerline of the heads of the
testingmachineandthatthecoatingtestplanebeperpendicular
to the axial load.Any departure from this requirement (that is,
any eccentric loading) will introduce bending stresses that are
not included in the usual stress calculation (force/cross-
sectional area).
6.2.2 YokeandDowelPinGrips—Aschematic diagram of a
typical gripping device for specimens with holes drilled for pin
FIG. 1 Yoke and Dowel Pin Grips for Tensile Testing Porous Sur-
loading is illustrated in Fig. 1. There should be two perpen-
faces
dicular pins in order to maximize off-axis loading.
7. Materials
8. Test Specimens
7.1 Adhesive Bonding Agent—A polymeric adhesive bond-
8.1 General:
ing agent in film form, or filled viscous adhesive cement, when
8.1.1 In order to ensure precision and accuracy in test
used, shall be identified and shall meet the following require-
results, it is important that care be exercised in the preparation
ments.
of specimens, both in machining and in the case of multi-part
7.1.1 The bonding agent shall be capable of bonding the
specimens, in the assembly. Specimen components must be
coatingonthetestspecimencomponentswithatensilestrength
properly aligned in order that generated stresses be purely
that is at least 34.5 MPa (5000 psi) or as great as the minimum
axial, that is, normal to the coated surface.
required adhesion or cohesion strength of the coating.
8.1.2 Tensile-Type Specimens—Three general types of test
7.1.2 In instances where porosity extends to the coating
specimens are illustrated in Figs. 2 and 3. A complete,
substrate interface, the bonding agent shall be sufficiently
assembledtestassemblyconsistseitheroftwosolidpieces;one
viscous and application to the coating sufficiently careful to
with a coated surface and the other with an uncoated surface or
assure that it will not penetrate through the coating to the
three solid pieces; two with uncoated surfaces and one with a
substrate. The FM 1000 Adhesive Film with a thickness of
coating applied on one side. The uncoated surface may be
0.25 mm (0.01 in.) has proven satisfactory for this test. If a
roughened to aid in the bonding of the adhesive.
material other than FM 1000 is used, or the condition of the
8.1.3 The cross-sectional area of the substrate upon which
FM 1000 is unknown, it must be tested to establish its
2 2
the coating is applied shall be nominal 5.07 cm (0.78 in. ).
equivalence fresh FM 1000. Testing should be performed
When specimens of another cross-sectional area are used, the
without the presence of the coating to establish the perfor-
data must be demonstrated to be equivalent to a 5.07 cm
mance of the adhesive.
standard cross-sectional area, and the specimen size should be
reported.
The sole source of supply of the apparatus known to the committee at this time
8.1.4 Alltestspecimensforcoatingcharacterizationshallbe
is Cytec Engineered Materials, Inc., 1300 Revolution St., Havre de Grace, MD
prepared from indicative coating lots, using production feed-
21078. If you are aware of alternative suppliers, please provide this information to
stock lots and be coated on the same equipment used for actual
ASTM International Headquarters. Your comments will receive careful consider-
ation at a meeting of the responsible technical committee, which you may attend. implants.
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F1147 − 05 (2017)
FIG. 3 Smooth Tensile Specimens
it is cured. One suggested adhesive commonly used with
calcium phosphate coatings is FM 1000 having a thickness of
0.25 mm (0.01 in.). This material has successfully been cured
usingthefollowingcycle:Wheretestingporouscoatings,more
than one layer of glue may need to be employed.
NOTE1—Inthecaseofporouscoatings,caremustbetakentoguarantee
that the adhesive does not bond to the substrate.
9.1.2 Align the adhesive with the surface of the coating,
taking precautions to align the adhesive in the center of the
FIG. 2 Tensile Specimens for Testing Porous Surfaces
coating.
9.1.3 Apply a constant force using a calibrated high tem-
perature spring, resulting in a stress of 0.138 MPa (20 psi)
8.2 Specimen Coating Preparation:
between the coating and the opposing device that will test the
8.2.1 Coatings may be applied by any one of a number of
coating.
techniques. The coating should consist of a layer which is
9.1.3.1 Care must be taken to maintain alignment of the
mechanically or chemically attached and covers the surface.
coating and the matching counterface during the curing of the
8.2.2 All thermal treatments normally performed on the
adhesive.
devices should be performed on the test specimens.
9.1.4 Place the assembly in an oven and heat at 176°C
8.2.3 If employed, passivation and sterilization techniques
(350°F) for 2–3 h.
should be consistent with those used for actual devices.
9.1.4.1 The exact amount of time necessary to cure the
8.2.3.1 If the passivation and sterilization processes can be
adhesive will need to be determined by each user, as oven
shown not to influence the tensile strength, these steps may be
temperature may vary with load size and oven type. It is
eliminated.
suggested that the curing cycle be optimized without the
8.2.4 Inspection—Before testing, visual inspections should
coating present, first.
be performed on 100 % of the test specimens. Lack of coating
9.1.5 Remove the cured assembly from the oven and allow
in highly stressed regions, as well as non-uniform coating
it to cool to room temperature.
appearance, shall be cause for specimen rejection.
9.1.6 Remove all excess glue which has protruded from the
9. Procedure coated surface.This process must not compromise the integrity
of the sample.
9.1 Specimens tested with FM 1000 adhesive shall be
prepared as follows: 9.2 Placethespecimenassemblyinthegripssothatthelong
9.1.1 Curing the Adhesive—The test results achieved are axis of the specimen coincides with the direction of applied
greatlydependentupontheadhesiveusedandthewayinwhich tensile load through the centerline of the grip assembly.
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F1147 − 05 (2017)
9.3 Apply a tensile load to each test specimen at a constant abilitystandarddeviation(S )was613lbf/in. (4.23MPa).Any
r
rate of cross-head speed of 0.25 cm/min (0.10 in.⁄min). The two such results (would be expected to differ by more than)
test should be continued until complete separation of the 1715 lbf/in. (11.8 MPa) only 1 time in 20.
components has been achieved. Record the maximum load 12.1.2 Reproducibility—For independent results obtained
applied. by different operators working in different laboratories on
nominally identical test materials, the reproducibility standard
10. Calculation
deviation (S ) was 772 lbf/in. (5.32 MPa). Any two such
R
results (would be expected to differ by more than) 2160 lbf/in.
10.1 Calculate the substrate area upon which the coating is
2 2
(14.8 MPa) only 1 time in 20.
applied to the nearest 0.006 cm (0.001 in. ). Record peak
(failure) load and calculate failing stress in MPa (psi) of
NOTE 2—The precision study under 12.1 was conducted using coupons
adhesive bond area as follows:
which had a one square inch area (1.13 in. diameter). The bead tensile
strength was intentionally lowered for this round robin comparison to
S 5 F/A (1)
produce coating fractures rather than glue failures in the coupons.
where:
12.2 Precision (HA Coating)—The precision of this test
method was established by an interlaboratory comparison
S = adhesion or cohesion strength,
among seven (7) laboratories. The substrate of the specimens
F = maximum load to failure, and
A = cross-sectional area.
tested was titanium-6aluminum-4vanadium, which was
hydroxylapatite-coated. The mean tensile strength was 8405
11. Report
lbf/in. (58.0) MPa for all samples tested by all laboratories.
12.2.1 Repeatability—For replicate results obtained by the
11.1 The report shall include the following information:
same operator on nominally-identical test materials, the repeat-
11.1.1 Identification of the materials used in the specimen,
ability standard deviation S was 1016 lbf/in. (7.0 MPa). Any
including the bonding agent if used.
r
two such results (would be expected to differ by more than)
11.1.2 Identification of methods used to apply the coating,
2845 lbf/in. (19.6 MPa) only one time in 20.
including the coating method, heat-treatment, and other data if
12.2.2 Reproducibility—For independent results obtained
available, including date, cycle number, and time and tempera-
by different operators working in different laboratories on
ture of the run.
nominally-identical test materials, the reproducibility standard
11.1.3 Dimensional data including the bond cross-sectional
deviation (S ) was 1758 lbf/in. (12.1 MPa). Any two such
area and the thickness of the porous or other coated layer.
R
results (would be expected to differ by more than) 4922 lbf/in.
11.1.4 Number of specimens tested.
(33.9 MPa) only one time in 20.
11.1.5 Report all values for the failure load, including
maximum, minimum, and mea
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