1、Designation: F3160 16Standard Guide forMetallurgical Characterization of Absorbable MetallicMaterials for Medical Implants1This standard is issued under the fixed designation F3160; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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.1. Scope1.1 This guidance document provides metallurgical charac-terization information that may be beneficial in the e
3、valuationof absorbable metallic materials intended for medical implantapplications. This guide is primarily intended for absorbablemetallic materials that undergo further processing into afabricated final device. Therefore, this standard does notrequire assessments that are more appropriately conduc
4、ted onthe final device, such as biological evaluation. However, a fewrelevant standards for finished implant devices are included forinformation purposes.1.2 The purpose of this guide is to identify appropriate testmethods and relevant medical product standards that can beused to develop future stan
5、dards for new or modified absorb-able metallic materials.1.3 This guide is not intended to cover other major classesof absorbable materials such as polymers, ceramics,composites, and tissue-engineered materials.1.4 This standard guide is focused on the chemical,physical, microstructural, and mechani
6、cal properties plus in-spection guidelines for metallic materials that are used formedical implants designed to be absorbed in the body over aperiod of time. This guide focuses on material characteriza-tions and does not address device specific mechanical testingthat may be necessary to determine sa
7、fety and functionality ofthe implant.1.5 Compliance with materials specifications developed inaccordance with this standard may not necessarily result in amaterial suitable for its intended purpose. Additional testingspecific to the intended use may be required.1.6 Since surface modifications of med
8、ical implants aregenerally applied in the latter stages of manufacturing, thisstandard guide does not cover the characterization of eitherabsorbable or non-absorbable surface coatings that are metallicin origin such as oxides or from the addition of other materialssuch as ceramics or polymers. Howev
9、er, this standard doesapply to absorbable metallic materials, regardless of thepresence or absence of a coating.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate saf
10、ety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2A262 Practices for Detecting Susceptibility to IntergranularAttack in Austenitic Stainless SteelsA342/A342M Test Methods for Permeability of WeaklyMagnetic Mate
11、rialsA480/A480M Specification for General Requirements forFlat-Rolled Stainless and Heat-Resisting Steel Plate,Sheet, and StripA484/A484M Specification for General Requirements forStainless Steel Bars, Billets, and ForgingsA555/A555M Specification for General Requirements forStainless Steel Wire and
12、 Wire RodsA751 Test Methods, Practices, and Terminology for Chemi-cal Analysis of Steel ProductsA957 Specification for Investment Castings, Steel andAlloy,Common Requirements, for General Industrial UseB69 Specification for Rolled ZincB80 Specification for Magnesium-Alloy Sand CastingsB86 Specificat
13、ion for Zinc and Zinc-Aluminum (ZA) AlloyFoundry and Die CastingsB90/B90M Specification for Magnesium-Alloy Sheet andPlateB107/B107M Specification for Magnesium-Alloy ExtrudedBars, Rods, Profiles, Tubes, and WireB199 Specification for Magnesium-Alloy Permanent MoldCastingsB403 Specification for Magn
14、esium-Alloy Investment Cast-ings1This guide is under the jurisdiction of ASTM Committee F04 on Medical andSurgical Materials and Devices and is the direct responsibility of SubcommitteeF04.12 on Metallurgical Materials.Current edition approved April 1, 2016. Published May 2016. DOI: 10.1520/F316016.
15、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 Box C
16、700, West Conshohocken, PA 19428-2959. United States1B557M Test Methods for Tension Testing Wrought and CastAluminum- and Magnesium-Alloy Products (Metric)B661 Practice for Heat Treatment of Magnesium AlloysB949 Specification for General Requirements for Zinc andZinc Alloy ProductsB953 Practice for
17、Sampling Magnesium and MagnesiumAlloys for Spectrochemical AnalysisB954 Test Method for Analysis of Magnesium and Magne-sium Alloys by Atomic Emission SpectrometryD3648 Practices for the Measurement of RadioactivityE8/E8M Test Methods for Tension Testing of Metallic Ma-terialsE18 Test Methods for Ro
18、ckwell Hardness of Metallic Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE45 Test Methods for Determining the Inclusion Content ofSteelE112 Test Methods for Determining Average Grain SizeE290 Test Methods for Bend Testing of Material for
19、 Ductil-ityE340 Practice for Macroetching Metals and AlloysE354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE384 Test Method for Microindentation Hardness of Mate-rialsE407 Practice for Microetching Metals and AlloysE5
20、36 Test Methods for Chemical Analysis of Zinc and ZincAlloysE1245 Practice for Determining the Inclusion or Second-Phase Constituent Content of Metals by Automatic ImageAnalysisE1382 Test Methods for Determining Average Grain SizeUsing Semiautomatic and Automatic Image AnalysisE1441 Guide for Comput
21、ed Tomography (CT) ImagingE2627 Practice for Determining Average Grain Size UsingElectron Backscatter Diffraction (EBSD) in Fully Recrys-tallized Polycrystalline MaterialsF601 Practice for Fluorescent Penetrant Inspection of Me-tallic Surgical ImplantsF629 Practice for Radiography of Cast Metallic S
22、urgicalImplantsF2052 Test Method for Measurement of Magnetically In-duced Displacement Force on Medical Devices in theMagnetic Resonance EnvironmentF2119 Test Method for Evaluation of MR Image Artifactsfrom Passive ImplantsF2182 Test Method for Measurement of Radio FrequencyInduced Heating On or Nea
23、r Passive Implants DuringMagnetic Resonance ImagingF2213 Test Method for Measurement of Magnetically In-duced Torque on Medical Devices in the Magnetic Reso-nance EnvironmentF2229 Specification for Wrought, Nitrogen Strengthened23Manganese-21Chromium-1Molybdenum Low-NickelStainless Steel Alloy Bar a
24、nd Wire for Surgical Implants(UNS S29108)F2393 Specification for High-Purity Dense Magnesia Par-tially Stabilized Zirconia (Mg-PSZ) for Surgical ImplantApplicationsF2581 Specification for Wrought Nitrogen Strengthened11Manganese-17Chromium-3Molybdenum Low-NickelStainless Steel Alloy Bar and Wire for
25、 Surgical Implants(UNS S29225)F2902 Guide for Assessment of Absorbable Polymeric Im-plantsIEEE/ASTM SI 10 American National Standard for MetricPractice2.2 Aerospace Material Standards (AMS):3AMS 2248 Chemical Check Analysis Limits Corrosion andHeat Resistant Steels and Alloys, Maraging and OtherHigh
26、ly-Alloyed Steels, and Iron AlloysAMS 2630 Inspection, Ultrasonic Product Over 0.5 inch(12.7 mm) ThickAMS 2632 Ultrasonic Inspection of Thin Materials2.3 ISO Standards:4ISO 404 Steel and Steel ProductsGeneral Technical De-livery RequirementsISO 643 SteelsMicrographic Determination of the Appar-ent G
27、rain SizeISO 3116 Magnesium and Magnesium AlloysWroughtMagnesium AlloysFourth editionISO 3815-1 Zinc and Zinc AlloysPart 1: Analysis of SolidSamples by Optical Emission SpectrometryISO 3815-2 Zinc and Zinc AlloysPart 2: Analysis byInductively Coupled Optical Emission SpectrometryISO 4967 SteelDeterm
28、ination of Content of NonmetallicInclusionsMicrographic Method Using Standard Dia-gramsISO 6892-1 Metallic MaterialsTensile TestingPart 1:Method of Test at Room TemperatureISO 10993-15 Biological Evaluation of Medical DevicesPart 15: Identification and Quantification of DegradationProducts from Meta
29、ls and AlloysISO 10993-17 Biological Evaluation of Medical DevicesPart 17: Establishment of Allowable Limits for LeachableSubstancesISO 10993-18 Biological Evaluation of Medical DevicesPart 18: Chemical Characterization of MaterialsISO/TS 10993-19-Part 19 Physico-chemical, Morphologicaland Topograph
30、ical Characterization of MaterialsISO 13067 Microbeam AnalysisElectron BackscatterDiffractionMeasurement of Average Grain SizeISO 13485 Medical Devices Quality ManagementSystemsRequirements for Regulatory PurposesSecond editionISO 16220 Magnesium and Magnesium AlloysMagnesium Alloy Ingots and Castin
31、gsISO/TS 17137 Cardiovascular Implants and ExtracorporealSystemsCardiovascular Absorbable Implants3Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,PA 15096, http:/www.sae.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY
32、 10036, http:/www.ansi.org.F3160 162ISO 24173 Microbeam AnalysisGuidelines for Orienta-tion Measurement Using Electron Backscatter DiffractionISO/TR 37137 Biological Evaluation of Medical DevicesGuidance for Absorbable ImplantsISO 9001 Quality Management SystemsRequirements3. Terminology3.1 Definiti
33、ons:3.1.1 absorbable, adjin the body, an initially distinctforeign material or substance that either directly or throughintended degradation can pass through or be metabolized orassimilated by cells and/or tissue. F29024. Summary of Guide4.1 Novel absorbable metallic implant materials that do notyet
34、 have industry standards are being developed for use inapplications such as cardiovascular, orthopedic, generalsurgical, and diagnostic. The lack of a standard guide for themetallurgical characterization of these new materials maycontribute to material property non-uniformity which couldcreate varia
35、tion in the observed performance of the finalproduct. It is the intent of this guide to provide materialproperty information, corresponding test methods, and relevantmedical product standards to serve as a guide for the metal-lurgical characterization of new or modified materials. Theseguidelines ar
36、e tabulated to assist with the development ofspecifications for new or modified absorbable metallic materi-als.4.2 This guide is focused on providing a characterizationscheme for materials prior to their fabrication into a finishedmedical implant. The characterization and testing of absorb-able meta
37、llic materials after they have been manufactured intofinished and sterilized medical implants will depend on thedesign, mass, shape, anatomic location, and end-use applica-tion.5. Significance and Use5.1 The metallurgical properties of materials used to manu-facture absorbable metallic implants can
38、influence biologicalreactions and mechanical interaction with soft and hard tissuein the body. This standard guide describes a suggested materialcharacterization scheme for absorbable metallic materials toensure reproducibility of properties prior to their manufactureinto medical implants.6. Charact
39、erization6.1 Overview:6.1.1 The metallurgical characterization of absorbable me-tallic materials includes the influence of chemical,microstructural, physical, and mechanical properties in addi-tion to material inspection methods that are utilized to docu-ment initial material quality and uniformity.
40、6.1.2 This metallurgical characterization guide will focus onmagnesium (Mg)-base, iron (Fe)-base, and zinc (Zn)-basealloys since these are the main classes of metallic materials thathave been documented in the literature for potential absorbablemetallic implant applications. This guide may be applic
41、able toother absorbable alloy systems.6.1.3 The below described evaluations are general in theirscope, with additional unlisted material assessments potentiallyneeded to address the performance requirements of a specificimplant application.6.2 General:6.2.1 General requirements are specified in B90/
42、B90M andB107/B107M for wrought Mg-base product forms; A480/A480M, A484/A484M, and A555/A555M for wrought Fe-base product forms; and B949 for Zn-base product forms.6.2.2 Requirements are specified in B403 for Mg-basecastings; A957 for Fe-base castings; and B86 for Zn-basecastings.6.3 Chemical:6.3.1 S
43、ome examples of absorbable Mg compositions thathave been investigated to date include pure Mg, conventionalMg alloys, and experimental Mg alloys containing combina-tions of aluminum (Al), calcium (Ca), lithium (Li), manganese(Mn), neodymium (Nd), rare earth (RE), silver (Ag), yttrium(Y), zinc (Zn),
44、or zirconium (Zr).6.3.2 Some examples of absorbable Fe compositions thathave been investigated to date include pure Fe, a range ofFe-Mn alloys with and without silicon (Si) or palladium (Pd),and novel binary Fe compositions containing either aluminum(Al), boron (B), carbon, (C), cobalt (Co), sulfur
45、(S), or tungsten(W).6.3.3 Some examples of absorbable Zn compositions thathave been investigated to date include pure Zn, commercial Znalloys, and binary Zn-Mg combinations.6.3.4 Relevant technical information5has been publishedfor the majority of the absorbable alloy compositions docu-mented in 6.3
46、.1 and 6.3.2.6.3.5 Elemental concentrations present at specified major,minor, residual, or trace levels are defined in A751 and ISO3116. Within this context, a trace classification does notinclude elements that are a specified component of the alloy,regardless of concentration.NOTE 1For the material
47、s covered by this standard, no biocompatibil-ity assessment is required since this standard focuses on characterizationof materials that are subject to further fabrication into a final device.However, since the overall composition of any absorbable implant can beexpected to have a significant impact
48、 on its biocompatibility, the entirecomposition of materials covered by this standard (including the intendedcomposition, metallic degradation species, and any residual or tracemetallic or non-metallic impurities) should be preliminarily assessed fortheir potential impact on any later ISO 10993 risk
49、 assessment of the finaldevice. In addition to the ISO 10993 series, additional supplementalguidance specific for the biological evaluation of absorbable implants canbe found in ISO TR37137.6.3.6 Chemical analysis may be performed according toE354 for Fe-base materials, B954 for Mg-base materials, andE536 for Zn-base materials.6.3.7 Chemical check analysis tolerance limits specified inAMS 2248 may be used to verify heat analysis of Fe-basematerials.5Hendra Hermawan, Biodegradable Metals from Concept to Applications,Spinger, 2012, ISSN 2192-1091; ISSN 2192- 1
