1、Designation: F 2384 05Standard Specification forWrought Zirconium-2.5Niobium Alloy for Surgical ImplantApplications (UNS R60901)1This standard is issued under the fixed designation F 2384; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers the chemical, mechanical, andmetallurgical requirements for wrought zirco
3、nium-2.5niobiumalloy to be used in the manufacture of surgical implants (1).21.2 The values stated in inch-pound units are to be regardedas the standard. The SI equivalents in parentheses may beapproximate.2. Referenced Documents2.1 ASTM Standards:3B 550/B 550M Specification for Zirconium and Zircon
4、iumAlloy Bar and WireE8 Test Methods for Tension Testing of Metallic MaterialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE112 Test Methods for Determining Average Grain SizeE 1552 Test Method for Determining Hafnium in Zirco-nium and Zirconium A
5、lloys Using the D-C Argon PlasmaSpectrometerF67 Specification for Unalloyed Titanium for SurgicalImplant Applications (UNS R50250, UNS R50400, UNSR50550, UNS R50700)F 748 Practice for Selecting Generic Biological Test Meth-ods for Materials and Devices2.2 ISO Standard:4ISO 6829 Metallic Materials Te
6、nsile Testing at AmbientTemperature2.3 American Society for Quality Standard:5ASQ C1 Specification of General Requirements for a Qual-ity Program3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 annealed, adjmaterial that exhibits a recrystalizedgrain structure.3.1.2 lot, nthe t
7、otal number of mill products producedfrom the same melt heat under the same conditions at essen-tially the same time.4. Product Classification4.1 barrounds, flats or shapes from 0.1875 to 4 in. (4.76to 101.60 mm) in diameter or thickness (other sizes and shapesby special order).4.2 wirerounds or fla
8、ts less than 0.1875 in. (4.76 mm) indiameter or thickness.5. Ordering Information5.1 Include with inquiries and orders for material under thisspecification the following information:5.1.1 Quantity,5.1.2 ASTM designation and date of issue,5.1.3 Grade (if applicable),5.1.4 Form (bar, or wire),5.1.5 Co
9、ndition (see 6.3),5.1.6 Mechanical properties (if applicable for special con-ditions),5.1.7 Finish (see 6.2),5.1.8 Applicable dimension including size, thickness, width,or drawing number,5.1.9 Special tests, if any, and5.1.10 Other requirements.6. Materials and Manufacture6.1 Materials covered by th
10、is specification shall be pro-duced by multiple vacuum melting in arc furnaces, electronbeam melting, or other melting processes conventionally usedfor reactive metals.1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct r
11、esponsibility ofSubcommittee F04.12 on Metallurgical Materials.Current edition approved Jan. 1, 2005. Published January 2005.2The boldface numbers in parentheses refer to the list of references at the end ofthis standard.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
12、 ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.5Available from American Society
13、for Quality (ASQ), 600 N. Plankinton Ave.,Milwaukee, WI 53203.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 FinishThe mill product may be furnished to theimplant manufacturer as descaled or pickled, abrasivelyblasted, chemicall
14、y milled, ground, machined, peeled, pol-ished, or as specified by the purchaser.6.3 ConditionBarstock shall be furnished in the annealedcondition unless otherwise specified.7. Chemical Requirements7.1 The heat analysis shall conform to the chemical com-position of Table 1. Ingot analysis may be used
15、 for reporting allchemical requirements, except hydrogen, oxygen, and nitro-gen. Samples for hydrogen, oxygen and nitrogen shall be takenfrom the finished mill product. The supplier shall not shipmaterial with chemistry outside the requirements specified inTable 1.7.1.1 Requirements for the major an
16、d minor elementalconstituents are listed in Table 1. Also listed are importantresidual elements. Analysis for elements not listed in Table 1 isnot required to verify compliance with this specification.7.2 Product Analysis:7.2.1 Product analysis tolerances do not broaden the speci-fied heat analysis
17、requirements but cover variations betweenlaboratories in the measurement of chemical content. Theproduct analysis tolerances shall conform to the producttolerances in Table 2.7.2.2 The product analysis is either for the purpose ofverifying the composition of a heat or manufacturing lot, or todetermi
18、ne variations in the composition within the heat.7.2.3 Acceptance or rejection of a heat or manufacturing lotof material may be made by the purchaser on the basis of thisproduct analysis.7.3 For referee purposes, use Test Method E 1552 or otheranalytical methods, or both, as agreed upon between thep
19、urchaser and the supplier.7.4 The samples for chemical analysis shall be representa-tive of the material being tested. The utmost care must be usedin sampling zirconium for chemical analysis because of itsaffinity for elements such as oxygen, nitrogen, and hydrogen.In cutting samples for analysis, t
20、herefore, the operation shouldbe carried out insofar as possible in a dust-free atmosphere.Cutting tools should be clean and sharp. Samples for analysisshould be stored in suitable containers.8. Mechanical Requirements8.1 The material supplied under this specification shallconform to the mechanical
21、property requirements in Table 3.8.2 Specimens for tension tests shall be machined from barin the longitudinal direction and tested in accordance with TestMethods E8. Tensile properties shall be determined using astrain rate of 0.003 to 0.007 in./in./min (mm/mm/min) throughyield and then the crosshe
22、ad speed may be increased so as toproduce fracture in approximately one additional minute.8.3 Number of TestsPerform a minimum of two tensiontests from each lot (see 3.1.2). Should either of the two testspecimens not meet the specified requirements, test two addi-tional test pieces representative of
23、 the same lot in the samemanner. The lot will be considered in compliance only if bothadditional test pieces meet the specified requirements.8.4 Tension test results for which any specimen fracturesoutside the gage length shall be considered acceptable, if boththe elongation and reduction of area me
24、ets the minimumrequirements specified. Refer to Test Method E8 sections7.11.4 and 7.11.5. If either the elongation or reduction of areais less than the minimum requirement, discard the test andretest. Retest one specimen for each specimen that did not meetthe minimum requirements.9. Significance of
25、Numerical Limits9.1 The following applies to all specified limits in thisspecification: For purposes of determining conformance withthese specifications, an observed value or calculated value shallbe rounded to the nearest unit in the last right-hand digit usedin expressing the specification limit,
26、in accordance with therounding method of Practice E29.TABLE 1 Chemical RequirementsElementComposition % mass/massmin maxNiobium 2.40 2.80Oxygen 0.09 0.13Carbon 0.027Chromium 0.020Hafnium 0.010Hydrogen 0.0025Iron 0.15Nitrogen 0.0080Tin 0.0050Zirconium balanceAbalanceAAThe percentage of zirconium is d
27、etermined by difference and need not bedetermined or certified.TABLE 2 Product Analysis TolerancesAlloying ElementPermissible Variation fromthe Specified Range,% mass/massNiobium 0.050Oxygen 0.020Carbon 0.002Chromium 0.002Hafnium 0.002Hydrogen 0.0005Iron 0.002Nitrogen 0.0016Tin 0.001TABLE 3 Mechanic
28、al PropertiesAConditionTensile Strength,min, psi (MPa)Yield Strength(0.2 % offset),min, psi (MPa)ElongationBin2 in. or 4D or 4W,min, %Annealed 65 000 (450) 45 000 (310) 15AMechanical properties for conditions other than those listed in this table maybe established by agreement between the supplier a
29、nd the implant manufacturer.BElongation of material 0.063 in. (1.6 mm) or greater in diameter (D) or width(W) shall be measured using a gage length of 2 in. or 4D or 4W. The gage lengthmust be reported with the test results. The method for determining elongation ofmaterial under 0.063 in. (1.6 mm) i
30、n diameter or thickness may be negotiated.Alternately, a gage length corresponding to ISO 6892 may be used when agreedupon by supplier and purchaser. (5.65 =So, where So is the original crosssectional area).F238405210. Special Requirements10.1 The microstructure shall be a fine dispersion of thealph
31、a and beta phases resulting from processing in the alphaplus beta field. There shall be no coarse, elongated alphaplatelets. The average grain size of forgings shall be ASTMNo. 8 or finer when tested in accordance with Test MethodsE112.11. Certification11.1 The supplier shall provide a certification
32、 that thematerial was tested in accordance with this specification. Areport of the test results shall be furnished to the purchaser atthe time of shipment.12. Quality Program Requirements12.1 The supplier shall maintain a quality program asdefined in ASQ C1.13. Keywords13.1 metals (for surgical impl
33、ants); orthopaedic medicaldevices; zirconium alloys; zirconium alloys (for surgicalimplants)APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 The purpose of this specification is to characterize thechemical, mechanical, and metallurgical properties of wroughtzirconium-2.5niobium alloy to be used
34、 in the manufacture ofsurgical implants.X1.2 ISO standards are listed for reference only. Use of anISO standard in addition to or instead of a preferred ASTMstandard may be agreed upon between the purchaser andsupplier.X1.3 This zirconium alloy is based on Specification B 550/B 550M, Grade R60705, a
35、nd has been used extensively in thechemical industry since the 1970s.X2. BIOCOMPATIBILITYX2.1 The suitability of this material from a human implantperspective is dependent on the specific application. Thebiological tests appropriate for the specific site, such asrecommended in Practice F 748, should
36、 be used as a guideline.A summary of the in vitro and animal testing that has beenperformed as of the approval date of this specification isprovided in X2.3.X2.2 No known surgical implant material has ever beenshown to be completely free of adverse reactions in the humanbody. The alloy composition c
37、overed by this specification,however, has been subjected to testing in laboratory animals,and has been used clinically since January 1996 (2-4). Theresults of these studies indicate a well-characterized level oflocal biological response that is equal to or less than thatproduced by the reference mat
38、erial unalloyed titanium (seeSpecification F67) that has a long history of successful clinicalapplication in soft tissue and bone implants in humans.X2.3 As of the time of the original approval of thisspecification, this zirconium alloy material had a limitedhistory of clinical use in humans.An exte
39、nsive series of in vitroand animal studies had been performed as follows, comparingthe biological response to that of a reference material. Thesetests were conducted to support the usage of this material insurgical implant devices (1,5). In all cases, the results indicatedthat this material was no m
40、ore reactive with the environmentthan the reference material.X2.3.1 L929 MEM-Cytotoxicity (Mouse Fibroblasts),X2.3.2 Sensitization Assay (Kligman Maximization Study),X2.3.3 Rabbit Pyrogen Test,X2.3.4 Mammalian Mutagenicity Test (Rodent Bone Mar-row Micronucleus Test),X2.3.5 Rabbit Intramuscular Impl
41、antation Test,X2.3.6 Rabbit Blood Hemolysis Test,X2.3.7 Ames Mutagenicity Assay, andX2.3.8 Systemic Toxicity and Irritation Test (USP XXIIBiological Test).F2384053REFERENCES(1) Davidson, J. A., Asgian, C. M., Mishra, A. K., and Kovacs, P.,“Zirconia (ZrO2)-coated Zirconium-2.5Nb Alloy for Prosthetic
42、KneeBearing Applications,” Bioceramics 5, T. Yamamuro, T. Kokubo, andT. Nakamura (eds.), Kobunshi Kankokia, Kyoto, Japan, 1992, pp.389-401.(2) FDA 510(k) No. K914878.(3) FDA 501(k) No. K934353.(4) FDA 501(k) No. K962557.(5) Goodman, S. B., Davidson, J. A., Fornasier, V. L., and Mishra, A. K.,“Histol
43、ogical Response to Cylinders of a Low Modulus TitaniumAlloy (Ti-13Nb-13Zr) and a Wear Resistant Zirconium Alloy (Zr-2.5Nb) Implanted in the Rabbit Tibia,” J. Appl. Biomater., 4 (4), 1993,pp. 331-339.ASTM International takes no position respecting the validity of any patent rights asserted in connect
44、ion with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsibl
45、e technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful cons
46、ideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 B
47、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).F2384054
