1、Designation: F 1713 03Standard Specification forWrought Titanium-13Niobium-13Zirconium Alloy for SurgicalImplant Applications (UNS R58130)1This standard is issued under the fixed designation F 1713; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se of revision, 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. Scope*1.1 This specification covers the chemical, mechanical, andmetallurgical requirements for wr
3、ought titanium-13niobium-13zirconium alloy to be used in the manufacture of surgicalimplants (1).21.2 The values stated in inch pound units are to be regardedas the standard. The SI equivalents in parentheses are providedfor information only.2. Referenced Documents2.1 ASTM Standards:E 8 Methods of T
4、ension Testing of Metallic Materials3E 120 Test Methods for Chemical Analysis of Titanium andTitanium Alloys4F 748 Practice for Selecting Generic Biological Test Meth-ods for Materials and Devices5F 1472 Specification for Wrought Titanium-6Aluminum-4Vanadium Alloy for Surgical Implant Applications (
5、UNSR56400)52.2 Aerospace Material Specification:AMS 2249 Chemical Check Analysis Limits, Titanium andTitanium Alloys62.3 American Society for Quality (ASQ) Standard:ASQ C1 Specifications of General Requirements for aQuality Program72.4 ISO Standard:ISO 6892 Metallic Materials Tensile Testing at Ambi
6、entTemperature83. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 capability aged, nthe condition of the material thatis obtained if, following solution treatment, a sample of themill product is subjected to an aging treatment such as givenbelow, for certification testing.3.1.1.1
7、 Age for 6 6 0.25 h at 923 6 25F (495 6 14C).3.1.1.2 Remove from furnace and air cool to room tempera-ture.3.1.2 solution treated, nthe condition of the material thatis obtained if, following the final hot-working or cold-workingoperation, the mill product is rapidly quenched, for example,by water q
8、uenching, from a temperature above 1112F(600C).3.1.3 unannealed, nthe condition of the material that isobtained after the normal hot-working or cold-working opera-tion used for fabrication of the mill product. There are nosubsequent heat treatment requirements.4. Product Classification4.1 BarRounds
9、or flats from316 in. (4.75 mm) to 4 in.(101.60 mm), inclusive, in diameter or thickness. (Other sizesand shapes by special order.)4.2 WireRounds or flats less than316 in. (75 mm) indiameter or thickness.5. Ordering Information5.1 Include with inquiries and orders for material under thisspecification
10、 the following information.5.1.1 Quantity (weight or number of pieces),5.1.2 Applicable ASTM designation,5.1.3 Form (wire or bar),5.1.4 Condition (see Section 3),5.1.5 Mechanical properties (if applicable, for special con-ditions),5.1.6 Finish (see 6.2),5.1.7 Applicable dimensions including size, di
11、ameter, thick-ness (for rectangular wire), or print number,5.1.8 Special tests, and5.1.9 Special requirements.1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.12 on Metallurgical Mater
12、ials.Current edition approved June 10, 2003. Published July 2003. Originallyapproved in 1996. Last previous edition approved in 1996 as F 1713 96.2The boldface numbers in parentheses refer to the list of references at the end ofthe text.3Annual Book of ASTM Standards, Vol 03.01.4Annual Book of ASTM
13、Standards, Vol 03.05.5Annual Book of ASTM Standards, Vol 13.01.6Available from Society of Automotive Engineers (SAE), 400 CommonwealthDr., Warrendale, PA 15096-0001.7Available from American Society for Quality (ASQ), 600 N. Plankinton Ave.,Milwaukee, WI 53203.8Available from American National Standa
14、rds Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Materials and Manufacture6.1 The various titanium
15、 mill products covered in thisspecification normally are formed with the conventional forg-ing and rolling equipment found in primary ferrous andnonferrous plants. The alloy is usually multiple melted in arcfurnaces (including furnaces such as plasma arc and electronbeam) of a type conventionally us
16、ed for reactive metals.6.2 FinishThe mill product may be furnished to theimplant manufacturer as descaled, pickled, sandblasted,ground, machined, or combinations of these operations.7. Chemical Requirements7.1 Ensure that the heat analysis conforms to the chemicalcomposition of Table 1. Ingot analys
17、is may be used forreporting all chemical requirements, except hydrogen. Takesamples for hydrogen from the finished mill product.7.1.1 Requirements for the major and minor elementalconstituents are listed in Table 1. Also listed are importantresidual elements. Analysis for elements not listed in Tabl
18、e 1 isnot required to verify compliance with this specification.7.2 Product analysis tolerances do not broaden the specifiedheat analysis requirements but cover variations between labo-ratories in the overcheck measurement of chemical content.The manufacturer shall not ship material that is outside
19、thelimits specified in Table 1. Overcheck analyses outside theProduct Analysis Tolerances of Table 2 are cause for rejectionof the material and subject to referee analyses.7.3 For referee purposes, use Test Methods E 120 or otheranalytical methods agreed upon between the purchaser and thesupplier.7.
20、4 Ensure that the samples for chemical analysis arerepresentative of the material being tested. The utmost caremust be used in sampling titanium for chemical analysisbecause of its affinity for elements such as oxygen, nitrogen,and hydrogen. In cutting samples for analysis, therefore, theoperation s
21、hould be carried out insofar as possible in adust-free atmosphere. Chips should be clean and sharp.Samples for analysis should be stored in suitable containers.8. Mechanical Requirements8.1 Ensure that the material supplied under this specificationconforms to the mechanical property requirements giv
22、en inTable 3.8.2 Specimens for tension tests shall be machined and testedin accordance with Test Methods E 8. Tensile properties shallbe determined using a strain rate of 0.003 to 0.007 in./in./min(mm/mm/min) through the specified yield strength, and thenthe cross-head speed shall be increased so as
23、 to producefracture in approximately one additional minute.8.3 Number of TestsPerform a minimum of two tensiontests from each lot. A lot is defined as the total number of millproducts produced from the same heat under the same condi-tions at essentially the same time. Should either of the two testsp
24、ecimens not meet the specified requirements, test two addi-tional test pieces representative of the same lot in the samemanner. The lot will be considered in compliance only if bothadditional test pieces meet the specified requirements. If aspecimen fails outside the gage, the test is null in accord
25、ancewith Methods E 8, and a retest shall be performed.9. Special Requirements9.1 Ensure that the microstructure is martensitic with finelydispersed alpha or beta phases, or both. The alpha or betaphases, or both, may be too fine to be visible metallographi-cally but must be present to ensure adequat
26、e strength. Nocontinuous alpha network at prior beta grain boundaries will bepresent. The microstructure within the prior beta grain bound-aries will be acicular. Perform metallographic evaluation in theaged condition.9.2 Determine the beta transus temperature for each heat bya suitable method and r
27、eported on the materials certification, ifrequired by the purchaser.9.3 Products supplied with a machined or ground surfacefinish will have no alpha case. For other products, there will beno continuous layer of alpha case, when examined at 1003.TABLE 1 Chemical RequirementsElement Composition, % mas
28、s/massNitrogen, max 0.05Carbon, max 0.08Hydrogen, max 0.012AIron, max 0.25Oxygen, max 0.15Niobium 12.514.0Zirconium 12.514.0TitaniumBbalanceAMaterial 0.032 in. (0.813 mm) and under may have hydrogen content up to0.015 %.BThe percentage of titanium is determined by difference and need not bedetermine
29、d or certified.TABLE 2 Product Analysis ToleranceAElementTolerance Under the Minimum orOver the Maximum Limit %BNitrogen 0.02Carbon 0.02Hydrogen 0.0020Iron 0.10Oxygen 0.02Niobium 0.30Zirconium 0.40ARefer to AMS 2249.BUnder the minimum limit not applicable for elements where only a maximumpercentage
30、is indicated.TABLE 3 Mechanical PropertiesA,BConditionTensileStrength min,psi (MPa)Yield Strength(0.2 % offset),min psi (MPa)Elongationmin,%CReductionof Area min,%DCapability aged 125 000 (860) 105 000 (725) 8 15Solution treated 80 000 (550) 50 000 (345) 15 30Unannealed 80 000 (550) 50 000 (345) 8 1
31、5AUp to 4 in. (101.60 mm) inclusive diameter.BSolution treated or unannealed material is not intended for use as a finalproduct without subsequent hot working or heat treatment, or both.CLimits apply to tests taken both longitudinal and transverse to the direction ofrolling. Elongation of material 0
32、.063 in. (1.575 mm) or greater in diameter (D) orthickness (T) shall be measured using a gage length of 2 in. or 4D or 4T. The gagelength must be reported with the test results. The method for determiningelongation of material under 0.063 in. (1.575 mm) in diameter or thickness may benegotiated. Alt
33、ernately, a gage length corresponding to ISO 6892 may be usedwhen agreed upon between supplier and purchaser. (5.65 square root So, whereSois the original cross sectional area.)DApplies to bar only.F171303210. Certification10.1 The supplier will provide a certification of the materialthat the materi
34、al was manufactured and tested in accordancewith this specification. A report of test results will be furnishedat the time of shipment.11. Quality Program Requirements11.1 The producer will maintain a quality program, such asis defined in Specification ASQ C1.12. Keywords12.1 metals (for surgical im
35、plants)titanium alloys; ortho-paedic medical devicestitanium/titanium alloy; titanium/titanium alloys (for surgical implants)APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 The purpose of this specification is to characterize thechemical, mechanical, and metallurgical properties of wroughttita
36、nium-13niobium-13zirconium alloy to be used in the manu-facture of surgical implants.X1.2 The microstructural requirements contained in thisspecification represent the current general consensus withrespect to optimization of mechanical properties for implantapplications.X1.3 The minimum mechanical p
37、roperties specified ensurea baseline of strength and ductility for the highly stresseddevices for which this alloy is typically used.X1.4 The stress corrosion cracking resistance of this alloyis similar to that of standard grade titanium-6aluminum4vanadium alloy (2).X2. BIOCOMPATIBILITYX2.1 The suit
38、ability of this material from a human implantperspective is dependent on the specific application. Thebiologic tests appropriate for the specific site, such as recom-mended in Practice F 748 should be used as a guideline. Asummary of the in vitro and animal testing that has beenperformed as of the a
39、pproval 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 covered by this specification,however, has been subjected to testing in laboratory animals,and has been
40、used clinically since June 1994. The results ofthese studies indicate a well-characterized level of localbiological response that is equal to or less than that producedby the reference material titanium-6aluminum-4 vanadiumalloy (see Specification F 1472) that has a long history ofsuccessful clinica
41、l application in soft tissue and bone implantsin humans.X2.3 As of the time of the original approval of thisspecification, this titanium alloy material had a limited historyof clinical use in humans. An extensive series of in vitro andanimal studies had been performed (3,4,5,6), as listed asfollows,
42、 comparing the biological response to that of a refer-ence material, titanium-6aluminum-4vanadium alloy. Thesetests were conducted to support the usage of this material insurgical implant devices (6,7,8,9). In all cases, the resultsindicated that this material was no more reactive with theenvironmen
43、t than 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 Implantation Test,X2.3.6 Rabbit Blo
44、od Hemolysis Test,X2.3.7 Ames Mutagenicity Assay, andX2.3.8 Systemic Toxicity and Irritation Test (USP XXIIBiological Test).F1713033REFERENCES(1) Mishra, A.K., Davidson, J.A., Kovacs, P., and Poggie, R.A., “Ti13Nb-13Zr: A New Low Modulus, High Strength, Corrosion Resistant, NearBeta Alloy for Orthop
45、aedic Implants,” Beta Titanium Alloys in the1990s, D. Eylon, R.R. Boyer, and D.A. Koss, eds., The Minerals,Metals and Materials Society, Warrendale, PA, 1993, pp. 6172.(2) Mishra, A.K., and Davidson, J. A., “Stress Corrosion CrackingResistance of Ti-13Nb-13Zr,” Annals of Biomedical Engineering,Vol21
46、(1), 1993, pp. 67.(3) Mishra, A.K., Davidson, J.A., Kovacs, P., and Poggie, R.A., “Mechani-cal, Tribological and Electrochemical Behavior of Ti13Nb-13ZrANew, Low Modulus Titanium Alloy for Orthopaedic Implants,” Proc.12th S. Biomedical Eng. Conf., New Orleans, LA, April 24, 1993,IEEE, Piscataway, NJ
47、, 1993, pp. 1315.(4) Goodman, S.B., Davidson, J.A., Fornasier, V.L., and Mishra, A.K.,“Histological 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,” Journal of Applied Biomate-rials, Vol 4, 1993, pp. 3
48、31339.(5) Kovacs, P., and Davidson, J.A., “The Electrochemical Behavior of aNew Titanium Alloy with Superior Biocompatibility,” Titanium 92:Science and Technology, F.H. Froes and I. Caplan, eds., The Minerals,Metals and Materials Society, Warrendale, PA, 1993, pp. 27052712.(6) FDA 510(k) No. K914343
49、.(7) FDA 510(k) No. K930480.(8) FDA 510(k) No. K936233.(9) FDA 510(k) No. K943523.SUMMARY OF CHANGESCommittee F04 has identified the location of selected changes to this standard since the last issue(F 1713 96) that may impact the use of this standard. (Approved June 10, 2003.)(1) This latest edition of F 1713 is for the periodic six-yearreview. In addition, changes were made to conform to the mostrecent template for titanium alloy standards. Changes weremade to satisfy negative votes and comments on the previousballot (F04.12 01-01). Other changes corrected
