1、Designation: F 2063 05Standard Specification forWrought Nickel-Titanium Shape Memory Alloys for MedicalDevices and Surgical Implants1This standard is issued under the fixed designation F 2063; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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, physical, me-chanical, and metallurgical requirements
3、for wrought nickel-titanium bar, flat rolled products, and tubing containing nomi-nally 54.5 % to 57.0 % nickel and used for the manufacture ofmedical devices and surgical implants.1.2 Requirements are for mill product, measuring 6 to 130mm (0.24 to 5.12 in.) diameter or thickness, in its annealedco
4、ndition.1.3 The values stated in SI units are to be regarded as thestandard. The values given in inch-pound units are for infor-mation only.2. Referenced Documents2.1 ASTM Standards:2E4 Practices for Force Verification of Testing MachinesE8 Test Methods for Tension Testing of Metallic MaterialsE112
5、Test Method for Determining Average Grain SizeE 1019 Test Method for Determination of Carbon, Sulfur,Nitrogen and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1097 Guide for Direct Current Plasma Emission Spec-trometry AnalysisE 1172 Practice for Describing and Specifying aWavelength-Dispe
6、rsive X-Ray SpectrometerE 1245 Practice for Determining the Inclusion or Second-Phase Constituent Content of Metals by Automatic ImageAnalysisE 1409 Test Method for Determination of Oxygen andNitrogen in Titanium and Titanium Alloys by the Inert GasFusion TechniqueE 1447 Test Method for Determinatio
7、n of Hydrogen inTitanium and Titanium Alloys by the Inert Gas FusionThermal Conductivity MethodE 1479 Practice for Describing and Specifying Inductively-Coupled Plasma Optical Emission SpectrometersE 1941 Test Method for Determination of Carbon in Refrac-tory and Reactive Metals and Their AlloysF 17
8、10 Test Method for Trace Metallic Impurities in Elec-tronic Grade Titanium by High Mass-Resolution GlowDischarge Mass SpectrometerF 2004 Test Method for Transformation Temperature ofNickel-Titanium Alloys by Thermal AnalysisF 2005 Terminology for Nickel-Titanium Shape MemoryAlloysF 2082 Test Method
9、for the Determination of Transforma-tion Temperature of Nickel-Titanium Shape Memory Al-loys by Bend and Free Recovery2.2 ASQ Standard:C1 General Requirements for a Quality Program33. Terminology3.1 The terminology describing the physical and thermalproperties of these alloys shall be as defined in
10、TerminologyF 2005.3.2 See also Practice E4: General Terminology.4. Product Classification4.1 BarRound bars and flats (other sizes or shapes byspecial order).4.2 PlateAny product with width equal to or greater thanfive times the thickness.4.3 TubingHollow cylindrical shapes.5. Ordering Information5.1
11、 Inquiries and orders for material under this specificationshall include the following information:5.1.1 Quantity: weight, length, or number of pieces.5.1.2 Alloy formulation, in terms of transformation tempera-ture parameter (see Section 8).5.1.3 Form: bar, plate, or tubing (see Section 4).5.1.4 Co
12、ndition (see Sections 6.3 and 10.1).5.1.5 Mechanical Properties, if applicable for special con-ditions (see Section 10).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 Metallurg
13、ical Materials.Current edition approved Nov. 1, 2005. Published November 2005. Originallyapproved in 2000. Last previous edition approved in 2000 as F 2063 00.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of
14、ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American Society for Quality (ASQ), 600 N. Plankinton Ave.,Milwaukee, WI 53203.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr H
15、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1.6 Surface Condition (see Sections 6.4).5.1.7 Applicable Dimensions, including diameter, thickness,width, and length (exact, random, multiples) or print number.5.1.8 Special Tests, for example, chemical analysis on thefinis
16、hed mill product.5.1.9 Special Requirements (see section 11).6. Manufacture6.1 The material shall be made from ingot made from nickeland titanium with no other intentional alloy additions.6.2 The material shall be vacuum or inert atmospheremelted to control metallurgical cleanliness and alloy chemis
17、try.6.3 Bar, plate, and tubing shall be supplied as hot finished orcold finished and annealed or heat treated as specified in thepurchase order.6.4 Surface condition may be oxidized, descaled, pickled,blasted, machined, ground, mechanically polished, or elec-tropolished.7. Chemical Composition7.1 Th
18、e heat analysis shall conform to the requirements ofTable 1. Ingot analysis may be used for reporting all chemicalrequirements except hydrogen. Samples for hydrogen analysisshall be taken from the finished mill product (see Section 4)oras agreed upon between the customer and supplier. Thesupplier sh
19、all not ship material that is outside the limitsspecified in Table 1.7.1.1 Requirements for major and minor elements are listedin Table 1. Important residual elements are also listed.Analysisfor elements not listed in Table 1 is not required to verifycompliance with this specification.7.2 Analytical
20、 MethodsMajor elements shall be analyzedby direct current plasma spectrometry according to GuideE 1097; atomic absorption, inductively coupled plasma spec-trometry according to Practice E 1479; X-ray spectrometeraccording to Practice E 1172; glow discharge mass spectrom-etry according to Test Method
21、 F 1710; or an equivalentmethod. Carbon shall be measured by combustion according toTest Methods E 1019 or E 1941. Hydrogen shall be measuredby inert gas fusion or vacuum hot extraction according to TestMethod E 1447. Nitrogen and oxygen shall be measured byinert gas fusion according to Test Method
22、E 1409.7.3 The titanium content of these alloys shall be determinedby difference and need not be analyzed.7.4 Product analysis limits shall be as specified in Table 2.Product analysis tolerances do not broaden the specificationheat analysis requirements, but cover variation between labo-ratories in
23、the measurement of chemical content. The manu-facturer shall not ship material that is outside the limitsspecified in Table 1.8. Transformation Temperature8.1 The nickel and titanium contents of nickel-titaniumshape memory alloys cannot be measured to a precisionrequired to guarantee shape memory or
24、 superelastic properties.Calorimetry or an equivalent thermomechanical test methodmust be used to assure the alloy formulation in terms oftransformation temperature.8.2 Alloy formulation shall be specified in terms of thetransformation temperature parameter(s) required by the pur-chase order. This p
25、arameter shall be one of the following: Mf,Mp,Ms,As,Ap,Afas defined in Terminology F 2005 and asmeasured in accordance with Test Method F 2004, Test MethodF 2082 or as measured in accordance with another appropriatethermomechanical test method.8.3 When measured in accordance with Test Method F 2004f
26、or transformation temperature by thermal analysis, theAsshallbe uniform to within the process capability of 610C on thepurchased product or as agreed upon by the customer andsupplier.8.4 Transformation temperature parameters are normallyspecified in the wrought product in the annealed condition asde
27、fined in F 2005. Other conditions for the certification of alloytransformation temperature shall be considered a special re-quirement.9. Metallurgical Structure9.1 Microstructure:9.1.1 Product shall have an average grain size number (G)of 4 or larger as measured by Test Method E 112.9.2 Microcleanli
28、ness:9.2.1 For all mill products, the maximum allowable dimen-sion of porosity and nonmetallic inclusions such as Ti4Ni2Oxand TiC particles shall be 39.0 m (0.0015 in.). Furthermore,porosity and nonmetallic inclusions shall not constitute morethan 2.8 % (area percent) of the structure as viewed at 4
29、003 to5003 in any field of view. Porosity and nonmetallic inclusionsTABLE 1 Chemical RequirementsElement % (mass/mass)Nickel 54.5 to 57.0Carbon, maximum 0.050Cobalt, maximum 0.050Copper, maximum 0.010Chromium, maximum 0.010Hydrogen, maximum 0.005Iron, maximum 0.050Niobium, maximum 0.025Nitrogen plus
30、 Oxygen, maximum 0.050TitaniumABalanceAApproximately equal to the difference between 100 % and the sum percentageof the other specified elements. The percentage titanium content by difference isnot required to be reported.TABLE 2 Product Analysis ToleranceAElement Tolerance Under the Minimum Limitor
31、 Over the Maximum Limit,% (mass/mass)BCarbon 0.002Cobalt 0.001Copper 0.001Chromium 0.001Hydrogen 0.0005Iron 0.01Nickel 0.2 under min; 0.2 over maxNiobium 0.004Nitrogen 0.004Oxygen 0.004AProduct analysis tolerance limits are based on analytical capabilities that havebeen demonstrated for this composi
32、tion.BUnder minimum limit not applicable for elements where only a maximumpercentage is indicated.F2063052shall be evaluated in mill product at a section size not largerthan 94.0 mm (3.70 in.) and not smaller than 6.3 mm (0.25 in.)in diameter, thickness, width, height, wall thickness, and soforth. M
33、easurements shall be made in accordance with PracticeE 1245 or an equivalent method with longitudinal samplesparallel to the working direction. The supplier and purchasershall agree upon the number and location of samples in theproduct, the sample preparation, the number of fields of viewand the mea
34、surement technique.10. Mechanical Property Requirements10.1 Samples from the final product, annealed so that thematerial reaches a minimum temperature of 800C for aminimum time of 15 min followed by rapid cooling by waterquenching, gas quenching, or air cooling, shall conform to themechanical proper
35、ties found in Table 3.10.2 Material may be ordered in the cold worked or heattreated condition to higher ultimate tensile strength and lowerelongation or other physical and mechanical properties asagreed upon between the supplier and purchaser.10.3 Specimens for product above 50 mm (1.96 in.) indiam
36、eter or thickness may be taken from plate or strip rolledfrom the product. For product 50 mm (1.96 in.) or less indiameter or thickness, specimens shall be made from theproduct.10.4 Tensile properties shall be measured in the longitudinaldirection with respect to the final fabrication of the sample.
37、Transverse tensile properties for wide flat products shall be asagreed upon between the customer and the supplier.10.5 Tensile testing shall be performed in accordance withTest Method E8. Tensile properties shall be those listed inTable 3 using the appropriate gage length for the product sizebeing t
38、ested.10.6 Other special mechanical tests shall be as specified onthe purchase order.11. Special Requirements11.1 Size variation and out-of-round tolerance shall bespecified in the purchase order.11.2 Special transformation temperature requirements interms of product form, test location or heat trea
39、tment shall bespecified on the purchase order.11.3 Surface roughness shall be specified on the purchaseorder.12. Certification12.1 The supplier shall provide at the time of shipment acertification that the material was manufactured and tested inaccordance with this specification. The certification s
40、hallinclude a summary of the test results for chemical composition,transformation temperature, metallurgical structure, directionof metallurgical structural analysis, and mechanical propertiesas agreed upon by the customer and supplier (see Sections 7, 8,9, and 10).13. Quality Program13.1 The suppli
41、er shall maintain a quality program such asdefined in Requirements C1.14. Keywords14.1 cardiac devices; metals; NiTi; TiNi; nitinol; nickel-titanium alloys; titanium-nickel alloys; orthopaedic medicaldevices; vascular devices; shape memory alloys; stents; super-elastic alloys; surgical implantsAPPEN
42、DIXES(Nonmandatory Information)X1. RATIONALEX1.1 The purpose of this specification is to characterize thechemical, physical, thermomechanical and metallurgical prop-erties of wrought nominally 54.5 to 57.0 % nickel-titaniumalloys to be used in the manufacture of medical devices andsurgical implants.
43、X1.2 The purchasers choice of shape memory alloytransformation temperature and mechanical properties is de-pendent upon the design and application of the medical device.X1.3 Thermo-mechanical process history, particularly coldwork and heat treatment, affects the transformation tempera-ture and other
44、 physical and mechanical properties of nickel-titanium shape memory alloys. The annealed condition stipu-lated in Sections 8.4 and 10.1 are for the test samples only.Finished product is normally purchased in the cold worked orcold worked and heat treated condition.X1.4 Ingot chemical analysis can be
45、 affected by subsequentthermo-mechanical and chemical processing. For example,pickling can result in hydrogen pick up. Therefore, hydrogen isspecified for the finished mill product (see Section 7.2).X1.5 The nickel-titanium alloys covered by this standardare commonly called nitinol alloys. Nitinol i
46、s not a single alloy,it is a family of alloys each designated by a transformationtemperature measured under controlled conditions and after aspecified thermo-mechanical history.X1.6 Transformation temperature uniformity refers to theTABLE 3 Annealed Mechanical PropertiesADiameter or DistanceBetween
47、Parallel Sides,mmTensile Strength MPa,MinimumElongation in 50 mm (2 in.)or 4 D, % MinimumBUp to 50 (1.96 in.) 551 (79.9 KSI) 15Over 50 551 (79.9 KSI) 10ATested at ambient temperature of 20.0 to 24.0C (68 to 75.2F).B4D indicates 4 times diameter.F2063053range ofAs measured on an alloy formulation tes
48、ted by a singlelaboratory working to Test Method F 2004.X1.7 The elements carbon, cobalt, copper, hydrogen, iron,niobium, and oxygen are residual elements in these alloys (seeTable 1). They are controlled to special limits in order to ensuregood shape memory physical and mechanical properties. Thepr
49、oduct analysis tolerance limits are based upon the analyticalcapabilities that have been demonstrated for thesecompositions.X2. BIOCOMPATIBILITYX2.1 The material compositions covered by this specifica-tion have been employed successfully in human implants,exhibiting a well-characterized level of local biological re-sponse since 1972. References are as follows:Castleman, L. S., et al., “Biocompatability of Nitinol Alloyas an Implant Material,” J. Biomedical Materials Research,Vol10, 1976, pp. 695731.Ryhanen, J., et al., “Biocompatability of Nickel TitaniumShape Memory Metal
