1、Designation: F1580 18Standard Specification forTitanium and Titanium-6 Aluminum-4 Vanadium AlloyPowders for Coatings of Surgical Implants1This standard is issued under the fixed designation F1580; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 of revision, the 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. Scope*1.1 This specification covers the requirements for unalloyedtitanium and Ti-6Al-4V alloy powder
3、s for use in fabricatingcoatings on titanium alloy implants.1.2 Powders covered under this specification may be used toform coatings by sintering or thermal spraying techniques.1.3 This specification covers powder requirements only. Itdoes not address properties of the coatings formed from them.1.4
4、Finely divided titanium powder may be consideredpyrophoric and should be handled in accordance with theappropriate guidelines.1.5 UnitsThe values stated in either SI units or inch-pound units are to be regarded separately as standard. Thevalues stated in each system may not be exact equivalents;ther
5、efore, each system shall be used independently of the other.Combining values from the two systems may result in non-conformance with the standard.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on
6、 Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2B214 Test Method for Sieve Analysis of Metal PowdersB215 Practices for Sampling Metal Po
7、wdersB299 Specification for Titanium SpongeE11 Specification for Woven Wire Test Sieve Cloth and TestSievesE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE2371 Test Method for Analysis of Titanium and TitaniumAlloys by Direct Current Plasma and Indu
8、ctively CoupledPlasma Atomic Emission Spectrometry (Performance-Based Test Methodology)F67 Specification for Unalloyed Titanium, for Surgical Im-plant Applications (UNS R50250, UNS R50400, UNSR50550, UNS R50700)F981 Practice for Assessment of Compatibility of Biomate-rials for Surgical Implants with
9、 Respect to Effect ofMaterials on Muscle and Insertion into BoneF1472 Specification for Wrought Titanium-6Aluminum-4VanadiumAlloy for Surgical ImplantApplications (UNSR56400)IEEE/ASTM SI 10 American National Standard for MetricPractice2.2 ISO Standards:3ISO 9001 Quality Management System Requirement
10、s2.3 Aerospace Material Specifications:4AMS 2249 Chemical Check Analysis Limits, Titanium andTitanium AlloysAMS 4998 Powder, 6Al-4V3. Significance and Use3.1 Coatings formed from metallic powders have becomewidely used as a means of improving tissue attachment toimplants. Such coatings have also bee
11、n demonstrated toimprove bonding of acrylic cement to prostheses. Thisspecification addresses the special requirements of the metalpowders used to form these coatings.4. Ordering Information4.1 Include with inquiries and orders for material under thisspecification the following information:4.1.1 Qua
12、ntity (weight),4.1.2 ASTM specification and date of issue,1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is under the direct responsibility ofSubcommittee F04.12 on Metallurgical Materials.Current edition approved Nov. 15, 2018. P
13、ublished December 2018. Originallyapproved in 1995. Last previous edition approved in 2012 as F1580 - 12. DOI:10.1520/F1580-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information
14、, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from Society of Automotive Engineers (SAE), 400 CommonwealthDr., Warrendale, PA 15096-0001, http
15、:/www.sae.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standa
16、rdization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.1.3 Method of ManufactureType of powder (un-alloyed,sponge or Ti-6Al-4V),4.1.4 Units to
17、be CertifiedSI or inch-pound,4.1.5 Sieve analysis per 7.1,4.1.6 Powder cleanliness per 8.2,4.1.7 Special tests, if any, and4.1.8 Other requirements.5. Methods of Manufacture5.1 Powders may be manufactured by the plasma rotatingelectrode process, inert gas atomization, hydride-dehydride, orother meth
18、od capable of producing powder meeting the re-quirements of this specification.6. Chemical Requirements6.1 The chemical analysis of the powder shall conform tothe requirements specified in Table 1.6.1.1 Requirements for the major and minor elementalconstituents for unalloyed titanium and Ti-6Al-4V a
19、lloy pow-ders are listed in Table 1. Also listed are all important residualelements. Analysis for elements not listed in Table 1 is notrequired to verify compliance with this specification.6.1.2 All commercial metals contain small amounts ofelements other than those which are specified. It is neithe
20、rpractical nor necessary to specify limits for unspecifiedelements, whether residual elements or trace elements. Theproducer is permitted to analyze for unspecified elements andis permitted to report such analyses. The presence of anunspecified element and the reporting of an analysis for thatelemen
21、t shall not be a basis for rejection.6.1.3 Intentional elemental additions other than those speci-fied in Table 1 are not permitted.6.2 Product Analysis:6.2.1 The product analysis tolerance shall conform to therequirements set forth in Table 2.6.3 For referee purposes, Test Method E2371 shall be use
22、d.6.4 Intentional elemental additions other than those speci-fied in Table 1 are not permitted.6.5 For powder that includes particle size fractions finerthan 74 m (200 mesh), the oxygen content limits shall beagreed upon between buyer and seller.7. Particle Size7.1 Powder shall be sieved to the cust
23、omers requirementswith stainless steel screens conforming to Specification E11.Analysis of sieved powder for conformance to the customersparticle size range requirements shall be in accordance withTest Method B214.8. Cleanliness8.1 Powder shall be handled at all times so as to ensurefreedom from con
24、tamination with nonmetallic materials orother metal alloy powders or both.8.2 Powder cleanliness shall be determined by examining arepresentative sample, per Practices B215 or as agreed uponbetween buyer and seller, comprising at least 6.45 cm2(1 in.2)of a closely packed mono-layer of powder per lot
25、 at 20magnification. No foreign material shall be visible under theseconditions.9. Dimensions and Permissible Variation9.1 Units of Measure:9.1.1 SelectionThis specification requires that the pur-chaser selects the units (SI or inch-pound) to be used forproduct certification. In the absence of a sta
26、ted selection ofunits on the purchase order, this selection may be expressed bythe purchaser in several alternate forms listed in order ofprecedence.9.1.2 If the purchaser and supplier have a history of usingspecific units, these units shall continue to be certified untilexpressly changed by the pur
27、chaser.TABLE 1 Chemical RequirementsElementUnalloyedTi PowderA% (mass/mass)Ti SpongePowderB% (mass/mass)Ti-6Al-4VPowderC% (mass/mass)Min Max Min Max Min MaxAl 0.05 5.50 6.75V 3.50 4.50O 0.40 0.40D0.20Fe 0.50 0.15 0.30C 0.08 0.03 0.08H 0.05 0.03 0.015N 0.05 0.02 0.05Cu 0.10Sn 0.10Si 0.04Cl 0.20ENaFY
28、0.005CTi balanceGbalanceGbalanceGAChemistry per Specification F67 except hydrogen.BChemistry per Specification B299, general purpose grade.CChemistry per Specification F1472.DOxygen per Specification B299 is 0.15 %. This level is reasonable for spongeproduct but not for powder because of the increas
29、ed surface area of small particlepowder product.ELower maximum chlorine content may be agreed upon between buyer purchaserand seller supplier.FSodium or magnesium, 0.50 maximum.GApproximately equal to the difference of 100 % and the sum percentage of theother specified elements. The percentage of th
30、e titanium difference is not requiredto be reported.TABLE 2 Product Analysis TolerancesAElement Element Variation Under Min or OverMaxAluminum 0.04Vanadium 0.015Oxygen 0.03BOxygen 0.02CHydrogen 0.002Iron 0.10Carbon 0.02Nitrogen 0.02Copper 0.05Tin 0.15Silicon 0.02Yttrium 0.0005CARefer to AMS 2249.BFo
31、r unalloyed Ti powder.CFor Ti-6Al-4V alloy powder.F1580 1829.1.3 In the absence of historic precedence, if the units usedto define the product on the purchasers purchase order,specification, and engineering drawing are consistent, theseunits shall be used by the supplier for product certification.9.
32、1.4 If the purchasers selection of units is unclear, theunits of measure shall be agreed upon between the purchaserand supplier.9.1.5 Conversion of UnitsIf the suppliers test equipmentdoes not report in the selected units, the test equipment unitsmay be converted to the selected units for certificat
33、ion pur-poses. Accurate arithmetic conversion and proper use ofsignificant digits should be observed when performing thisconversion. IEEE/ASTM SI 10 provides guidelines for the useof SI units.AnnexAof IEEE/ASTM SI 10 provides conversiontables and Annex B of IEEE/ASTM SI 10 provides rules forconversi
34、on and significance.10. Significance of Numerical Limits10.1 The following applies to all specified numerical limitsin this specification. To determine conformance to these limits,an observed or calculated value shall be rounded to the nearestunit in the last right hand digit used in expressing thes
35、pecification limit, in accordance with the rounding method ofPractice E29.11. Certification11.1 The supplier shall provide a certification that thematerial was tested in accordance with this specification andmet all requirements. A report of the test results shall befurnished to the purchaser at the
36、 time of shipment.12. Quality Program Requirements12.1 The supplier shall maintain a quality program, such asthat defined in ISO 9001 or similar quality program.13. Keywords13.1 coatings; metallic; metals (for surgical implants tita-nium alloys); orthopaedic medical devices (titanium/titaniumalloys)
37、; powder; porous coatings; titanium/titanium alloys (forsurgical implants)APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 Coatings formed from metallic powders have becomewidely used as a means of improving tissue attachment touncemented orthopedic joint prosthesis. Such coatings havealso been
38、 demonstrated to improve bonding of acrylic cementto prostheses.X1.2 The biocompatibility of metallic implants is a directfunction of their composition. The compositions of titaniumand titanium alloy powders allowed by this specification havebeen used in wrought form for surgical implants and are in
39、widespread commercial use for fabrication of porous coatings.X1.3 Chemical composition limits for oxygen, iron, carbon,and nitrogen in the unalloyed grade are taken from Specifica-tion F67, Grade 4. Limits for silicon, chlorine, hydrogen, andsodium are taken from Specification B299, Grade SL.X1.4 Ch
40、emical composition limits for aluminum,vanadium, oxygen, iron, carbon, hydrogen, and nitrogen in theTi-6Al-4V grade are taken from Specification F1472. Limitsfor copper and tin are taken from AMS 4998.X1.5 Product analysis tolerances are taken directly fromAMS 2249. No recognized product analysis to
41、lerances cur-rently exist specifically for chlorine or sodium in titaniumalloys.X1.6 Processing aids are frequently used to facilitate pow-der processing and application of porous coatings to implantsurfaces. It is beyond the scope of this specification to identifysuitable processing aids or define
42、their use. It is the responsi-bility of the implant manufacturer to ensure that any processingaid or residue of a processing aid has no detrimental effect onbiocompatibility or coating properties.X1.7 It should be recognized that the heat treatments used toform porous coatings can create microstruct
43、ures that aresubstantially different from wrought titanium alloys. Porouscoated implants also exhibit much greater surface area thanmonolithic implants. For these reasons, the biocompatibilityand corrosion behavior must be characterized on finishedcoatings.X1.8 Likewise, these heat treatments can cr
44、eate microstruc-tures that give substantially different corrosion fatigue behaviorfrom that of typical wrought titanium alloys. Corrosion fatiguebehavior must be evaluated on finished coated substrates.X1.9 Pore size and morphology are important factors influ-encing tissue ingrowth and acrylic penet
45、ration of porouscoatings. Particle size, size distribution, and shape are criticalto controlling the pore size and morphology in the finalcoating. Particle size and size distribution are conventionallycontrolled by screening. The referenced ASTM Internationalstandards allow comparison of powder to a
46、 manufacturersspecifications for a given coating process. A number ofmethods to characterize particle shape exists. The coatingmanufacturer should select a means of particle shape charac-terization suitable for this process.X1.10 This specification requires sampling for particle sizeand powder clean
47、liness on each powder lot. In some cases,sampling on each shipping container of powder may beappropriate.F1580 183X1.11 Other process parameters are also critical to deter-mining final pore size and morphology in the final coating.Because these parameters are not directly related to thechemical and
48、physical characteristics of the starting powder,they are not addressed in this specification.X1.12 The requirements for powder cleanliness ensure free-dom from contaminants that might adversely affect either thebiocompatibility or the finished coatings or the ability to bondthe coating properly duri
49、ng manufacturing. The method in 8.2(Practices B215) is commonly used for relatively coarsespherical powders used to fabricate sintered porous coatings.Other types of powders may require different methods forcleanliness characterization. The development and implemen-tation of such methods are the responsibility of the implantmanufacturer.X2. BIOCOMPATIBILITYX2.1 The alloy composition covered by this specificationhas a long history of successful clinical application in softtissue and bone implants in humans, with a well-characterizedlevel of biological response.X2.2 No
