1、Designation: F 1580 07Standard Specification forTitanium and Titanium-6 Aluminum-4 Vanadium AlloyPowders for Coatings of Surgical Implants1This standard is issued under the fixed designation F 1580; 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 requirements for unalloyedtitanium and Ti-6Al-4V alloy pow
3、ders 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.2. Referenced Documents2.1 ASTM Standards:2B 214 Test Method for Sieve Analysis of Metal PowdersB 215 Practices for Sampling Metal PowdersB 299 Specification for Titanium
5、SpongeE11 Specification for Wire Cloth and Sieves for TestingPurposesE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 2371 Test Method for Analysis of Titanium and TitaniumAlloys by Atomic Emission Plasma SpectrometryF67 Specification for Unalloyed
6、Titanium, for SurgicalImplant Applications (UNS R50250, UNS R50400, UNSR50550, UNS R50700)F 981 Practice for Assessment of Compatibility of Bioma-terials for Surgical Implants with Respect to Effect ofMaterials on Muscle and BoneF 1472 Specification for Wrought Titanium-6Aluminum-4Vanadium Alloy for
7、 Surgical Implant Applications (UNSR56400)2.2 ISO Standards:3ISO 9001 Quality Management System Requirements2.3 American Society for Quality (ASQ) Standards:4ASQ C1 General Requirements for a Quality Program2.4 Aerospace Material Specifications:5AMS 2249 Chemical Check Analysis Limits, Titanium andT
8、itanium 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 been demonstrated toimprove bonding of acrylic cement to prostheses. Thisspecification addresses
9、the special requirements of the metalpowders used to form these coatings.4. Methods of Manufacture4.1 Powders may be manufactured by the plasma rotatingelectrode process, inert gas atomization, hydride-dehydride, orother method capable of producing powder meeting the re-quirements of this specificat
10、ion.5. Chemical Requirements5.1 The chemical analysis of the powder shall conform tothe requirements specified in Table 1.5.1.1 Requirements for the major and minor elementalconstituents for unalloyed titanium and Ti-6Al-4V alloy pow-ders are listed in Table 1. Also listed are all important residual
11、elements. Analysis for elements not listed in Table 1 is notrequired to verify compliance with this specification.5.2 The product analysis tolerance shall conform to therequirements set forth in Table 2.5.3 For referee purposes, Test Method E 2371 shall be used.5.4 Intentional elemental additions ot
12、her than those speci-fied in Table 1 are not permitted.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 Dec. 1, 2007. Publi
13、shed December 2007. Originallyapproved in 1995. Last previous edition approved in 2001 as F 1580 - 01.2For 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
14、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 American Society for Quality (ASQ), 600 N. Plankinton Ave.,Milwaukee, WI 53203, http:/www.asq.org.5Available from So
15、ciety of Automotive Engineers (SAE), 400 CommonwealthDr., Warrendale, PA 15096-0001, http:/www.sae.org.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.Copyright by AST
16、M Intl (all rights reserved); Fri Feb 22 00:30:33 EST 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.5.5 For powder that includes particle size fractions finerthan 200 mesh (74 m), the oxygen content limits shall beagreed upon between buy
17、er and seller.6. Particle Size6.1 Powder shall be sieved to the customers 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 B 214.7. Cleanliness7.1
18、 Powder shall be handled at all times so as to ensurefreedom from contamination with nonmetallic materials orother metal alloy powders or both.7.2 Powder cleanliness shall be determined by examining arepresentative sample, per Practices B 215 or as agreed uponbetween buyer and seller, comprising at
19、least 1 in.2(6.45 cm2)of a closely packed mono-layer of powder per lot at 203magnification. No foreign material shall be visible under theseconditions.8. Significance of Numerical Limits8.1 The following applies to all specified numerical limits inthis specification. To determine conformance to thes
20、e limits, anobserved or calculated value shall be rounded to the nearestunit in the last right hand digit used in expressing thespecification limit, in accordance with the rounding method ofPractice E29.9. Certification9.1 Powder shipped under this specification shall be accom-panied by certificatio
21、n that includes:9.1.1 ASTM designation and date of issue.9.1.2 Quantity (weight).9.1.3 Method of manufacture.9.1.4 Chemical analysis per 5.1.9.1.5 Sieve analysis per 6.1.9.1.6 Powder cleanliness per 7.2.9.1.7 Other requirements.10. Quality Program Requirements10.1 The supplier shall maintain a quali
22、ty program, such asthat defined in the ASQ C1 or ISO 9001, for example.10.2 The purchaser shall be ensured of the suppliers qualityprogram for conformance to the intent of ASQ C1 or otherrecognized programs.11. Keywords11.1 coatings; metallic; metals (for surgical implants tita-nium alloys); orthopa
23、edic medical devices (titanium/titaniumalloys); powder; porous coatings; titanium/titanium alloys (forsurgical implants)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
24、.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 0.005CTi balanceGbalanceGbalanceGAChemistry per Specification F67except hydrogen.BChemistry per Specification B 299, general purpose grade.CChemistry per Specification F 1472.DOxygen per
25、Specification B 299 is 0.15 %. This level is reasonable for spongeproduct but not for powder because of the increased surface area of small particlepowder product.ELower maximum chlorine content may be agreed upon between buyerpurchaser and seller supplier.FSodium or magnesium, 0.50 maximum.GThe per
26、centage of titanium is determined by difference and need not bemeasured.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 0.0005CAR
27、efer to AMS 2249.BFor unalloyed Ti powder.CFor Ti-6Al-4V alloy powder.F1580072Copyright by ASTM Intl (all rights reserved); Fri Feb 22 00:30:33 EST 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.APPENDIXES(Nonmandatory Information)X1. RAT
28、IONALEX1.1 Coatings formed from metallic powders have becomewidely used as a means of improving tissue attachment touncemented orthopedic joint prosthesis. Such coatings havealso been demonstrated to improve bonding of acrylic cementto prostheses.X1.2 The biocompatibility of metallic implants is a d
29、irectfunction of their composition. The compositions of titaniumand titanium alloy powders allowed by this specification havebeen used in wrought form for surgical implants and are inwidespread commercial use for fabrication of porous coatings.X1.3 Chemical composition limits for oxygen, iron, car-b
30、on, and nitrogen in the unalloyed grade are taken fromSpecification F67, Grade 4. Limits for silicon, chlorine,hydrogen, and sodium are taken from Specification B 299,Grade SL.X1.4 Chemical composition limits for aluminum, vana-dium, oxygen, iron, carbon, hydrogen, and nitrogen in theTi-6Al-4V grade
31、 are taken from Specification F 1472. Limitsfor copper and tin are taken from AMS 4998.X1.5 Product analysis tolerances are taken directly fromAMS 2249. No recognized product analysis tolerances cur-rently exist specifically for chlorine or sodium in titaniumalloys.X1.6 Processing aids are frequentl
32、y used to facilitatepowder processing and application of porous coatings toimplant surfaces. It is beyond the scope of this specification toidentify suitable processing aids or define their use. It is theresponsibility of the implant manufacturer to ensure that anyprocessing aid or residue of a proc
33、essing aid has no detrimentaleffect on biocompatibility or coating properties.X1.7 It should be recognized that the heat treatments usedto form porous coatings can create microstructures that aresubstantially different from wrought titanium alloys. Porouscoated implants also exhibit much greater sur
34、face area thanmonolithic implants. For these reasons, the biocompatibilityand corrosion behavior must be characterized on finishedcoatings.X1.8 Likewise, these heat treatments can create microstruc-tures that give substantially different corrosion fatigue behaviorfrom that of typical wrought titaniu
35、m alloys. Corrosion fatiguebehavior must be evaluated on finished coated substrates.X1.9 Pore size and morphology are important factorsinfluencing tissue ingrowth and acrylic penetration of porouscoatings. Particle size, size distribution, and shape are criticalto controlling the pore size and morph
36、ology in the finalcoating. Particle size and size distribution are conventionallycontrolled by screening. The referenced ASTM Internationalstandards allow comparison of powder to a manufacturersspecifications for a given coating process. A number ofmethods to characterize particle shape exists. The
37、coatingmanufacturer should select a means of particle shape charac-terization suitable for this process.X1.10 This specification requires sampling for particle sizeand powder cleanliness on each powder lot. In some cases,sampling on each shipping container of powder may beappropriate.X1.11 Other pro
38、cess 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 physical characteristics of the starting powder,they are not addressed in this specification.X1.12 The requirements for powder cl
39、eanliness ensurefreedom from contaminants that might adversely affect eitherthe biocompatibility or the finished coatings or the ability tobond the coating properly during manufacturing. The methodin 7.2 (Practices B 215) is commonly used for relatively coarsespherical powders used to fabricate sint
40、ered 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 hist
41、ory of successful clinical application in softtissue and bone implants in humans, with a well-characterizedlevel of biological response.X2.2 No known surgical implant material has ever beenshown to be completely free from adverse reactions in thehuman body. Long-term clinical experience of the use o
42、f thematerial referred to in this specification, however, has shownthat an acceptable level of biological response can be expected,if the material is used in appropriate applications.F1580073Copyright by ASTM Intl (all rights reserved); Fri Feb 22 00:30:33 EST 2008Downloaded/printed byGuo Dehua (CNI
43、S) pursuant to License Agreement. No further reproductions authorized.SUMMARY OF CHANGESCommittee F04 has identified the location of selected changes to this standard since the last issue(F 1580 01) that may impact the use of this standard. (Approved Dec. 1, 2007.)(1) Test Methods E 120 is replaced
44、with Test Method E 2371in 2 and 5.3.(2) Section 8 was renamed to Significance of NumericalLimits.(3) Added 1.4 in Section 1.(4) Added ISO 9001 in Section 2 and Section 10.(5) Removed 9.1.7 in Section 9.(6) Updated reference to American Standard for Quality inSection 2.(7) AMS 4998A Powder 6Al-4V Pre
45、mium Quality (non con-current) has been cancelled in 2002. AMS 4998C is the currentstandard. AMS 4998C states a maximum tin and coppercontent of 0.10 wt %. Subsections 2.4 and X1.4 were updated.(8) The iron content was reinstated to 0.30 wt % max in Table1.(9) The reference to processing aids was re
46、moved in subsec-tion 7.2 and Section 8.(10) Added E29to subsections 2.1 and 8.1(11) Section 6, footnote E, Table 1 the words “buyer “ and“seller” were updated to “purchaser” and “supplier”.(12) Subsection 7.2, the words “buyer” and “seller” wereupdated to “purchaser” and “supplier”.(13) Subsection 1
47、0.1, the word “producer” was updated to“supplier”.(14) Subsection X1.9, removed the reference to MPIF stan-dards.(15) Subsection X2.1, removed the reference to F 981 andrestated.(16) Section Appendix X2, the phrase “For CONTROL AL-LOYS” was removed.(17) Table 1, yttrium callout of 0.005 wt % inserte
48、d for Ti 6Al4V powder. Yttrium callout inserted in Table 2.(18) Table 1, carbon content callout changed to 0.08 wt % forthe unalloyed titanium powder as referenced in X1.3 andSpecification F67Grade 4.(19) Subsection 5.1, the statement “Analysis shall be per-formed before the addition of any processi
49、ng aids” wasremoved.ASTM International takes no position respecting the validity of any patent rights asserted in connection 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 responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision o
