Standard Specification forAutocatalytic (Electroless) Nickel-Phosphorus Coatings on Metal ' Thrs standard is lrsued under h e fired deri%mrionB 733: the numbcr irnmcdialcly f o l i o r i n ~!he drri~mationindica~esthe ycnr of original adoption or, in the case ofrevision, the year of larl revlson. A number in parentheses indicales the year af larl reapproval. A superscript cprilo~l(E) ind~cvtesan edilorial chanee since Ule l a s ~revision or reapproval. Tlii, s,o,rdord hm bee,, ',~,~rol.i.d /or ,,sc hl. ogn~cicr"/ihc Dcpornneni o/Defeme 1. Scope 1. I This specification covers requirements for autocatalytic (electroless) nickel-phosphorus coatings applied from aqueous solutions to metallic products for engineering (functional) uses. 1.2 The coatings are alloys of nickel and phosphorus pro-duced by autocatalytic chemical reduction with hypophosphite. Because the deposited nickel alloy is a catalyst for the reaction, tlie process is self-sustaining. The chemical and physical properties of the deposit vary primarily with its phosphorus content and subseque~itheat treatment. The chemical makeup of the plating solution and the use of the solution can affect tlie porosity and col~osionresista~iceof the deposit. For more details, see S T M STP 265 (1)' and Refs (2) (3) (4) and (5) also refer to Figs. XI.1, Figs. X1.2, and Figs. XI.: in the Appendix of Guide B 656. 1.3 The coatings are generally deposited from acidic solutions operating at elevated temperatures. 1.4 The process produces coatings of uniform thickness on il~egularlyshaped parts, provided tlie plating solution circulates freely over tlieir surfaces. 1.5 The coatings have multifunctional properties, such as hardness, heat hardenability, abrasion, wear and col~osion resistance. magnetics, electrical conductivity p~ovidediffusion barrier, and solderability. They are also used for the salvage of '.om or mismachined parts. 1.6 The low phosphorus (2 to I % P) coatings are microcrystalline and possess high as-plated hardness (620 to 750 HK 100). These coatings are used in applications requiring abrasion and wear resistance. 1.7 Lower phosphorus deposits in the range between 1 atid 3 % phosphorus are also microcrystalline. These coatings axe used in electronic applications providing solderability, bondability, increased electrical conductivity, and resistance to strong alkali solutions. * ' This ipec~ficalionis under the jurisdiction of ASTM Commillce 8-08 on Melal Pordcrr and Mesa1 Powder Produca and is the direct rcipo~ir~blllry of Subcommillee B06.08.01 on Englneenng Coatings C u n m , cdition approved July 10. 1997. Published October 1997. Oiiginally published as B 713 - 81 Last prevlour edition B 733 - 90 (19941. 'The boldfac, numbrrr in rercr lo a lis1 of references 0 , ,hr end of rhe ex,. l .8 The medium phosphorous coatings (5 to 9 % P) are most widely used to meet the general purpose requirements of wear and corrosion resistance. 1.9 The high phosphorous (more than 10 % P) coatings have superior salt-spray and acid resistance in a wide range of applications. They are used on beryllium and titanium parts for low stress properties. Coatings with phosphorus contents greater than 11.2 % P are not considered to be ferromagnetic. 1.10 The values stated in S1 units are to be regarded as standard. 1.11 The following precautionary statement pertains only to the test method ponion, Section 9, of this specification. T11is s m ~ ~ d adoes r d n o r p u r p o r ~ro nddress a l l o/rhe sq/erv concerns. i/ar??, associo~edwiih ils use. 11 IS rhe responsibilip o/lhe user of lhis sla~ldnrd10 eslnblish appropriare sa/e(v and Ircnlfh pracrices and delern~inethe applicabili~yo/regula~oo;iintirario17sp,-ior lo use. 2. Referenced Documents 2.1 ASTM Sra~~dards: B 368 Test Method for Copper-Accelerated Acetic AcidSalt Spray (Fog) Testing (CASS Testing)' B 374 Terminology Relating to Electroplating3 B 380 Test Method of Corrosion by the Corrodkote Procedure3 B 487 Test Method for Measurement of Metal and Oxide Coating Thicknesses by Microscopical Examination of a Cross Section' B 199 Test Method for Measurement of Coating Thicknesses by the Magnetic Method: Nonmagnetic Coatings on Magnetic Basis Metals3 B 504 Test Method for Measurement of Thickness of Metallic Coatings by the Coulometric Method3 B 537 Practice for Rating of Electroplated Panels Subjected to Atmospheric Exposure' B 567 Method for Measurement of Coating Thickness by the Beta Dackscatter ~ e t h o d ~ B 568 Method for Measurement of Coating Thickness by X-Ray Spectrometry3 '.l!a>i,oIBook o j l S T A 4 Yundords, Vol 020S Copyrlghl OASTM International 100 Ban Harbor Dive. PO Box C100. Wart CmnrhMosXen PA 19428-2959, United Slales "' Dirconun8.4.4n. 0. 01 -iSTW S.2.ai:abIe from Amencan Nacianai Standarb Inrtitule. \'a1 15. W. 13th . Book 01 ASTM Srundordr.ides for a scheme to select an electroless nickel coating to meet specific performance requirements based on alloy composition.1 TYPE describes tlie general composition of the deposit with respect to the phosphorus content and is divided into five categories which establish deposit properties (see Table 1). Val 09. \lo1 02. Norr ]-Due la the preciscan of some phosphorus analysis methods a deviation of 0. '..~Sta17dar. Terminology 3.7 %would have a classification of TYPE V.0 1 Val 05.1 The coating classification system pro\.000004 ( 0.4!i??<rI Book of. NY 10036.1. 700 Robbinr Ave.0005 0. 1.4STM Sinndords.0002 ( ) J SC2 Mild Service Moderate Service Severe Service 13 25 75 0. or both. or As A Final Finish3 D 1193 Specification for Reagellt Wale9 D 2 6 7 0 Method for Measuring Wear Properties of Fluid Luhricants Methodi6 .ondord:.2 144ilira1.02. 4. Rounding aflhe lest rerulls due lo the precision of the limits provider for an effective limit of 4.-r. Allay TYPES.1 D. Vol 06.1 m-This is defined by a minimum coatine thickness lo erovide soecific material oroo.04.4nri?rol Book o/ASTM Slundords.B 571 Test Methods for Adhesion of Metallic Coatings3 8 578 Test Method for Microhardness o f Electroplated Coatings3 B 602 Test Method for Attribute Sampling of Metallic and Inorganic Coating" B 656 Guide for Autocatalytic Nickel-Phosphorus Deposition on Metals for Eneineerine Use3 B 667 Practice for Cot%uctio. Vol 0J. 42nd SI..1 5 0. Blda 4 Seclion D.2 SCO hlinimunt Se. 4. PA 19111-5094.?dordr. Autocatalytic Nickel. and Use o f a Probe for Measuring Electrical Contact Resistance" B 678 Test Method for Solderability of Metallic-Coated Products' B 697 Guide for Selection of Sampling Plans for Inspection of Electrodeposited Metallic and lnorganic Coatings" B 762 Method for Variable Sampling of Metallic and Inorganic Coating? B 849 Specification for Pre-Treatment of Iron or Steel for Reducing the Risk of Hydrogen Embrinlement3 B 850 Specification for Post-Coating Treatments of lron or Steel f i r Reducing the Risk o f Hydrogen Embrittlement3 B 85 1 Specification for Automated Controlled Shot Peening of Metallic Articles Plior to Nickel. Applications - " ''A\. \bl " in3rr101 Book of. see 1992 Ann~rnlBook oJASTM Siondards.1 Service condition numbers are based on the severity of the exposure in which the coating is intended to perform and minimum coating thickness to provide satisfactory performance (see Table 2).ilijtol Book 'Aari.osdnrdr.5 and 9.4STMSiondordr. 1 significant sur/aces-those substrate surfaces which the coating must protect from corrosion or wear. erties and extend the life o f a pan or its function.ruI 3.5 4h has been designed inra !his classificalion scheme. '. Ann: WODS.2. " Anrilrol Book o/lSTMSio. thickness and hardness. I 1 Floor.DeF~litions-Teminolo B 374 defines most of the technical terms used in this specification. . and that are essential to the perfomlance. 4. Coating Classification 4.d~: MIL-R-81841 Rotary Flap Peening of Metal PartsI3 TABLE 1 Deposit Alloy Types Type P h o ~ p h o w%~~t I Nil Requiremen1 for Phosphorus II I 103 111 2 io 4 5 to 9 10 and above IV v TABLE 2 Service Conditions Coating Thickness Requirements Mtn8mum Coaling Thickness SpeciScauon Condllon ~rm in (mm) SCO SCI Minlrnun Thickness Light Service 0. Philadelphia.Vol 03.03 . Chromium.05. ' .~~(Falex ~~ .01 9 A r i r l ~ o Bovl i ~JiSJMSrondords.001 0003 ( [ ) ) ( ) sc3 SC4 MIL-S-13 165 Shot Peening of Metal PartsI3 MIL-STD-105 Sampling Procedures and Tables for lnspection by AttributeI3 2. 11. see Appendix X?.moi Book q/ASTM S. coaling with 3 rest resull for phosphorus of 9.2 Orher.ice. New York. D 2714 Method for Calibration and Operation of an Alplia LFW-I Friction and Wear Testing Machine6 D 1951 Practice for Commercial Packaging' D 4060 Test Method for Abrasion Resistance of Organic Coatings by tlie Taber ~ b r a s e r ' E 60 Practice for Photometric h4ethods for Chemical Analysis of Metals9 E 156 Test Metliod for Determinatio~i of Phosphorus in Higll-Phosphorus Brazing Alloys (Photometric Met11od)'~ E 352 Test Methods for Chemical Analysis of Tool Steels and Other Similar Medium-and High-Alloy Steel9 F 519 Test Method for Mechanical Hydrogen Embrinlementll G 5 Practice for Standard Reference Method for Making Pote~itiostaticand Potentiodynamic Anodic Polarization Measurements" G 3 1 Practice for Laboratory l ~ n n ~ e r s i oCorrosion n Testing of Metals" G 59 Practice for Conducting Potentiodynamic Polarizatio~i Res~stanceMeasurements" G 85 Practice for Modified Salt Spray (Fog) Testing" 2. Far example.02.3 IS0 Standards: 1SO 4527 Autocatalytic Nickel-Phosphorus CoatingsSpecification and Test Methods" ~ ~ .efini/io~i: 3 1 .02.ed. 4.5 % respecti\. " Available from Standard~acianDocumcnli Ordm Desk.2 Service Corldirion Based art T/ticX7tess: 4.05.ely. Vol 03. thickness of 5 pm for extending the life of the part. roll and die marks. no heat treannent.11 T ~ ~ ~ ~ . d 13 W-This is defined by mild corrosion and wear environments.2. wear and corrosion resistance..3. and year ofissue of this specification.6). hydrogen ulfide and carbon dioxide oil service. Adesignation STM number.2. inert or reducing atmosphere for heat treatment above 260°C to prevent surface oxidation of the coating (see S3).3 Posr Hear Pear1ne111 Class-The nickel-phosphorus coatings shall be classified by heat treamient after plating to increase coating adhesion and or hardness (see Table 3).5).1 S~~bslrare-Defects in the surface of the basis metal such as scratches. non agehardened aluminum alloys. copper. non uniform surfaces require thicker coutinxs than smootll surfaces to achieve maximum corrosion resistance and minimum porosiry 4. if any. NOTE&The pnrchaser should furnish separate lesl specimens or coupons of rhe basis metal for lest purposes to be plated coneunentiy with the artieles la be plated (see 8.1. very severe wear.1.1.. 5. elevated temperature and pressure. despite the obser\. 51. solderability.6 Class 6-Heat treatment at 300 to 320°C for at least 1 h to improve coating adhesion for titanium alloys. service condition.3 S C l Light Ser?'ice. 5 1 .3. electrical co~~ductivity and wear and corrosion protection in specialized environments. liigll-temperature chloride systems.2 P. Careful selection of the pre and past heal treatments are recommended. if required (see 6.4 Class 4-Heat treatment at 120 to 130DCfor at least 1 h to increase adhesion of heat-treatable (age-hardened) aluminun) alloys aud carburized steel (see Note 3).4 SC2 ~ i l Service. 4. indoor corrosion protection to prevent rusting. 6. (see 6. 5 wpThisis minimum coating . Rough. copper alloys and berylliutn.1 4 Peening. Ordering Information 5. NOTE ?-The performance af the autacatalytic nickel coating depends ra a large errent on rbe surface finish of t h e article to be plated and lrow it was prelreated. and marine immersion.6 SC4 Severe Sen~ice.6 Hydrogen Embrittlernent Relief after plating. class.6). 5.10 Test methods for coating adhesion.1. a 4..i to improve coating adhesion for aluminum. 4.11 Requirements for sampling (see Section 8).3 C1as. and roughness may adversely affect the appearance and performance of tlie deposit. thickness.5 SC3 Moderare Service.Typical environments would include acid solutions.include requirements for diffusion barrier. 5. undercoat. Typical environments include light-load lubricated wear. - ro over ~~~ 5.1 Tlie following informati011 shall be supplied by The purchaser in either the purchase order or on the engineering drawing of the pan to be plated: 5. pits. selected from those found in Section 9 and Supplemental Requirements.3. A suitable method shall activate tlie surface and remove oxide and foreign materials. TABLE 3 1 Post Heat Treatment Oe~cription CLRSS 2 Classification of Temperature xme (hl i°Cl No HealTrealment. As Plated Heal Treatment for Maximum Hardness TYPE I 260 285 320 n nn TYPE I 1 TYPE I l l TYPE IV TYPF V 3 4 5 Hydmgen Embriniemenl and Adhesion on Sleel Adhesion. cold shuts. laps. and for soldering and mild abrasive wear.5 Class 5-Heat treatment at 110 to 150°C for at least I . composition. 6 .1. porosity.r 3-Heat treatment at 180 to 200°C for 2 to 4 11 to improve coating adhesion on steel and to provide for hydrogen embrittlement relief (see section 6. if these conditions have been brought to the attention of the purchaser. 4. An example is leaded steel which may exhibit liquid or ernbrittlemen1 afrer heal treatment. 4. The producer shall not be responsible for coatings defects resulting from surface conditions of the metal..5 Stress relief heat treatment before plating.4). and moderate wear. 25 pm-This is defined by moderate environments such as non marine outdoor exposure. NOTE3-Heal-treatable aluminum alloys such as Type 7075 can undergo micrortructu~vl changes and lose strength =.3).1.2 Class 2-Heat treatment at 260 to 400°C to produce a minimum hardness of 850 HK100. 5. specific phosphorus content. if required. Materials and Manufacture 6.1.2. 4.er~eamte~il--Pansto be autocatalytic nickel plated may be pretreated in accordance with Guide B 656. burrs. contact resistance and packaging selected from Supplemental Requirements.2 Classification of the deposit by type. cracks. 4.ance of the best plating practice. 4. Carburized Steel and Age Hardened Aluminum Adherlo" on Beryllium and 180 to 200 12010 130 140 to 150 1 to 2 30C~320 14 Aluminum 6 Adhesion on Xlanium 4. It is characterized by industrial atmosphere exposure on steel substrates in d~ or oiled environments. which may cause poor adhesion and coating porosity. NOTE5-Heat eical solid .3. porosity.2. Any such defects on significant surfaces shall be brought to the attention of the purchaser before plating. 5.: l Class I-As-deposited. treatment of the base material may effecr its metallurproperties.hen licarcd 130-c.3.3) 5 1 .75 pm-This is defined by a very aggressive enviro~lment. (see 6.9 Requirement for a vacuum. alkali salts at elevated temperature. 5. 8 Suppletnental or Special Government Requirements such as. (see 4.2 and 4. 3 Specify maximum dimension and tolerance requiremeuts. abrasion wear or corrosion resistance of tlie coating. 4. 5. inclusions. 4.7 Significant surfaces and surfaces not to be plated must be indicated on drawings or sample. the duration of thc hcat trcatment shall cornmetice from the rime at which the wl~oleof each part attains the specified temperature.8 Heal T. The location of rack or wire marks in the coating shall be agreed upon between the producer and purchaser. 6. tlie shut peclling shall be accomplished on all surfaces for which the coating is required and all immediate adjacent surfaces when they contain notches.6).3. 6. as well as surface hardened parts. (See Supplementary Requirements). 6. nickel and liypopliosphite.rarn~erif. the heat treatments in Table 3 should be perfonned as soon as practical after plating (see 4. T i e test method. After coating and if specified. l Prerr-ealnienl offron andSleel/or~Reduciiigthe Risk of Hydrogen En~brirllemenl-Parts that are made of steel with ultimate tensile strength of greater than 1000 Mpa (hardness of 31 HRC or greater). High phosphorus deposits may require longer time or a higher rempcrarure.1 The coating surface shall have a uniform.3. 7.forIrorr arid Sleel/or Redt.3 Su-ess Relief 6. the tensile strength to be supplied by the purchaser.2 Higli-strength steel pans with acrual tensile strengths greater than 1000 MPa (corresponding hardness values 300 HV10. or cold straightened subsequent to heat treatment.1 Heat treatment shall be perfomied prefetably within 1 I1 but not Inore than 3 li of plating on plated afier plating of steel palis to reduce tlie i s k of hydrogen enibrittlement. 7.1 Process-The coating shall be produced froni an aqueous solution through chemical reduction reaction. Nors &Contolled shotpeening is the preferred method because rhere . and cracks (see 9. 6. that have been machined.2 and Figs.3. Replenislments to the plating solutioli should be as fiequent as required to maintain tlie concentration of :lie nickel and l~ypopl~osphire between 90 and 100 % of set point. shall require post coating hydrogen embrittlement relief baking when specified by the purchaser.a r e georneoy's where rotary flap peening is not effective.See S11. NOTE 8-Inerr or rcducing atmosphere or Wacuum rufficienrto prevent oxidation is recamrnendzd for hear treatment above 260°C.2 Imperfections that arise froni surface conditions of the substrate which the producer is unable lo remove using conventional pretl-eatmcnt tcchniques and that persist in the coating shall not be cause for rejection (see 6. 7.6.1 To increase the hardness of the coating a heat treatment of over 2h03C is required.3).9). . 6. 7.3 Steel parts which are designed for unlimited life under dynamic loads shall be shot peened or rotary flap peened. 6.1.4 and Test Methods B 571). discoloration due to heat treatment shall not be cause for rejection unless special heat treatment atmosphere is spccificd (see section 5. Avoid rapid heating and cooling of plated parts.6.6.-ealmenl . In all cases. Specification B 850 may be consulted for a list of post treatments that are widely used.2.2 Tliicbiess-The thickness of the coating shall exceed the niiliimuni requirements in Table 2 as specified hy the service condition agreed to prior to plating (see 9. 6. or other abrupt changes of section size where strcsscs will be concentrated.cirig the Risk of HI^-ogen Ei7ibrir/ler1re1ir-Partn that are made of steel with ultimate tensile strengths of 1000 Mpa (hardness of 31 HRC or greater). tcmperature. UOIE 9-The thickness of the caatms canno1 be canrrolled in blind or small diameter dcep holes or where salution circulat~anis rcsrricted.6 Posr Cooririg T. Specification B 849 may be consulted for a list of pretreatments that are widely used. NOTE 7-The length of time to reach maximum hardness vanes with the phosphorus content of the deposit. Table 3 describes thc heat treatment for maximum hardness.8.. Figs. X1. or both.5.2. 7. Also.Platirrg ro Intpwve Adhesiort-To improve the adhesion of the coating to various substrates.2 See Appendixes 3 and 4 and Guide B 656. Suficient time must be allowed for large parts to reach oven temperature.~gto Irrcreose Har-drress: 6.3.6. Requirements 7. and number of allowable spots per unit area shall be specified (see section 5.1 ilppear-aiice: 7.3). which can reduce loss of fatigue strength and improve stress corrosion resistalice after plating.2 Mechanical movement of parts and agitation of tlie bath is recommended to increase coating smoothness and uniformity and prevent pitting or streaking due to hydropcn bubbles.2. 6.5. 6. X1.8.4 Racking-Parts should be positioned so as to minimize trapping of hydrogen gas in cavities and holes.2. allowing free circulation of solution over all surfaces to obtain uniforni coating thickness.7 Hear Trennnenl Afler. especially for conditions o f lower temperarures and longer timcs.4 Porosi+The coatings sliall be essentially pore free when tested according to one of the methods of 9. 6. ground.3 Adl~esion-The coating shall have sufficient adhesion to the basis metal to pass the specified adhesion test (see 9. pimples.303 HB or 3 1 HRC) slid surface hardened parts shall be processed after coating in accordance with Specification B 850. 7. 6. Individual alloys should be tested for rnaxinum hardness attainable. the duration of the test. cold formed.2. Da not usegas containing hydrogen u. pits.2 Acceprarice Requir-ernenrs-These requirements are placed on each lot or batch and can be evaluated by tesling the plated part.3.110 and 9.2). 7.4per Plati. the bath niust be monttored periodically for pH.3 A heat treatment at 260°C for greater than 20 h should be used to reduce rhe loss of surface hardness and strength of some ferrous basis metals.1. fillets.2.1).ith high-srrength steel parts. metallic appearance without visible defects such as blisters.1.1. 6.2.1 To obtain consistent coating properties. the part shall not exceed maximu111 dimension on sig~iificantsurface (sce section 5. 6.3.5 Plarirtg Process: 6.3).8.1 Unless otlicwisc specified.2 Peening-Peening prior to plating may be required on liigh-strength steel pans to induce residual conipressive stresses in the surface. 'he use of a statistical regimen to establish tlie control limits -nd frequency of analysis may be employed to ensure quality deposits are produced. shall require stress relief hear treatment when specified by the purchaser the tensile srrength to be supplied by the purchascr. thar contain more than 11 mass % phosphorus (not ferromagnetic) and that have not been heattreated. rest coupon. Piare. . The purchaser and producer may On the to be If do Test 762 identifies the plan ro be used.34 nm Pb 283. and titan~um. 7.2 Micioho~-dness-The microhardness of Class 2 deposits shall be determined by Test Method B 578 (Knoop). The w'e~ghtpercent of p l i o s p l l o ~ sshall be in the range designated by type classification (see 4. Properly perfomled this will ensure coated products of satisfactory quality and will reduce the amount of acceptance inspection. . 9. 9. V deposits shall be analyzed for alloy composition by testins for P ~ (see 9. Tesr Method B 602 conrains four sampling plans. and Test Method B 762 conlain rampling plans rhat are designed far thc sampling inspection of coatings.94 nm ~ Cu 324. 8.3. Terr Merhod B 602 identifier the plan to be used.3. Meihod-Test Method R 567 is only to coatings On magnesium.1 The purchaser and producer are urged to employ statistical process control in the coating process.5 Weigh.1. or pin ill a specific spot before and after plating using a suitable micrometer Make sure that the sutiaces measured are smooth.1.1). .3 and 9.2 The sampling plan used for the inspectioti of a quantity of coated parts (lot) shall be Test Method B 602 unless otherwise specified by purchaser in the purchase order or contract (see section 5. 9.2 Appenrance-Examine the coating visually for compliance with the requirements of 7. Ti. alloy to within 0.5).. samolinc insoecrion. Tlie tests for these qualification requiremelits shall be performed monthly or more frequently.The instrument must be calibrated with standards havitlg the same compositioti as the coating.55 nrn Zn 206. weigh the nearest milligram before and after plating making sure that the Part or coupon is dry and at room ternperamre f i r each measurement. For Class 2 coatings.. Guide B 697. NOTE 12-inductively coupled plasma techniques can determine the . ~ . and dry. 15-The density varier u.1 Compositiot~-Type 11.3 All specimens used in the sampling plan for acceptance tests shall be made of the same basis material and in tlie same metallurgical condition as articles being plated to this specification. 8. clean. 9.3 Beta Backrcaltet. Test Methods 9. NOTE 10-Usually. Tlie conversion of Vickers to h o o p using Tables E 140 is not recommetided.1 Deposil Anahsis /or Phosphorus: mass % 9. %. Ni 216.1).aser and producer need to a g e e on the plan to be used. is selected at random and inspected.3 Tltickf~ess: NOTE13--Eddy-current type insrruments give erraric measurements due to variarions in conductivity of the coalings with changes in phaspharur content.21 is examined for compliance with the requirements placed an the parts a relatively small number of parrr. 9. 7. Test Methods E 352. Terr Merhod B 762 contains several plans and also gives instmclionr for calculating plans to meet speeial needs.40 nrn CO 238. The instrument shall be calibrated with deposits plated in the same under the same on magnetic ". the sample.4 All specimens shall be provided by the purchaser unless othenrise agreed to by the producer. that Ihave becn produced to the samc rpecificat~on. ~h~ ~ m c e d u r eis known as %. .3. 9. 111. . elccrroplare the specimens with a minimum of 5 p of nickel or capper prior to croir sectioning.1.5 %.1 Phosphorr~s Dererniinarion-Determine phosphorus content according to Practice E 60. Weigh Method-Using a similar substrate surface area.11 and S. When Guide 697 is rDccihed. For Coatings requiring alloy analysis and corrosion testing weekly sampling should be considered as an opuon.hen a collection of coated parts (the inspection lot E.3 M~drogerl E1tibrirrieme17r-TI1e process used to deposit a coating onto high shength steels shall be evaluated for 'lydrogen embrittlement by Test Method F 519. such as coating thicknerr. the microhardness sliall equal or exceed a minimum of 850 (HKLOO (or equivalent Vickers) (see 4. ~ N~~~ 1 1 -~~ l .Il. rhc purcl. Test Method B 762 can be used only for coating requirements that have a numerical limir.ir11 rbe requirements bared on the results of the inspection the sample and the criteria of sample. The purchaser and produccr may agree an the plan(s) to be used.2.3.44 nrn Fe 238.--.62 nrn Cr 284. that have been coated by a single producer at one rime ar approximately the same time undcr essentially identical conditions. .10nrn Cd 214. lfrhey do not.1).1. 7. 8.2 Mogiiefic Inducfion I ~ ~ s l r u i i ~Method-Test enf Method B 499 is applicable to magnetic substrates ~ I a t e dwith autocatalvtic nickel deoosits.2 Composition can be determined by atomic absorption.1.3.The following analysis wavelength lines have been used with minimum inteiference to determine the alloy. Guide B 697 a laye number ofplans and pives guidance an the selecrion of a dan. 9. (7) 8.30 nm P 213.32 nm Sn 198. three far use with tests thal are nondestructive and one for use w!th tests h a t are destructive. 9.1 Sampling plans can only screcn out unsatisfactory products without assurance that none of them will be accepted.75 nnr Al 202. emission or X-ray fluorescence spectrometry. The last must yield a numcncal value and certain swrirrical reauiremeers must bc met.3. Sampling 8.3. ~ autocawlyric P ~ praccsr ~is dmamic ~and a daily~ nickel is recommended. and thar are submitted for scceprance or reject~onan a group. T h e inspection lor is li~en classified as complying or no1 complying u.20 nrn 9.20 nrn P 215.7. 8.3.e etermined by the application o f statistics.3 Qual~ficaiion Requirentenrs-These requiremetits are placed on the deposit and process and are performed on specimens to qualify the deposit and plating process. An inspection lat shall be defined as a collection of coated parts which are o f the same kind.irh its mass % ms content ( S e e Appendix X2).oscopica1 Merhod-Measure tlie coating thickness of a cross section according to rest Method B 487. Three standards Test Method B 602. or Test Method E 156 on known weight of deposit dissolved in warm concentrated nitric acid.4 Micrvtnerer Melhod-Measure the vart. IV.1 Mio. NOTEI L T o protect the edger. specific gravity. the purchaser shall be furnished certification that tlie samples representing each lot have been processed. apply a solution of potassium ferrocyanide prepared by dissolving 1 g of potassium ferrocyanide and 1. apply glac~alacetic acid until the violet color disappears. Certification 11.-There is no universally accepted test for porosity.5. which is cause for rejection. Any red spots remaining indicate pores. a minimum coating thickness of 75 pin is recommended. 0. and grams per cubic centimetres (see Appendix X2). after cooling. 9. 9.1 Calibrate standard thickness specimens with deposits plated in the same solution under the same conditions. and apply a solution of alizarin sulfonate prepared by dissolving 1. When required. tested and inspected as directed in this specification and the requirements have been .4.6. . Rejection shall be reponed to tlie producer promptly in writing. Conversions of Vickers or K~ioophardness number to Rockwell C is not recommended. type of indenter.4 Alimriri Tesr for Alrdi~~i~~urn Allo~.6. rinse.1 g sodium alizarin sulfonate. Mahix effect due to the dismbutian of phosphoms in layers af the coating also effect the measurement accuracy and require t h a ~calibration svrndards be made under the same conditions as the produclion process. dissolved in 5 mL of ethanol is added. A100 g load is recommended. 200 lo 300 mm long and 3 to 6 mrn illick.7 + 0. one ofthe following tests can be used on the plated part or specimen.4 Adhesion: 9. It will v a ~ y depending on loads. l l ~ erhombic Knoop indenter gives higher hardness readings than tlie square-hase pyramidal Vickers diamond ~ndenterfor 100 to 300 g loads. examine the pan for blue spots. Tlie instrument must be alibrated with standards having the same composition as the -coating. 9.6.3. After rinsing and air drying. Rejection and Rehearing 10..6 POI-osih. For ~narimurnaccuracy. The phosphorus content ofthe coating must be known to calculare the thickness of the deposit. Tlie surface of the coating shall be cleaned prior to testing (see Note 14). After 4 min contact.1 When specified in the purchase order or contract.6. The precision and bias requiremetits will vary for each type of test. 9. total surface area in squarc centimetres. aoneslon suggesrea. If an alternate test is specified it shall be agreed upon between the producer and the purchaser. nor more than 20 min after tlie initial application of heat.3. 9. the producer may make a claim for a hearing Coatings that show imperfections may be rejected.6 Coulo~aerricMethod-Measure the coating thickness in accordance with Test Method B 504. 9. Continue to boil the water for 30 min. NOTE 19-Aerated water is prepared by bubbling clean compressed air rhrough disrilled ujater by means of a glass diffusion disk at room tempemrum for 12 h. and examine for rust spots. 9. Apply heat to the beaker at such a rate that the water begins to boil in not less than 15 min. 10.2 In~pnct Tesl-A spring-loaded center punch with a \-point having 2 to 3 m m radius is used to test adhesion of the coating on nansignificant suifaces of the plated pan. 9. Nore 1 8 4 n thick (75 pm+) coatings on steel a surface microhardness derennination is permissible. and operator. Make three closely spaced tndentations and examine under IOX ~iiagnificatlonfor flaking or blistering of the coating.2 Boiling Walei.4.3 Aernled N'aler Test for Iron-Base Subsrt-aresImmerse the part for 4 h in vigorously aeratedType 1V or better water (see Specification D 1193) at 25 t 2°C temperature and then examine the part for rust spots. Then remove the pan. 9. Insertion of a sharp probe at the tnterface of the coating and basis metal to detem~ine the .1 Part(s) that fail to conform to the requuements of this standard may be rejected.The appearance of brown spots after 2 min indicate pores. The coating is examined for blistering or other evidence of poor adhesion at 4X magnification.5 g of methyl cellulose in 90 mL of boiling water to which. air dry.1 D = = NOTE l&Ti>is method is only recommended for depasjts in the as-plared condition.5 g methyl cellulose in 90 mL of boiling distilled \x8atcr. The solution to be used shall be in accordance with manufacturcr's recommendations. Nari 17-Appropnare rest specimens are strips approximately 25 mln wide.?ess-The microhardness of the coating can be measured by Test Method B 578 using Knoop indenter and is reponed in Knoop Hardness Number (HK). After cleaning.3 Tl7er-mnlS11ock-The coated pan is heated to 200°C in an oven and then que~ichedin room temperature water.1 Ferroxj~lTest for h a n Base Sr~bslrates-Prepare the test solution by dissolving 25 g of potassium ferricyanide and 15 g of sodium chloride in 1 L of distilled water. which form at pore sites. 1s .6.Calculate the thickness from the increase in weight. Fine cracks in tlie coating on the tension side of the bend are not an indication of poor adhesion. .5 Porosih Tesr for Copper Subslrares-Wipe the plated pan or specimen with glacial acetic acid After 3 min. 9.1 Bend Tesl (Test Metliods B 571)-A sample specimen is bent 180" over a mandrel diameter 4X the thickness (10 mm minimum) of the specimen and examined at 4X power magnification for flaking or separation at tlie interface.3. In the case of dissatisfaction occurs with tlie results of a test. The pH of the aerated water should he 6.7 X-Ray S p e o r o r n e r ~ ~ M e a s u the r e coating thickness in accordance with Test Method B 568.6. 9. 11. immerse the part for 30 s in the test solution at 25°C. ta 50 9. see Ref (6). After 3 min contact.Test for Iron-Base SubstraresCompletely immerse the pan to be treated in a vessel filled with aerated water at room temperature. wliich indicate pores.5 M~c~ahard. .Wioe the nlated part or specime~iwith 10 mass "o sodium hydroxide solution.7 Other Tesl Methods-Test methods which have been developed that are equal to or better than these may be substituted.1. 9. and area as follows: where: It' = weight gain in milligrams. 9.s. Duration of the test is 6000 cycles and it can be extended to 25 000 cycles for more complete resnlts. the part(s) shall be shot peened prior to plating in accordance with Specification B 851 or MIL-S'3165.2 Con~posifion-When specified by tlie purchaser in the orderiny information the phosplioms content shall be maintained in the deposit to within 1 %. the coating shall be tested for hdliesive wear resistance usine Test Method D 2714 or Test Method D 2670. S l .1. The results should be averaged witl~outthe first 1000 cycles and abrasion wear resistance is reported as the wetght loss in rngIlOO0 cycles (Taber Wear Index). the coating shall be tested for abrasion wear resistance using the method in Appendix XI of this specification. inert. APPENDIXES (Nonrnandator! Inlormation) XI.1. electroless.ith MIL-S-13 165 or rotary flap peened in accordance with MIL-R-81841. chemical nickel. Ihe wear rite shall be specified by the purchaser and agreed to by the producer.8 Solderabili1)-When specified by the purchaser in the ordering information. S1.1.l Shot Peening-When specified by the purchaser in the ordering information. comosion resistance. nickel: nickel phosphorus..met. 12. thc unaged coating shall pass Test Method B 678 on solderability.eWeor-When specified by tlie purchaser in 5 ordering information. CASS). TAHEHABRASER WEAR TEST METHOD Xl. S1.7 Coi7tacr Resisrance-When specified by the purchaser in the ordering information.nsiorl Resbrance-Use Method G 85 (acetic acid-salt spray test).fArmosphere-When specified by the purchaser in the orderiny information. S1.1 Scope X1. conductive. a report of the test results shall be funislied. functional. Thc coating shall tuect a maximum wear rate which is specified by the purchaser and agreed to by the producer.11.1 This test method will evaluate the resistance of the coating to abrasive wear. . NOTEXll-Variation in results ha\w been atrributed la the humidiry i n the laboratory and [he storage conditions of [he CS-10 WIIPPIP. Care X1. S I . The test is performed by rotating a plated panel under rotatins rubber wheels and weighing the panel after each 1000 cycles for weight loss. S1. the coating shall be heat treated in a vacuum. When specified in the purchase order or contract. S1.10 Pirling Col.3 Packaging--Parts shall be packaged in accordance with Practice D 3951. or Method B 380 (Corrodkote) lo evaluate the corrosion resistance of the coating to pitting. 11.9 Corrusiori R e s i s f a n c e W h e n specified by the purchaser in the ordering information the coating shall pass any special corrosion tests agreed to by the producer The corrosion resistance of tlie coating to a specific liquid medium can be determined by means of immersion tests (see Practice G 3 I) or electrochemical test (see Practices G 5 and G 59). coatings. S 1. $1. I I . 2 Sl~otPeening--High strength steel palt(s) processed Tor US Government and Mililaty use shall be shot peened in accordance u.4 Hydrogen Embi-itrlemerzr-When specified by the purchaser in the ordering informatinn tlie plating process shall be evaluated at the time of processing pans for hydrogen embrittlement using Test Method F 5 19. the coating shall be tested for contact resistance using Test Method B 667. wear resistance SUPPLEMENTARY REQUIREMENTS The following supplementary requirements shall apply only when specified by the purchaser in tlie contract or order. S1 5 Abr-orice Wear-When specified by tlic purchaser in the ordering information. S1.2 The results are variable between tests and therefore three plated test specimens should be tested to 6000 cycles each. S1. Method B 368 (copper-accelerated acetic acid-salt spray. be conrrol lhe IJumidiv bewee" tests. or reducing am~ospliere to prevent surface oxidation of tlie coating. 1 l Specioi Goven~~nent Reqlrirernents: S 1. 3 1rrer.1 Sonipling-Part(s) plated for the US Govcrnrnent and Militaly use shall use MIL-STD-105 as tlie sampling plan. (see Note 6).6 Adhrsi~. Use the test methods described in 9. S l .1 autocatalytic. 2. Report the mean and standard deviation for the coating.Use CS-10 (resilient rubber) Taber wheels. X1.1 Plate three specimens with 0.2. (100 by 100 by 1. To reface the wheels use CS-I1 discs from Taber The hardness of CS-I0 wheels can change with time and call effect the reproducibility of results (see Test Method D 4060).3.-" X1.5 Repeat X1.2 Wear test the specimens.4 Ana/lrrcal Balance-Scale which is capable of measuring lo 150 g 5 0. 14'ear.Test specimens shall be made from 20 gage CR steel 4 by 4 in. .2.3. X1.2.1 .3 and Xl. X1.250 (6.3 mm) with a 0.3 k t Specimeiu. X1.2. ~~ ~~ X1. X1.4.35 mm) hole in the center.1 mg.1 Run the CS-I0 wheels on the coating for 1000 cycles to remove any surface roughness.4 until a total of 6000 cycles have been accomplished for each speclmen.3.3.2.4 Abrasion test the coating with 1000 g load for 1000 cycles.2.Testing Unit-The unit must be capable of loading u'itll 1000 g load and operating with a vacuum. For each of the three specimens complete the foilowing steps: X1.3 Procedure X1.4 Reporting XI .3.X1.001 in. Test specimens are available from Taher. (25 pm) of -nickel phosphorus coaling.Z Apparatus .3.2.2.3. X1.1 Determine the average weight loss in milligrams for each specimen per 1000 cycles Taber Wear Index and the mean weight loss per 1000 cycles for all specimens. X1.3.3.2.2 A~I-asior?Wlzeels.2.. The wheels shall be loaded with 1000 g with a vacuum on high for the entire test.1 Taber Abi-asei.3.2. X1.2.3 Dress the CS-I0 wheels with a CS-11 disc for 50 cycles. X1. X1.2 c o o l weigh (he specimen to the nearest 0. V o l 88. P h y s ~ r a c h e m ~ i a l Prlnrlples a f Nickel PIat8ng. OH 1991. E l e i t r o l e r r Nickel P l a t m g . Cinclnnat. X2. u n p u b l l r h e d Ratam. P:atlnq and S u r f a c e Flntshlng. Elnlr. B e r l ~ n1982 Mallory.Rajam r t a 1 M e t a i Flo\rh\og. S r h e r m g KG. '963 Vendor Siherlng. 1995 FIG. G l e x Ha:lary i t al. s t u d i e s and P r o p e r t i e s o f Very Hard E l e c t r o l e s s Nickel D e p a i c t r EN'95. u i l p u b l ~ s h e da n a l y t ~ c a rl e s u l t s . DENSITY O F AUTOCATALYTIC NICKEL DEPOSITS Density of Electroless Nickel Deposits Reidel. Thermal Condurriv8ty o f E l e c t r a l e r r N l i k e l . No 3 lI'18ll 0 K a n q e n .XZ. C S. V a l 68.P h o s p h o r u s A I l c y P l a l l n g . K M.1 Density of Autocatalytic Nickel Phosphorus Alloy Summaw of Reported Values . 0 D Smith. p92 DIN 50966 A + I S 0 152: Annex C Vendor. (lardner Management. 1'163 0 Garbunova. N a h a n a l S r l e n t e Foundahon. F ~ e l d ~ nOgburn g el a\. ASTM S I P No 265. H e r a l r P a r k . (lorbunova and A A Nlk!toroua. ASH 1n:ernallonal. i l e r t r o l e s s Nlckel P l a t ~ n g1959 Oak Rldse. W d f g a n g . No 11 119401 NIST. N a t ~ a n a Sl o e n c e Foundailan. OH. 1 The physical differences o f these TYPES provide for a wide variation in performance in wire bonding. machineability. reactivation and melting point. X4.X3. lubricity. X3. contact resistance.- 0 100 200 300 ! 1 1 - LOO 500 TEMPERATURE (C) I HOUR FIG.1 Hardness of Autocatalytic Nickel Phosphorus Versus Heat Treatment Versus Phosphorus X4. purity. and elongation may be necessary for same applicarions. Additional requirements far internal m e s s .e thickness resting by X-Ray and magnetic means. . These di5erences are produced by micro structural di5erences between ~i + Ni3p and ~ i 3 p~h~~~ differences also effect non-destmcti\. Careful attention to the selection of TYPE mill insure optimum perfonnai~ceof the deposit in the intended application. HARDNESS VERSUS HEAT TREATMENT HARDNESS OF ELECTROLESS NICKELvs TEMPERATURE vs TYPE LOO I ! ' I'1 . ALLOY TYPES NOTE X ? I-lllese d~fferentalloy TYPES are produeed from processes which are specifically formulared and controlled. .5.. undercoats.. SUMMARY PROGRAM 14 X5.. X5.. The program involved plating 12. The heat treatment temperature was considerably higher than typical processing and was chosento evaluate the formation of diffusion products of iron...1 Selected Properties of As Plated Autocatalytic Nickel Phosphorus Coatings by Phosphorus Content X5... . X5.. surface preparation..1........... . X4....3 The following matrix of test panels were prepared and exposed with subsequent analysis for alloy and thickness. X5.1..... ... North Caiolina: X5......... ..1 Results o f 110 Mo17lh Exposrtrr o f Aulocatalylic Nickel Deposits a/ Kurv Beach......2 There were nine different sources of deposits.. N C (Kure Beach)...... nickel and phosphorus.. .........1 Program 14 is part of an ongoing marine exposure testing process at the 75 m site at LaQue Ceriter for Corrosion 'echnology.... LOW HIGH NON FERRO MAGNETIC MAGNETIC FIG..HARDNESS STRENGTH MAGNETICS TYPES ... -.. and 7 5 p m thicknesses on smooth and ground surface and one smooth lot heat treated for hardness at 550°C for 2 11. The program called for the plating of both Type IV and Type V deposits on standard smooth and ground steel Q Panels.4 The interpretation of the results of these exposure test should be made on the basis of general performance of the coating on panels. 25. Base metal condition.... arid post processing all have a significant effect on the performance and should be given careful consideration when designing the part and pretreatment processing sequence...1. each providing five lots of five panels........... Panels were rated at Kure Beach each year by a team from ASTM Committee 8 8 using Practice B 537....1.............. Wrightsville..... 1974. "Effects of Heat Treatment on the Prapenier of Eiecrroiess Nlckel Deposits. F L 32826.ig Pl.iishirrg.?~. Pancullis Press. London.t nq REFERENCES (1) Symposium on Elecnolesr Nickel Plating. (7) Parker..6 1 3 0 Ground Smaath Smooth Smooth Smooth Ground Smoolh Smoolh Smooth Smooth Ground Smooth Smooth Smooth Smooth Ground Smooth Smooth Smaath Smooth Ground Smoolh Smooth Smooth Smooth Ground Smoolh Smooth Smoolh Smooth Ground Smoolh Smooth Smoath Smooth Ground 1 2 3 4 5 Smooth Smooth Smooth Smooth No Yea Gro." Plori.-oper-ties of Elecnadeposired hf~:Iolr orzd A/lr.". K. C l ~ e n ~ i c (Elecnulers) ol N i d e l Ploting.. " o w n s. N o l t h CarolinaA P ~ O S D ~ OAlloy R I S %wf Deposit Type Source Lot 1 Smoolh Smooth Smoolh Smoolh Heal Treatment Thickness. N'i (3) Gawrilav. C.. The lntemarianal Nickel Ca. 1959. 1986 Chapter 23. and HajduI. (2) D?~i~~rer-i. (6) Parker. 12644 Research Parkway.. ASTM. pm Actual ICP EDM Ractice B 537 Ralings 110 Months 3.2 . K. CC L O 11 s caper Mar (:on05 on i2etiormnn~r. December 1981.enre ProLr F n s n 1.Vol 6 1.. Inc. September 1971.mmanzro o) Dr George ) B a n ol h(:D n or Slce F r a Reporl un ASTM Fogrl.oprr-lies q(E1ecnuless Nickei. FL 32826.14 ho ro has DrcSPnleJ al i h r l (:oo'c. "Elecholess Plaling.<..5 25 75 Thickness.1 Results o f 110 M o n t h Exposure of Autocatalytic (Electroless) Nickel Deposits a t Kure Beash. G. pm Target NO 12. .TABLE X5. ronr ." Plorisg orzd B. ASTM STP 265...~.5 No No 12. 1990. The American Eleclroplaters and Surface Finishen Society.~' Hardness and Wear Rerirrance Tests of Elecrrolers Nickel Deposits.01 C h (:os.nJ 'ro ~ ~ ~ ~ " 80 7. W H. Orlando.lESF 12644 Research Parkway. 25 ~ 23 Te . (4) Safranek. Vol 68.on$ 'rum i n s mar r e e x v o s ~ r cp o g r m l a . (5) Mallary G. Orlando.1 .r./"cr Fi. Tile P. Ncw York... i.mg). 1W Ban Haaoi Drive. Users of hb sfandaid are expressly adwsed lhal deleiminalion of ihe vaiidily of any such palent rlqhls.ly This sleodard K subjecl to revision a1 any time by lhe iesponslbie lechnicai comminee and musl te reviewed eveiy five years and if no1 revised.Your commenls are invited miher tor revision oi lhis slandaid or for oidditiooal standards and should be addressed lo ASTM lnlemal~onalHeadquarlers. 610-832-9555 (fax). PO Box C700. or lhmugh lhe ASTM wcbsile (w.aslm. a1 the address shown below This slarldard is copyrighled by ASTM lnternaliononai. or ser/
[email protected] (email).nls (singie or muiupie copies) of lhrs standard may be oblamed by coolacting ASTM a1 h e above address or a1 610-832-9585 (phone). are enl~relylheii own rerpoosibil. West Cooshohocken. either reaowved or wrhdrawr~.ldivrdual iepi.Onal lakes no position respecling lhe validity of any paten1 "ghlr asserted in conneclion wih any rlem mentioned in his sfanaard. and lhe nsk of infnngemeol of such rights. Uoiled Slales.PA 19428-2959.ASTM inleroa1. . Youimmmenls Wli receive camfvl mosideiation a1 a meeling of me iesponsibie lecnnicai cornmillee. whrch you may anend if you feel ihal your mmmeotr have not received a fair heai~ngyou should make your views known lo the ASTM Commitlee an Standards.