ASTM B733

ADOPTION NOTICE

custodians: Adopting Activity:

h y " R Air Force - 11
Navy - AS (Proj No. MFFP-0565)
Air Force - 11

Review activity:
Air Force- 99

AREA MFFP
AMSC NIA
DISTRJBUTION STATEMENTA. Approved for public release; distribution is unlimited.

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 S T D - A S T M B733-ENGL 3777 W 0757530 Ob04732 T A U m

4Tb Designation: B 733 97 - AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken. PA 19428
Repmted from lhe Amua1 Book of ASTM StardardS. Copyright ASTM

Standard Specification for

Autocatalytic (Electroless) Nickel-Phosphorus Coatings on
Metal'

1. scope contents greater than I 1.2 76 P are not considered to be

t. 1 Thisspecificationcoversrequirementsforauto- ferromagnetic.
catalytic(electroless)nickel-phosphoruscoatingsapplied 1.10 The values stated in SI units are to be regarded as
from aqueous solutionsto metallic products for engineering standard.
(functional) uses. l . 1 1 The following precautionary statement pertains only
1.2 Thecoatingsarealloysofnickel and phosphorus to the test method portion, Section 9, of this specification.
producedbyautocatalyticchemicalreductionwith h m This stan&ud does not purport to address all of the safety
phosphite. Because the deposited nickel alloy iscatalyst
a for comem, if any, associated with its use. It is the responsi-
the reaction, the processis self-sustaining. The chemical and bility of the user of this standard to establish appropriate
physical propertiesof the depositvaryprimarilywithits safety and health practices and determine the applicability of
phosphoruscontentandsubsequentheattreatment.The regulatoty limitations priorto use.
chemical makeup ofthe plating solution andthe use of the
solution can affect the porosity and corrosion resistance of
the deposit. For more details, see ASTM STP 265 (1)2 and 2. R e f e r e d Docoments
Refs (2) (3) (4) and (5) also refer to Figs. X 1.I,X 1.2, and 2.1 ASTM Standardr:
X 1.3 in the Appendixof Guide B 656. B 368 Test Method for Copper-Accelerated Acetic Acid-
1.3 Thecoatingsaregenerallydepositedfromacidic Salt Spray (Fog) Testing (CAS Testing)3
solutions operatingat elevated temperatures. B 374 Terminology Relatingto Electroplating3
1.4 The process produces coatings of uniform thickness B 380 Test Method ofCorrosion by the Corrodkote
on irregularlyshaped parts, provided the plating solution P r d d
circulates freely over their surfaces. B 487 Test Method for Measurementof Metal and Oxide
1.5 The coatings havemultifunctional properties, such as Coating Thicknessesby Microscopical Examinationof a
hardness, heat hardenability, abrasion, wear and corrosion Cross W o n 3
resistance, magnetics, electrical conductivity provide dif€u- B 499 Test Method for Measurement of Coating Thick-
sion barrier, and solderability. They are also used for the nesses by the Magnetic M e t h d Nonmagnetic Coatings
salvage of worn or mismachined parts. on Magnetic Basis Metals3
1.6 The low phosphorus (2 to 4 % P) coatings are
microcrystalline and possess high as-plated hardness (620to B 504 Test MethodforMeasurementofThicknessof
750 HK 100). Thesecoatings are used inapplications Metallic Coatings by the CoulometricMethod3
B 537 Practice for Rating of Electroplated Panels Sub
requiring abrasion andwear resistance.
1.7 Lowerphosphorusdepositsintherange between 1 jeCtea to Atmospheric Expos&
and 3 % phosphorus are also microcrystalline. These coat- B 567 Method for Measurement of Coating Thickness by
ings are used in electronicapplicationspro,yidingsolder- the Beta Backscam Method3
ability,bondability,increasedelectricalconductivity, and B 568 Method for Measurement of CoatingThicknes by
resistance to strong alkali solutions. X-Ray Spectrometry3
1.8 The medium phosphorous coatings ( 5 to 9 96 P) are B 571 Test Methods for Adhesion of Metallic Coatings3
most widely used to meet the general purpose requirements B 578 Test Method for Microhardness of Electroplated
of wear and corrosion resistance. Coatings3
1.9 The high phosphorous (more than 10 % P) coatings B 602Test Method for Attribute Sampling of Metallic and
have superior salt-spray and acid resistance in a wide range Inorganic Coating?
of applications. They are used on beryllium and titanium B 656 Guide for Autocataytic Nickel-Phosphorus Deposi-
partsfor low stressproperties.Coatings with phosphorus tion on Metals for Engineering U&
B 667 Practice for Construction and Use of a Prok for
Measuring Electrical Contact Resistance4
'This specitication is under (he jurisdiction of ASIM Cornmittee Bo8 an B 678 Test Method for Solderability of MetalliGCoated
Metal Powders and Metal Po& Products and is tbe. direct responsibility of Products3
Subcommittee B08.08 on Eoginmiug coatingr
Current edition approved July IO, 1997. Published October 1997. origioauy
-
published as B 733 - 84. Last previous edition B 733 90(1994).
The boldface n u m b m given in parentheses refer to a List of references at the A d Book ofASTM &anh&, Vd 0205.
end of the text A d Bod ofAS7" &anh&, Vol 03.W.

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 B 697 Guide for Selection of Sampling Plans for Inspec- the coating must protect fiom corrosion or w ea
r
, or both,
tion of ElectrodepositedMetallic
and
Inorganic and that are esential to the performance.
Coatings3 3.2 Other D&itiom-Terminology B 374 defines most
B 762 MethodforVariableSamplingofMetallicand of the technical terms used in this specification.
Inorganic Coatings3
B 849 Specification for Pre-Treatmentof Iron or Steel for
Reducing the Risk of Hydrogen Embrittlement3 4. contingchapifuction
B 850 Specification for Post-CoatingTreatments of 4.1 The cuating dadication system provides for a
Iron or SteelforReducing the Risk ofHydrogen scheme to select an elechroless nickelcoatingto meet specific
Embrittlement3 performance requkments based on alloycomposition,
B 851 Specification for AutomatedControlledShot thickness and hardness.
PeeningofMetallicArticles Prior to Nickel, Auto- 4.1.1 TYPE describes the general composition of the
catalytic Nickel, Chromium, orAs A Final F e h 3 deposit with respectto the phosphorus content and is divided
D 1 193 Specification for Reagent W a t d into five categories which establish deposit properties (see
D 2670 Method for Measuring Wear Roperties of Fluid Table 1).
Lubricants (Falex Method)'
D 27 14 Method forCalibration and Operation of an Alpha . . 1-h" to the pmckion of some phosphorus analysismethods
NOTE
a&v1at~mof0.5%hpbeendesigecdintothisdarrificetionscbane.
L F W - 1 Friction and Wear Testing Machin&
D 395 1 practice for Commercial Packaging7 Roundingoftktcatresultsduttothe~ofthclimitspmrideJ
foran~limaofCSand9.5%~~.ForQCampk.~
D 4060 Test Method for Abrasion Resistance of organic withatestresultfar~of9.71wouldhaveaclasgificatiollof
Coatings by the Taber A b d TYPE V, stt Appeaaix 4, M o y TYPES.
E 60 Practice for PhotometricMethods for Chemical
Analysis of Metalsg 4.2 Service Condition Based on Thickness:
E 156 TestMethodfor Determination of Phospho- 4.2.1 service condition n u m b are based on the severity
NS inHigh-Phosphorus Brazing Alloys (Photometric of the exposure in which the coating is intended to perform
Method)Io and minimum coating thickness to provide satisfi&%ory
E 352 Test Methods for ChemicalAnalysis of Tool Steels performance (seeTable 2).
and Other Similar Medium-and High-Alloy Steel' 4.2.2 SC0 Minimum Service, 0.1 pm-This is defined by
F 519 Test MethodforMechanicalHydrogenEmbrit- a minimum coating thickness to provide specific material
tlement I properties and extend the life of a part or its finction.
G5 Practice for Standard Reference Method for Making Applications include requirementsfordiffusion barrier,
PotentiostaticandPotentiodynamicAnodicPolariza- undercoat, electrical conductivity and wear and c o d o n
tion Measurementst2 protection in specialized environments.
G 31 Practice for LaboratoryImmersionCorrosion 4.2.3 SC1 Light Mice, 5 pm-This is debed by a
Testing of Metals12 minimum coating thickness Of 5 pm for extending the life of
G 59 Practice for Conducting Potentiodynamic Polariza- the part. Typical environments includelight-load lubricated
tion Resistance Measurements12 w e ar
, indoor c o d o n protection to prevent rusting, and for
G 85 Practice for Modified Salt Spray(Fog) Testing'' soldering and mild abrasive wear.
2.2 Military Standards: 4.2.4 SC2 Mild Mice, 13 pm-This is defined by mild
MLR-81841 Rotary Flap Peening of Metal P a d 3 c o d o n and wear environments. It is &am&xid by
"S13165 Shot Peeningof Metal Parts13 industrial atmosphere exposureon steel substrates in dry or
"STLl-109 Sampling procedures and Tables for In- oiled environments
spection by Attribute" 4.2.5 SC3 Moderate Service, 25 Pm-This is defined by
2.3 I S 0 Stanaízrds: moderate environments such as non marine outdoor expo-
IS0 4527 Autocatalytc Nickel-Wosphorus Coatings- sure,alkaIi salts at elevated temperature,and moderate wear.
Specification and Test Meth0dd4 4.2.6 X 4 Severe Service, 75 pm-This is defined by a
very aggnssive environment. Typical environments would
3. Termindlagy indude acid solutions, elevated t empemm and pressme,
3.1 DeJirrition: hydrogen diide and carbon dioNde oil service, high-
3. l. 1 significant su$bces-those substrate surfaces which temperam chloride systems, very severe w e ar
, and marine
immersioa
'AlFmdLkddASTM&&dS,Vd 11.01. Nars2-"Ihe~oftherutocoEllytic~caatingdb
6A d Lkd t$ASTM s*abnrdr,Vd 05.02 pendstoa~cxtcotontbesurhabishofthearridetobepletal
A d Bod t$ASl"JzcAdrudr,Vd 09.02.
8AnnurrlBoakt$~~,VdOaOl.
A d Ba& t$ASl" Vd 03.05. TABLE1
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~4Avühbk6romrlmaicrn~SMdPd,lP.ttmtE,11W.~nd~.13tb V 10"
Flow,NewYork+NY10036.

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 B 733
TABLE2 senicecondilions 5.1.1 Title, ASTM designation number, and year of issue
Coating TNdrnert Requirrnnents of this specification.
Minmuncoating 5. I .2 Classification of the deposit by type, seMce condi-
secvicecondipbn Thidcness v m. (m) tion, class, (see4.1, 4.2 and 4.3).
specificetan
5.1.3 Specify maximum dimensionand tolerance require-
Sc0 Mr
iLnrn- 0.1 o.-( 1 ments, if any.
SC1 Light service 5 ~.oO02 ( 1
SC2 hwservice 13 o.O@x ( 1 5.1.4 Peening, if required (see6.5).
Sc3 Modmatesenice 25 0.001 ( ) 5.1.5 Stress relief heat treatment before plating, (see 6.3).
Sc4 severeservice 75 0.m ( ) 5.1.6 Hydrogen Embrittlement Relief after plathg, (see
6.6).
5.1.7 Sisnificant surfaces and surfices not to be plated
must be indicated on drawings or sample.
and how it was pretreated. Rough, non uniform wrfàces require thicker 5.1.8 Supplementalor Special Government Requirements
coatings than smooth surfaces to achieve maximum corrosion such as, specific phosphorus content,abrasion wear or
and minimum porosity. corrosion resistaace of the coatin& solderability, contact
resistance and packagingselectedfirom Supplemental Re-
4.3 Post Heul Treatment Class-The nickel-phosphorus quirements.
coatings shall be classified by heat treatment after plating to 5.1.9 Requirement for a vacuum, inert or reducing a t m e
increase coating adhesion and or hardness (seeTable 3). sphere for heat treatment above 26032 to prevent surface.
4.3.1 Class I-"deposited, no heat treatment. oxidation of the mating (see S3).
4.3.2 Class 2-Heat treatment at 260 to 400°C to produce 5. l. 10 Test methods for coating adhesion, composition,
a minimum hardness of 850 HKIOO. thickness, porosity, wear and corrosionresistance, if re-
4.3.3 Class 3-Heat treatment at 180 to 200°C for 2 to 4 quired, selected from those found in W o n s 9 and Supple-
h to improve coating adhesion on steel and to provide for mental Requirements.
hydrogen embrittlement relief (see 6.9). 5. l . 1 1 Requirements for sampling (seeSection 8).
4.3.4 Class 4-Heat treatment at 120 to 130°C for at least
1 h to increaseadhesion ofheat-treatable(age-hardened) N m 4" purchasa should furnish separate test specimens or
coupons of the basis metal for test purposes to be plated concurrently
aluminum alloys and carburizedsteel (see Note 3). with the articIes to be plated (see 8.4).
4.3.5 Class 5-Heat treatment at 140 to 150°C for at least
1 h to improve coating adhesion for aluminum, non age- 6. Materials and Mandacture
hardened aluminum alloys, copper, copperalloys and beryl- 6.1 Substrate-Defects in the surface of the basis metal
lium. such as scratches, porosity, pits,inclusions, roll and die
4.3.6 Class 6-Heat treatment at 300 to 320°C for at least
marks, laps, cracks, bum, cold shuts, and roughness may
1 h to improve coating adhesionfor titanium alloys.
advemly affect the appearance and performanœ of the
N m 3-Heat-treatablealuminum alloys such as Type 7075 can deposit, despite the observanœ of the best plating practice.
undergo microstructural changes and lose strength when heated to over Any such d e f m on signifïc8nt surfaces shall be brought to
130'C. the attention of the purchaser before plating. The producer
shall not be responsible for coatings defects resulting h m
5. Ordering Information s u r f a conditions of the metal, ifthese conditions have been
brought to the attention of the purchaser.
5.1 The following information shall be supplied by the 6.2 Pretreuttment"parts to be autocatalytic nickel plated
purchaser in either the purchase order or the
on engineering may be pmtreated in accordancewithGuide B656. A
drawing of the part to be plated: suitable method shall activate the surface and remove oxide
and foreign materials, which may cause poor adhesion and
TABLE 3 ClassilicaiionoiPostHeatTreabnent coating porosity.
CLASS oescription
CC)
Tm@) N m 5-Heat treatment of the base material may effect its metal-
lurgical pro
p ex t
e
i An example is leaded steel which may exhibit liquid
1 No Heat Treatment, As Plated or solid embritUement after heat treatment. Careful selection of the pre
2 IieatTrearmentforMaXinun
Hardness
and post heat treatmeatsare recommended.
TYPE I 260 20 6.3 Stress Reli&
285 16
320 8 6.3.1 Pretreatntent of Iron und Steelfor Reducing the Risk
400 1 of Hydrogen Embrittlement-Parts that are made of steel
NP€II 350t0380 1 with ultimatetensilestrength of greater than IO00 Mpa
TYPE 111 36ot0390 1
(hardness of 31 HRC or greater), that have been machined,
TYPE IV 366to400 1
TYPE V 375 to 400 1 ground, coldformed,or cold straightened subsequent to heat
3 HvaogenEmbrittlementand 18oto200 2to4 treatment, shall require stress relief heat treatment when
Adhes*n on steel specified by the purchaser, the tensile strengthto be supplied
4 A&esim.carbwidsteeland 120to130 1-6
" egA
by the purchaser, Specification B 849 may be consulted for a
5 AdhesbnmBerycunand 140 to 150 lto2 list of premtments that are widely used.
Aluminum 6.3.2 Peening-Peening prior to plating may be required
6 AdhesanOnTrtaniun 300-320 I 4
on high-st~~ngth steel parts to induce residual compressive

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 ~~

S T D - A S T M B733-ENGL L777 D 0757530 Ob07735 7 9 T

@ B733
stresses in the sudace, which can reduœ loss offatigue 6.8.2 See Appendixes 3 and 4 and Guide B656 Fgs
strength and improvestress corrosion resistance after plating, X1.2 and X1.3.
(See Supplementary Requirements). 6.8.3 A heat treatment at 260’C for greater than 20 h
6.3.3 Steel parts which are designedfor unlimited life sho~dbeusedtoreduœthelossofsurfacehardn~and
underdynamicloads shall be shot peened or rotary flap strength of some ferrous basis metals. Avoid rapid heating
peened. and cooling of plated pouts.Suffiicient time must be allowed
for large parts to reach oven temperature.
N m bcontroUed shot peening is the ppefkred method because
thereare~~’swh~~taryOappeeningisaoteffectimSeeSl11. NOIE7-Th~~oftinact0reachmaximumhardaessvarieswah
tbCphosphanucontentOftllCdeposit.Highpbogpbanrs~tS~~
6.3.3.1 Unless otherwise specitïed, the shot peening shall mquireb~timcorahigbertem~orboth.Iadividualalloys
be accomplished on all s u r k a for which the coating is should be tested for maximum hardness attainaMe, especially for
required and all immediateadjacent surfàces whenthey COIlditi~Of”andloaggtima.
~8-rncrtorreducingatmosphereor~umsufficientt0
contain notches, fillets, or other abrupt changes of section ~toxidpoionisrrawmendedforheattreatmentrbovc26oxDo
size where stresses will be concentrated. notusegasam~hydrogenwithhigh~stedparts
6.4 Racking-Parts should be positioned so as to mini-
&trapping of hydrogen gas in cavities and holes, allowing
free circulation of solutionoverall surfaces to obtain 7. Requirements
uniform coating thickness. The location ofrack or wire 7.1 fiocm-Tbe coating shall be produced h m an
marks in the coating shall be agreed upon betwen the aqueous solution through chemical reduction reaction.
producer and purchaser. 7.2 AcxqMam? Requiren?ents”These requirements are
6.5 Plating Process: placed on each lot or batch and can be evaluated by testing
6.5.1 To obtainconsistent coating properties, the bath the plated part.
must be monitored periodically for pH, temperature, nickel 7.2.1 Appearance:
and hypophosphite. Replenishments to the plating solution 7.2.1.1 The coating surface shall have a d o r m , metallic
should be as frequent as required to maintain the concentra- appearanœ withoutvisible d e f a such as blisters, pits,
tion of the nickel and hypophosphite between90 and 100 % pimples, and m ks (see9.2).
of set point. The use of a statistical regimento establish the 7.2.1.2 Imperféctions that arise from surface conditions of
control limits and frequency of analysis may be employed to the substrate which the producer is unable to remove using
ensure quality deposits are produced. conventional pretreatmenttechniques and thatpersist in the
6.5.2 Mechanical movement of parts and agitation of the coating shall not be cause for rejection (see 6.1). Also,
bath is recommended to increase coating smoothness and discoloration due to heat treatment shall not be cause for
uniformity and prevent pittingor StreaLing due tohydrogen rejection unless special heat treatment atmosphere is speci-
bubbles. fied (see5.9).
6.6 Post Coating Treatment for Iron and Steel for Re- 7.2.2 Thkksts-The thickness of the coating shall ex-
ducing the Risk of Hydrogen Embrittlement-Parts that are ceed the minimum requirements in Table 2 as specified by
made of steel with ultimate tensile strengths of 10oO Mpa the servíœ condition agreed to prior to plating (see 9.3).
(hardness of 3 I HRC or -ter), as well as surface hardened Aftercoatingandifspecified,thepartshallnotexceed
p a r t s y shall require post coatinghydrogenembrittlement maximum dimension on signiscant surface (see5.3).
relíefbakingwhen specified by the purchaser, the tensile NOIE9--The~oftbecoatingcannotbecontrolledinMind
strength to be supplied by the purchaser. SpecificationB 850 orsmalldiameterdeepholcsorwheresolutioncirculationisrcstricted
may be consulted for a list of post treatments that are widely
used. 7.2.3 Adhesion-The coating shall have sufficient adhe
6.6.I Heat treatment shall be p e r f i i e d preferably within sion to the hasis metal to pas the specified adhesion test (see
1 h but not morethan 3 h of platingon plated after plating of 9.4 and Test Methods B 571).
steel parts to reduœ the risk of hydrogen embrittlement. In 7.2.4 PorositpThe coatings shall be essentiauy porefree
all cases, the durationof the heat treatment shall commence when tested Bccording to one ofthe methods of 9.6. The test
from the time at which the whole of each part attains the method, the duration of the test, and number of allowable
specified temperature. spots per unit axa shall be specified (see5.10 and 9.6).
6.6.2 High-strength steelpartswith actual t e d e strengths 7.3 Qual@cation Requirements-These requirements m
greater than loo0 MPa (correspondinghardness values 300 placed on the deposit and process and are performed on
HV10,303 HB or 31 HRC) and s d k e hardened parts shall specimens to qualï@ the deposit and plating process Tbe
be pn>cessed after coating in accordance with speciscation tests for these qualification requirementsshall be performed
B 850. monthly or more kquentIy.
6.7 Heat Treatment After Plating to Improve Adhesion- 7.3.1 Conrparition-Tm II, m,IV, V deposits shall be
To improve the adhesion of the coating to various substrats, analyzed far alloy composition by testing for phosphorus(see
the heat treatments in Table 3 should be performed as soon 9.1). The weight percent of phosphorus shall be in the range
as practical &el plating (see 4.3). designated by type dassitication (see4.1).
6.8 Heat Treatment ABer Plating to Increase Hurdms: 7.3.2 Mb-me microhardnesp of Class 2 de-
6.8.1 To increase the hardness of the coating a heat posits shall be determined by Test Method B 578 (KMIOP).
treatment of over 260.C is requid. Table 3 describes the ForClass2~themim~nessshalleq~orexceed
heat tnatment for maximumhardness. a minimum of 850 (HK100 (or equivalent Vickers) (see4.3

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 and 9.5).The conversion of Vickers to Knoop using Tables tion, emission or X-ray fluorescence spectrometry.
E 140 is not recommended. N m 12"Inductively coupled plasma techniques can determine the
7.3.3 Hydrogen Embrittlement-The process used to de- alloy to within 0.5 Om.The foUowing analysis wavelength lines have bee0
posit a coating ontohigh strength steels shallbe evaluated for ued with minimum interfaence to determine thealloy.
hydrogen embrittlement by Test Method F 5 19. Ni 216.10 nm Cd 214.44 nm Fe 23820 nm
P 215.40 nm CD 238.34 nm Pb 283.30 nm
8. Sampling P 213.62 nm Cr 284.32 om Sn 198.94 nm
Al 202.55 nm Cu 324.75 nm Zn 206.20 om
8.1 Thepurchaserandproducer are urged to employ 9.2 Appearance-Examine the coating visually for com-
statisticalprocesscontrol in thecoatingprocess.F'roperly pliance withthe requirements of 7.2.l.
performed this will ensure m t e d products of satisfactory 9.3 Thickness:
quality and w lireduce the amount of acceptance inspection.
8.1.1 Sampling plans can only screen out unsatisfactory N m 13-Eddy-cummt type instruments give enatic measurements
due to variations in conductivity of the coatings withchanges in
productswithout assurance thatnone ofthem will be phosphorus content.
accepted. (7)
8.2 Thesamplingplan used for theinspection of a 9.3.I Microscopicd Method-Measum the coating thick-
quantity of coated parts (lot) shall be Test Method B 602 ness of a cross section accordingto Test Method B 487.
unless otherwise specified by purchaser in the purchase order N m 14-To protect the edges, electroplate the specimens with a
or contract (see 5.1 1 and S.1 1.1). minimum of 5 pm of nicket or copper prior to c~(lsssectioning.
NOTE IO-Usually, when a collection of coated parts (the inspection 9.3.2 Magnetic Induction Instrument Method-Test
lot 8.2) is examined for compliance with the requirements placedthe on Methad B 499 is applicable to magnetic substrates plated
parts a relativelysmall number of parts, thesample, is selected at with autocatalytic nickel deposits,that contain morethan 11
random and inspected.The inspection lot is then clasifted as compIying
or not complying with the requirements based on the results of the
mass 96 phosphorus (not ferromagnetic) and that have not
inspection sample.The size of the sample andthe criteria of compliance been heat-treated The instrument shall be calibrated with
are determined by the application of statistics. The procedure is known deposits plated in the same solution under the same condi-
as sampling inspection. Three standads Test Method B 602, Guide tions on magnetic steel.
B 697, and Test Method B 762 contain sampling plansthat are designed 9.3.3 Beta Backscatrm Method-Test Method B 567 is
for the sampling inspectionof coatings. only applicableto coatings on aluminum, beryllium,magne-
Test Method B 602 contains four sampling plans, three for use with
tests that are nondestructiveandonefor use with tests that are sium, and titanium. The instrument mustbe calibrated with
destructive. Thepurchaserand prcduœr may on the plants) to be standards having the same compositionas the coating.
used. If they do not,Test Method B 602 identifig the plan to be used. N m 15-The density of the coating varies with its mass 56
Guide B 697 provides a large number of plans and also gives guidana phosphorus content (SeeAppendù X2).
on the selection ofa plan. When Guide B 697 is specified, the purchaser
and producer need to agree on the plan to be used. 9.3.4 Micrometer Meth0d"Measu-e the part, test
Test Method B 762 can be used only for coating requirements that coupon, or pin in a specific spot before and after plating
have a numerical limit, suchas coating thickness. The last must yield a usinga suitable micrometer. Make sure that the surfaces
numerical value and certain statistical requirements must be met. Test measured are smooth, clean, and dry.
Method B 762 contains several plans and also gives instructions for
calculating plans to meet s p i a l needs The purchaser and producer
9.3.5 Weigh. Plate, Weigh Meth0d"Using a similar sub
may agree on the plan(s)to be used. If they do not, Test Method B 762 strate material of known surface area, weigh to the neafest
idenfifies the plan to be used. milligram before and after plating makingsure that the part
An inspection lotshall be defined as a collection ofcoated parts which or couponis dry and at room temperature for each measure!-
are of the same kind,that have been produced to the same specification, ment. Calculate the thickness Erom the increase in weight,
that have been wated by a single producerat one timeor approximately specific gravity, and area as follows:
thesame timeunderessentiallyidenticalconditions,and that are
submitted for aczeptanœor rejection as a group. coating thickness, Fm = 10 W/(A X D)
8.3 All specimens used in the sampling plan for a m p where:
tance tests shall be made of the same basis material and in W = weight gain in milligrams,
the same metallurgical condition as articles being plated to A = total swface area in square centimetres, and
this specification. D = grams per cubic centimetres(seeAppendix X).
8.4 AU specimens shall be providedby thepurchaser 9.3.6 Coulometric Method-Measure thecoatingthick-
unless otherwiseagreed to by the producer. ness in accordancewith Test Method B 504.The solutionto
NOTEI I-The autocatalytic nickel pnxzss is dynamic and a daily be used shall be in accordanoe with mandachmr's m m -
sampling is recommended. For h q
i
tgrequiring alloy analysis and mendations. The surface of the coating shall be cleaned prior
corrosion testing weekly sampling should be considered as an option. to testing (see Note 14).
9.3.6.1 Calibrate standard thickness specimens with de+
9. Test Methods posits plated in the same solution under the same conditions.
9.1 Deposit Analysis for Phosphorus: 9.3.7 X-Ray Spectrometry-Measure the coating thick-
9.l . 1 Phosphorus Determination-Determine mass ?& ness in accordance withTest Method B 568.The instrument
phosphoruscontentaccording to Practice E 60, Test must be calibrated with standards having the same composi-
Methods E 352, or Test Method E 156 on known weight of tion as the coating.
deposit dissolved in warm concentrated nitric acid. N m I b T h i s method is only realmmended for deposits in the
9.1.2 Composition can be determined by atomic absorp- asplated condition. The phasphorus content of the coating must be

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 ~.
S T D - A S T M B733-ENGL 1777 D 0757530 Ob07737 Sb2
B733
known to calculate the thickness of the deposit. Matrix effect due to the
distribution of phosphorus in layers of the coating also effect thc
meaJwcmcnt B~CUT&CYand muhthat calibration standards be made
under the same conditions as the pmductioo p m
9.4 Adhesion:
9.4.1 Bend Test (Test M e t M B 571)"A sample spec
imen is bent 180' over a mandrel diameter 4 x the thickness
(10 mm minimum) of the specimen and examined at 4X
power magnification for Mcing or separation at the inter-
&. fine cracks in the mating on the tension side of the
bend are not an indication of poor adhesion. Insertion of a
sharp probe at the intedaœ of the coating and basis metal to
determine the adhesion is suggested.
NOTE17-Appropriate test specimens are strips approximately25 to
50mmwide,200to300mmloagand3to6mmthick.
9.4.2 Impact Test-A spring-loaded center punch with a
point having 2 to 3 m m radius is used to test adhesion of the
coating on nonsigni6cant surfaces of the plated part. Make
three closely spaced indentations and examine under IOX
magnification forflaking or blistering ofthe coating, which is
cause for rejection.
9.4.3 ThsnnalShuck-The coated part is beated to 200'C
in an oven and then quencbed in room temperam water.
The coating is examined for Mistering or other evidence of
poor adhesion at 4~ magnification.
9.5 híicrokrdness-The microhardness of the coating
can be measured by Test Metbod B578 using Knmp
indenter and is reported in Knoop Hardnes Number (HK).
It will vary depending on loads, type of indenter, and
operator. A L O O g load is recommended. The rhombic
h o o p indenter gives higher hardness readings than the
squarsbase pyramidal Vickm diamond indenter for 1 0 0 to
300 g loads, see Ref (6). For maximum accuracy, a min-
imum coating thickness of 75 pm is recommended. Conver-
sions of Vickm or Knoop hardness number to Rockwell C is
not recommended.
NOTE1 8 4 thick (75 Fm+) cuatings on steel a surface
microhardnessdetermination is permissible.
9.6 PorosiwThere is no universally accepted test for
porosity. When required,one of the following tests can be
used on the plated part or specimen.
9.6.1 Ferroxyl Test for Iron Base Substrates-Prepare the
test solution by dissolving25 g of potassium ferricyanide and
15 g of sodium chloride in 1 L of distilled water. After
cleaning, immerse the part for 30 S in the test solution at
25%. After rinsingand air drying, examine the part for blue
spots, which form at pore sites.
9.6.2 Boiling Water Test for Iron-Base Substrates-Com-
pletely immerse the part to be treated in a vessel filled with
aerated water at m m tempemture. Apply heat to the beaker
atsucharatethatthewa~beginstoboilinnotlessthan15
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~ ~~ ~ ~~
min, nor more than 20 min after the initial application of
heat. Continue to boil the water for 30 min. Then remove
the part, air dry, and examine for rust spots, which indicate
Po=.
N m 19-Auated wrta is prepared by bubbling clean cornpnssed
airthrougbdistilledwrtabymcansofaglaJPdiffusiondiskattoom
tempaatunfor12h.TbepHoftheaaatedwatasbouhibe6.7+0.5.
9.6.3 Aerated Water Test for Iron-Base Substrates-Im-
mersethepartfor4hinvigorouslyaeratedTypeIVorbettef
water (see Specification D 1193) at 25 f 2% t
emperam
andthenexaminethepartforrustspots.
9.6.4 AlizarinTest for AIuminwnAlloys-Wipe the
plated part or specimen with 10 mass 48 d u m hydroxide
solution. After 3 min contact, rinse, and apply a solution of
alizarin sulfonate prepared by dissolving 1.5 g ofmethyl
œllulosein90mLofboilingwatatowhich,afhcooling,
O. 1 g sodium alizarin MOM^, dissolved in 5 mL of ethanol
isadded.After4mincontaa,apply~aœticaciduntil
thevioletcdordisappearsAnyredspots~indicate
Po-
9.6.5 PorosityTest for Copper Substrutes-Wipe the
platedpartorspecimenwithglacialaceticacid.After3min,
apply a solution ofpotassiumferrocyanide prepared by
dissolving I g of potassium fkmcyan3k and 1.5 g methyl
œUulosein9OmLofboilingdistilledwater.Theappearanœ
0fbrownspotsafter2minindicatepores.
9.7 Other Test Method-Test methods which have been
developedthatareequaltoorbetterthanthesemaybe
substituted. The w o n and bias requimnents will vary
foreachtypeoftestIfanalternatetcstisspecifieditshallbe
agreeduponbctwecntheproduœrandthcpwchaser.
10. Re!jdlm d Rehearing
10.1 Part(s) that thil to conform to the requirements of
thisstandardmayk:rejected.Rejectonshallbereportedto
the producer promptly in writing. In the case ofdhatisfb
tionoccurswiththeresultsofatest,theproducermaymake
a claim fora hearing. coatings that show imperfections may
be rejected.
11. c k r t i f i i
11.1 Whenspecifedinthepurchaseorderorcontmct,the
purchaser shall be lùmished certitication that the samples
representing each lot have b n proased, tested and in-
spected as directed in this specification and the quirements
, h a been met. When specifiedin the purchase oder or
v e
contract,areportofthetestresultsshallbefurnished.
12 Keywords
12.1 autmatalytiq chemical nickek coati-, conductive;
c o d o n resistance; electrolq functional, nickeknickel
Phosphorus;"
 SUPPLEMENTARY REQUIREMENTS

The following supplementary requirements shall applyonlywhen specified by thepurchaser in the

contract or order.

S1.1 Shot Peening-When specified by the purchaser in S1.7 Conlact Resistance-When specified by thepur-
the ordering information, the part@) shall be shot peened chaser in the ordering information, the coating shall be tested
prior to plating in accordance with Specification B 85 1 or for contactresistance using Test MethodB 667.
MILS13165 S1.8 sOldetabi1ity"when specified by the purchaser in
S1.2 Composition-When specified by thepurchaserin the ordering information, the unaged coating shall pass Test
the ordering information the phosphorus content shall be Method B 678 on solderability.
maintainedinthedeposit to within 1 % . Use the test S1.9 Corrosion Resistance-When specified by the pur-
methods described in9. l. chaser in the ordering information the coating shall pass any
S 1.3 Inert Atmosphere-When specified by the purchaser special corrosion tests agreed to by theproducer. The
corrosion resistance of thecoating to aspecificliquid
in the ordering information, the coating shall be heat treated
medium can be determined by means of immersion tests (see
in avacuum,inert, or reducingatmosphere to prevent practice G 3 I ) or electrochemical test (seePractices G 5 and
surface oxidation of the coating. G 59).
S1.4 HydrogenEmbrittlement-Whenspecifiedby the S1.10 Pitting Corrosion Resiszance-Use Method G 85
purchaser in the ordering information the plating process (aceticacid-saltspraytest),Method B 368 (copper-accel-
shall be evaluated at thetime of processingpartsfor eratedaceticacid-saltspray, C M ) , or Method B380
hydrogen embrittlement using Test Method F 5 19. (Corrodkote) to evaluatethe c~rrosionresistance of the
S1.5 Abrasive Wear-When specified by the purchaser in coating to pitting
theorderinginformation,thecoating shall be testedfor S l. 11 Special Government Requirements:
abrasion wear resistance using the method in Appendix X1 Sl. 1 l . 1 Sampling-Part(s) plated for theUS Government
of thisspecification.Thecoating shall meetamaximum and Military use shall use MILSTD-105 as the sampling
wear rate which is specified by the purchaser and agreed to plan.
by the producer. S1.11.2 Shot P e e n i n g " strength steel part($ p m
S I .6 Adhesive Wear-When specified by the purchaser in cessed for US Government and Military use shall be shot
the orderinginformation,thecoating shall be testedfor peened in acconiance with -13165 orrotary flap
adhesive wear resistance using Test Method D 27 14or Test peened in aa;ordancewith Mil-R-8 184l. (seeNote 6).
Method D 2670. The wear rate shall bespecified by the SI. 1 1.3 Puckugin"parts shall be packaged in accor-
purchaser andagreed to by the producer. danq with Practice D 3951.

APPENDIX

(Nonmandatory Information)

XI. TABER ABRASER WEARTEST"I0D

x1.1 scope X1.2 Apparatus
X l . l. 1 This test methodwlievaluate the resistance of the X 1.2.I TaberAbraser Wear Testing Unit-The unit must
coating to abrasive wear. The test is performed by rotating a be capable ofloading with I O 0 0 g load and operating with a
plated panel under rotating rubber wheels and weighing the vacuum.
panel aller each l o 0 0 cycles for weightloss. Duration of the X1.2.2 Abrasion Wheels-Use Cs10 (resilientrubber)
test is 6000 cycles and itcan be extended to 25 O00 cycles for Taber wheels. To reface the wheels use CS-1 1 discs fkom
more complete results. Taber. The hardness of CS10 wheels can change with time
NOTEX1.I-Variation in results have been attributed to the hu- and can effect thereproducibility of results(seeTest Method
midity in the laboratory and the storage conditions of the CS10 wheels. D 4060).
Care should be.taken to control the humidity between tests. X1.2.3 TestSpecimens-Test specimens shall be made
X l . 1.2 The w d t s are variable between tests and there- fiom 20 gage CR stee.14 by 4 in. (100 by 1 0 0 by 1.3 mm)
fore three plated test specimens should be tested to 6000 with a 0.250 (6.35 mm) hole in the center. Test specimens
cycles each. The results should be averaged withoutthe lïrst are available fiom Taber.
l o 0 0 cycles and the abrasion wear resistance is reported as X1.2.4 Analytical Balance-Scalewhich is capable of
the weight loss in mg/1000cycles (Taber Wear Index). measuring to 150 g k O. 1 mg.

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 X13 Procedure
X1.3.1 Plate three specimens with 0.001 in. (25 Pm) of
nickel phosphorus mating.
X1.3.2 Wear test the specimens. For each of the three
specimens complete thefollowing steps:
X1.3.2.1 Run the CS10 wheels on the coating for IO00
cycles to remove any surface rouphness. The wheels shall be
loaddwith IOOOgwithavacuumonhighfortheentiretest.
X1.3.2.2 Cool and weigh the specimen to the nearest 0.1
mg.
X1.3.2.3 Dress the CS10 wheels with a C S 1 1 disc for 50
cycles.
X1.3.2.4 Abrasion test the coating with IO00 g load for
~Ooocycles.
X1.3.2.5 Repeat X1.3.2.2, X1.3.2.3and X1.3.2.4 until a
total of 6OOO cycles bave been accomplished for eacb
specimen.
X l A Reparthg
X1.4.1 Determine the average weight loss in m@cams
for each specimen per lo00 cycles Taber Wear Index and the
mean weight loss per lo00 cycles for all specimens. Report
the mean and standard deviation for the coatins

X2. DENSITY OF AUTOCATALYTIC NICKEL DEPOGITS

Density of Electrobs8 Nickel Deposits

Reidel, Wolfgang, Electroless Nickel PLating. ASM International, Metals Park, OH 1991, p92. DIN 50966
IS0 4527. Annex C
Vendor, Elnic, unpublished
Rajarn, K. S. Rajam e t al. Metal Finishing, Vol 88. No 11 119901
NIST, Fielding Ogburn e t al, Plating and Surface Finishing, Vol. 68, No 3 (19811
Kanigen. ASTM STP No. 265, Electroless Nickel Plating 1959
Oak Ridge, D. D. Smith, Thermal Conductivity o f Electroless Nickel-Phosphorus Alloy Plating. National
Science Foundation, 1963
Gorbunova, K. M. Gorbunova and A. A. Nikiforova, Physicochemical
Principles of Nickel Plating, National Science Foundation. 1963
Vendor, Schering, unpublished analytical results. ScheringKG. Berlin 1982
Mallory, Glenn Mallory e t al, Studies and Properties of Very Hard Electroless Nickel Deposits.
EN'95. Gardner Management, Cincinnati. OH, 1995

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 X3. HARDNESS VERSUS HEAT TREATMENT

NICKELvs TEMPERATURE
HARDNESS OF ELECTROLESS vs TYPE

1000

900
I
800

700

600

500

II
, I l I

!I I
I I I I l
t I I
I I I l I
400
O 100 200 300 400 500

x4. ALLOY TYPES

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 B733
TYPES
HARDNESS MAGNETICS STRENGTH
O

I """"""""

3
4

5
6
P% P%
7

IO

II

12 12

13 I3

.-
IL IL
LOW HIGH LOW
NON HIGH FERRO
MAGNETIC
MAGNETIC

FmX4.1 ~~dA."Nldrd~co11Oho,by"

X5. SUMMARY PROGRAM 14

X5. I Results of 110 Month Exposure of Autocatalytic
Nickel Depsits at Kure Beach, North Carolina:
X5.1.1 Program 14 is part of an ongoing marine exposure
testing process atthe 75 m site at Lame Center for
Corrosion Technology, Wrightsville, NC (Kure Beach). The
program c a
U d for the plating of both Type N and Type V
deposits on standard smooth and ground steel Q PaneIs.
X5.1.2 There were nineMerent sources of deposits, each
providing five lots of five panels. The program involved
plating 12.5,25, and 75 Fm thicknesses on smooth and
ground surface and one smooth lotheat treated for hardness
at 550'C for 2 h. The heattreatment temperature was
considerably higher than typical processing and was chosen
to evaluatetheformation of diffusion products of iron,
nickel andphosphorus
X5.1.3 The following matrix of test panels were prepared
and exposed with subsequent analysis for alloy and thick-
ness. Panels were rated at Kure Beach each year by a team
from A!RM committee B 8 using Ractice B 537.
X5.1.4 The interpmtationof the results of these exposure
test should be made on the basis of general performance of
the coating on panels. Base metalcondition, undercoats,
surface prcparation,and post processing all have a signiscant
effect on the performance and should be given mreful
consideraton when designing the part and p&reatment
processing sequenœ.

10

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 S T D - A S T M B733-ENGL L797 W 0 7 5 7 5 3 0 Ob097LI2 72T

1 smooth No 125 3.6 f 3.0

2 smooth No 25 9 2 f 0.3
V G 3 smooth No 75 m5 105 109 10*0
4 smooth YeS 25 92 f O 3
5 Grand No 25 7.0 f 0.4
1 smooth No 12.5 0.0 f 0
2 smooth No 25 0.0 f 0
V E 3 smooth No 75 77 10.0 102 *
9.8 0.4
4 smooth YeS 25 8 2 f 0.8
5 Grand No 25 42 fO A
1 smaoth No 12.5 6.8 f 1.3
2 smooth No 25 6 2 f 0-4
V C 3 smooth No 75 46 9.9 10.4 8.0 f 1.1
4 smooth YeS 25 6.8 f 1.3
5 Grand No 25 0.0 f 0
1 smooth No 12.5 0.0 f o
2 smooth No 25 5.8 f 0.4
IV J 3 smooth No 75 9.0 9.6 f 1.1
4 smooth YeS 25 7.0 f o
5 Grand No 25 1.0f2
1 smooth No 125 0.6 f Ob
2 smooth No 25 7-4 f 0 9
IV 3 smooth No 75 8.9 10.0 f 0
4 smooth YeS 25 4.0 f 1.1
5 Grand No 25 0.0 f 0
1 smooth No 125 0.0 f 0
2 smooth No 25 1.8f 1.6
IV 3 SnKKml No 75 79 8.3 6.0 f 1.0 7.3
4 smooth YeS 25 5.0 f 0
5 (;rand No 25 0.0 f 0
1 smooth No 12.5 0.0 f O
2 smooth No 25 0.0 f 0
IV 3 smooth No 75 77 02 9.5 5.0 f 1A
4 smooth YeS 25 5.4 f 0.5
5 oand No 25 0.0 f 0
1 smooth No 125 0.0 f 0
2 smooth No 25 0.0 f 0
IV K 3 smooth No 75 75 0.6 f 0.8
4 smooth YeS 25 5.6 f 2.8
5 (jmud No 25 0.0 f O
1 smooth No 12.5 0.0 f o
2 srooth No 25 0 2 f 0.4
N I 3 smooth No 75 80 7.1 0.4 f O 5
4 smooth YeS 25 4.6 f 0.0
5 25

REFERENCES

(1) Symposium on ElectrolessNickel Plating, ASTM STP 265, A S M , 12644 Raearch Parkway, Orlando, R.32826, 1986 Chapter 23.
1959. (5) Mallory G., and Hajdu J. " E k ct
ros
l
Phtbg," AESF 12644
(2) Engineering Properties of Electroless Nickel, The International Research Parkway, Orlando, FL 32826,1990.
Nickel Co., Inc., New York, NY. (6) m,K., "Hardmss and Wear Redanœ Tests of F i k c t r o I e s
(3) Gawrilov, C. G.,Chemical (Electroless) Nickel Plating, Portcullis N i Deposi4" W i n g , Vd 61,September 1974.
ReSS, London, 1974. (7) P ar
ke r
, K. of Heat Treatment on thc Ropemes of
(4) Saiìanek, W. H.,The Properties of Electroakposited Metals Md Electrokss Nickel Plating and S@îî Finishing, Vol
Afloys, The American Electroplatersand Sud&ce Finishen Society, 68,December 1981.

11

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