ASTM B733

ADOPTION NOTICE

custodians:
h y " R
Navy - AS
Air Force - 11

Adopting Activity:
Air Force - 11
(Proj No. MFFP-0565)

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

4Tb

AMERICAN SOCIETY FOR TESTING AND MATERIALS

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

Designation: B 733 97

Standard Specification for

Autocatalytic (Electroless) Nickel-Phosphorus Coatings on

Metal'

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

ferromagnetic.
1.10 The values stated in SI units are to be regarded as
standard.
l . 1 1 The following precautionary statement
pertains only
to the test method portion, Section 9, of this specification.
This stan&ud does not purport to address all of the safety
comem, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate
safety and health practices and determine the applicability of
regulatoty limitations priorto use.

1. scope
t. 1 Thisspecificationcoversrequirementsforauto-

catalytic(electroless)nickel-phosphoruscoatingsapplied
from aqueous solutionsto metallic products for engineering
(functional) uses.
1.2 Thecoatingsarealloysofnickel
and phosphorus
producedbyautocatalyticchemicalreductionwith
h m
phosphite. Because the deposited nickel alloy iscatalyst
a
for
the reaction, the processis self-sustaining. The chemical and
physical propertiesof the depositvaryprimarilywithits
phosphoruscontentandsubsequentheattreatment.The
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
Refs (2) (3) (4) and (5) also refer to Figs. X 1.I,X 1.2, and
X 1.3 in the Appendixof Guide B 656.
1.3 Thecoatingsaregenerallydepositedfromacidic
solutions operatingat elevated temperatures.
1.4 The process produces coatings of uniform thickness
on irregularlyshaped parts, provided the plating solution
circulates freely over their surfaces.
1.5 The coatings havemultifunctional properties, such as
hardness, heat hardenability, abrasion, wear and corrosion
resistance, magnetics, electrical conductivity provide difusion barrier, and solderability. They are also used for the
salvage of worn or mismachined parts.
1.6 The low phosphorus (2 to 4 % P) coatings are
microcrystalline and possess high as-plated hardness (620to
750 HK 100). Thesecoatings are used inapplications
requiring abrasion andwear resistance.
1.7 Lowerphosphorusdepositsintherange
between 1
and 3 % phosphorus are also microcrystalline. These coatings are used in electronicapplicationspro,yidingsolderability,bondability,increasedelectricalconductivity,
and
resistance to strong alkali solutions.
1.8 The medium phosphorous coatings ( 5 to 9 96 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
partsfor low stressproperties.Coatings with phosphorus

2. R e f e r e d Docoments

2.1 ASTM Standardr:

B 368 Test Method for Copper-Accelerated Acetic AcidSalt Spray (Fog) Testing (CAS Testing)3
B 374 Terminology Relatingto Electroplating3
B 380 Test Method ofCorrosion by the Corrodkote
P r d d
B 487 Test Method for Measurementof Metal and Oxide
Coating Thicknessesby Microscopical Examinationof a
Cross W o n 3
B 499 Test Method for Measurement of Coating Thicknesses by the Magnetic M e t h d Nonmagnetic Coatings
on Magnetic Basis Metals3
B 504 Test MethodforMeasurementofThicknessof
Metallic Coatings by the CoulometricMethod3
B 537 Practice for Rating of Electroplated Panels
Sub
jeCtea to Atmospheric Expos&
B 567 Method for Measurement of Coating Thickness
by
the Beta Backscam Method3
B 568 Method for Measurement of CoatingThicknes by
X-Ray Spectrometry3
B 571 Test Methods for Adhesion of Metallic Coatings3
B 578 Test Method for Microhardness of Electroplated
Coatings3
B 602Test Method for Attribute Sampling
of Metallic and
Inorganic Coating?
B 656 Guide for Autocataytic Nickel-Phosphorus
Deposition on Metals for Engineering U&
B 667 Practice for Construction and Use of a Prok for
Measuring Electrical Contact Resistance4
B 678 Test Method for Solderability of MetalliGCoated
Products3

'

This specitication is under (he jurisdiction of ASIM Cornmittee Bo8 an

Metal Powders and Metal Po&
Products and is tbe. direct responsibility of
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
end of the text

A
A

1
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the coating must protect fiom corrosion or w

e
a
r
, or both,
and that are esential to the performance.
3.2 Other D&itiom-Terminology
B 374 defines most
of the technical terms used in this specification.

B 697 Guide for Selection of Sampling Plans for Inspection of Electrodeposited

Metallic
and
Inorganic
Coatings3

B 762 MethodforVariableSamplingofMetallicand
Inorganic Coatings3
B 849 Specification for Pre-Treatmentof Iron or Steel for
Reducing the Risk of Hydrogen Embrittlement3
B 850 Specification for Post-CoatingTreatments
of
Iron or SteelforReducing
the Risk ofHydrogen
Embrittlement3
B 851 Specification for AutomatedControlledShot
PeeningofMetallicArticles
Prior to Nickel, Autocatalytic Nickel, Chromium, orAs A Final F e h 3
D 1 193 Specification for Reagent W a t d
D 2670 Method for Measuring Wear Roperties of Fluid
Lubricants (Falex Method)'
D 27 14 Method forCalibration and Operation of an Alpha
L F W - 1 Friction and Wear Testing Machin&
D 395 1 practice for Commercial Packaging7
D 4060 Test Method for Abrasion Resistance of organic
Coatings by the Taber A b d
E 60 Practice for PhotometricMethods for Chemical
Analysis of Metalsg
E 156 TestMethodfor
Determination of PhosphoNS inHigh-Phosphorus Brazing Alloys (Photometric
Method)Io
E 352 Test Methods for ChemicalAnalysis of Tool Steels
and Other Similar Medium-and High-Alloy Steel'
F 519 Test MethodforMechanicalHydrogenEmbrittlement I
G5 Practice for Standard Reference Method for Making
PotentiostaticandPotentiodynamicAnodicPolarization Measurementst2
G 31 Practice for LaboratoryImmersionCorrosion
Testing of Metals12
G 59 Practice for Conducting Potentiodynamic Polarization Resistance Measurements12
G 85 Practice for Modified Salt Spray(Fog) Testing''
2.2 Military Standards:
MLR-81841 Rotary Flap Peening of Metal P a d 3
"S13165 Shot Peeningof Metal Parts13
"STLl-109 Sampling procedures and Tables for Inspection by Attribute"
2.3 I S 0 Stanazrds:
IS0 4527 Autocatalytc Nickel-Wosphorus CoatingsSpecification and Test Meth0dd4

3. Termindlagy
3.1 DeJirrition:
3. l. 1 significant su$bces-those

4. contingchapifuction
4.1 The cuating dadication system provides for a
scheme to select an elechroless nickelcoatingto meet specific
performance requkments based on alloycomposition,
thickness and hardness.
4.1.1 TYPE describes the general composition of the
deposit with respectto the phosphorus content and is divided
into five categories which establish deposit properties (see
Table 1).
NOTE
. . 1-h" to the pmckion of some phosphorus analysismethods
a&v1at~mof0.5%hpbeendesigecdintothisdarrificetionscbane.
Roundingoftktcatresultsduttothe~ofthclimitspmrideJ
foran~limaofCSand9.5%~~.ForQCampk.~

withatestresultfar~of9.71wouldhaveaclasgificatiollof
TYPE V, stt Appeaaix 4, M o y TYPES.

4.2 Service Condition Based on Thickness:

4.2.1 service condition n u m b are based on the severity
of the exposure in which the coating is intended to perform
and minimum coating thickness to provide satisfi&%ory
performance (seeTable 2).
4.2.2 SC0 Minimum Service, 0.1 pm-This is defined by
a minimum coating thickness to provide specific material
properties and extend the life of a part or its finction.
Applications include requirementsfordiffusion
barrier,
undercoat, electrical conductivity and wear and c o d o n
protection in specialized environments.
4.2.3 SC1 Light Mice, 5 pm-This is debed by a
minimum coating thickness Of 5 pm for extending the life of
the part. Typical environments includelight-load lubricated
w
e
a
r
, indoor c o d o n protection to prevent rusting, and for
soldering and mild abrasive wear.
4.2.4 SC2 Mild Mice, 13 pm-This is defined by mild
c o d o n and wear environments. It is &am&xid by
industrial atmosphere exposureon steel substrates in dry or
oiled environments
4.2.5 SC3 Moderate Service, 25 Pm-This is defined by
moderate environments such as non marine outdoor exposure,alkaIi salts at elevated temperature,and moderate wear.
4.2.6 X 4 Severe Service, 75 pm-This is defined by a
very aggnssive environment. Typical environments would
indude acid solutions, elevated t
empemm and pressme,
hydrogen diide and carbon dioNde oil service, hightemperam chloride systems, very severe w
e
a
r
, and marine

substrate surfaces which

immersioa
Nars2-"Ihe~oftherutocoEllytic~caatingdb

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Licensed by Information Handling Services

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B 733
TABLE2 senicecondilions
Coating TNdrnert Requirrnnents
secvicecondipbn

Minmuncoating
Thidcness

specificetan
M
r
iL
n
r
n
-

Sc0
SC1
SC2

Light service

Sc3

Modmatesenice

Sc4

severeservice

hwservice

m
. (m)

0.1
5
13

o.-(
~.oO02

(
(

25
75

0.001
0.m

( )
( )

o.O@x

1
1
1

and how it was pretreated. Rough, non uniform wrfces require thicker
coatings than smooth surfaces to achieve maximum corrosion
and minimum porosity.

4.3 Post Heul Treatment Class-The nickel-phosphorus

coatings shall be classified by heat treatment after plating to
increase coating adhesion and or hardness (seeTable 3).
4.3.1 Class I-"deposited, no heat treatment.
4.3.2 Class 2-Heat treatment at 260 to 400C to produce
a minimum hardness of 850 HKIOO.
4.3.3 Class 3-Heat treatment at 180 to 200C for 2 to 4
h to improve coating adhesion on steel and to provide for
hydrogen embrittlement relief (see 6.9).
4.3.4 Class 4-Heat treatment at 120 to 130C for at least
1 h to increaseadhesion ofheat-treatable(age-hardened)
aluminum alloys and carburizedsteel (see Note 3).
4.3.5 Class 5-Heat treatment at 140 to 150C for at least
1 h to improve coating adhesion for aluminum, non
agehardened aluminum alloys, copper, copperalloys and beryllium.
4.3.6 Class 6-Heat treatment at 300 to 320C for at least
1 h to improve coating adhesionfor titanium alloys.

5.1.1 Title, ASTM designation number, and year of issue

of this specification.
5. I .2 Classification of the deposit by type, seMce condition, class, (see4.1, 4.2 and 4.3).
5.1.3 Specify maximum dimensionand tolerance requirements, if any.
5.1.4 Peening, if required (see6.5).
5.1.5 Stress relief heat treatment before plating, (see 6.3).
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.
5.1.8 Supplementalor Special Government Requirements
such as, specific phosphorus content,abrasion wear or
corrosion resistaace of the coatin& solderability, contact
resistance and packagingselectedfirom Supplemental Requirements.
5.1.9 Requirement for a vacuum, inert or reducing a t m e
sphere for heat treatment above 26032 to prevent surface.
oxidation of the mating (see S3).
5. l. 10 Test methods for coating adhesion, composition,
thickness, porosity, wear and corrosionresistance, if required, selected from those found in W o n s 9 and Supplemental Requirements.
5. l . 1 1 Requirements for sampling (seeSection 8).
N m 4" purchasa should furnish separate test specimens or
coupons of the basis metal for test purposes to be plated concurrently
with the articIes to be plated (see 8.4).

6. Materials and Mandacture

6.1 Substrate-Defects in the surface of the basis metal

such as scratches, porosity, pits,inclusions, roll and die
marks, laps, cracks, bum, cold shuts, and roughness may
advemly affect the appearance and performan of the
deposit, despite the observan of the best plating practice.
Any such d e f m on signifc8nt surfaces shall be brought to
the attention of the purchaser before plating. The producer
shall not be responsible for coatings defects resulting h m
s u r f a conditions of the metal, ifthese conditions have been
brought to the attention of the purchaser.
6.2 Pretreuttment"parts to be autocatalytic nickel plated
B656. A
may be pmtreated in accordancewithGuide
suitable method shall activate the surface and remove oxide
and foreign materials, which may cause poor adhesion and
coating porosity.

N m 3-Heat-treatablealuminum alloys such as Type 7075 can

undergo microstructural changes and lose strength when heated to over
130'C.

5. Ordering Information
5.1 The following information shall be supplied by the
purchaser in either the purchase order or the
on engineering
drawing of the part to be plated:
TABLE 3 ClassilicaiionoiPostHeatTreabnent
CLASS
1
2

oescription

5
6

N m 5-Heat treatment of the base material may effect its metallurgical p

r
o
p
e
x
t
e
i An example is leaded steel which may exhibit liquid
or solid embritUement after heat treatment. Careful selection of the pre
and post heat treatmeatsare recommended.

20

6.3 Stress Reli&

6.3.1 Pretreatntent of Iron und Steelfor Reducing the Risk
of Hydrogen Embrittlement-Parts that are made of steel
with ultimatetensilestrength of greater than IO00 Mpa
(hardness of 31 HRC or greater), that have been machined,
to heat
ground, coldformed,or cold straightened subsequent
treatment, shall require stress relief heat treatment when
specified by the purchaser, the tensile strengthto be supplied
by the purchaser, Specification B 849 may be consulted for a
list of premtments that are widely used.
6.3.2 Peening-Peening prior to plating may be required
on high-st~~ngth
steel parts to induce residual compressive

IieatTrearmentforMaXinun

NPII

Tm@)

No Heat Treatment, As Plated

Hardness
TYPE I

CC)

TYPE 111
TYPE IV
TYPE V
HvaogenEmbrittlementand
Adhes*n on steel

A&esim.carbwidsteeland

" egA
AdhesbnmBerycunand
Aluminum
AdhesanOnTrtaniun

260
285

320
400
350t0380
36ot0390
366to400
375 to 400

16

18oto200

1
1
1
1
1
2to4

120to130

1-6

140 to 150

lto2

300-320

I 4

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~~

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

@ B733
6.8.2 See Appendixes 3 and 4 and Guide B656 Fgs
stresses in the sudace, which can redu loss offatigue
strength and improvestress corrosion resistance after plating, X1.2 and X1.3.
6.8.3 A heat treatment at 260C for greater than 20 h
(See Supplementary Requirements).
sho~dbeusedtoreduthelossofsurfacehardn~and
6.3.3 Steel parts which are designedfor unlimited life
strength of some ferrous basis metals. Avoid rapid heating
underdynamicloads shall be shot peened or rotary flap
and cooling of plated pouts.Suffiicient time must be allowed
peened.
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~~

mquireb~timcorahigbertem~orboth.Iadividualalloys
should be tested for maximum hardness attainaMe, especially for
COIlditi~Ofandloaggtima.

6.3.3.1 Unless otherwise specited, the shot peening shall

be accomplished on all s u r k a for which the coating is
required and all immediateadjacent surfces whenthey

~8-rncrtorreducingatmosphereor~umsufficientt0

contain notches, fillets, or other abrupt changes of section

size where stresses will be concentrated.
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
uniform coating thickness. The location ofrack or wire
marks in the coating shall be agreed upon betwen the
producer and purchaser.
6.5 Plating Process:
6.5.1 To obtainconsistent coating properties, the bath
must be monitored periodically for pH, temperature, nickel
and hypophosphite. Replenishments to the plating solution
should be as frequent as required to maintain the concentration of the nickel and hypophosphite between90 and 100 %
of set point. The use of a statistical regimento establish the
control limits and frequency of analysis may be employed to
ensure quality deposits are produced.
6.5.2 Mechanical movement of parts and agitation of the
bath is recommended to increase coating smoothness and
uniformity and prevent pittingor StreaLing due tohydrogen
bubbles.
6.6 Post Coating Treatment for Iron and Steel for Reducing the Risk of Hydrogen Embrittlement-Parts that are
made of steel with ultimate tensile strengths of 10oO Mpa
(hardness of 3 I HRC or -ter),
as well as surface hardened
p a r t s y shall require post coatinghydrogenembrittlement
relefbakingwhen specified by the purchaser, the tensile
strength to be supplied by the purchaser. SpecificationB 850
may be consulted for a list of post treatments that are widely

~toxidpoionisrrawmendedforheattreatmentrbovc26oxDo
notusegasam~hydrogenwithhigh~stedparts

7. Requirements
7.1 fiocm-Tbe coating shall be produced h m an
aqueous solution through chemical reduction reaction.
7.2 AcxqMam? Requiren?entsThese requirements are
placed on each lot or batch and can be evaluated by testing
the plated part.
7.2.1 Appearance:
7.2.1.1 The coating surface shall have a d o r m , metallic
appearan withoutvisible d e f a such as blisters, pits,
pimples, and m
k
s (see9.2).
7.2.1.2 Imperfctions that arise from surface conditions of
the substrate which the producer is unable to remove using
conventional pretreatmenttechniques and thatpersist in the
coating shall not be cause for rejection (see 6.1). Also,
discoloration due to heat treatment shall not be cause for
rejection unless special heat treatment atmosphere is specified (see5.9).
7.2.2 Thkksts-The thickness of the coating shall exceed the minimum requirements in Table 2 as specified by
the serv condition agreed to prior to plating (see 9.3).
Aftercoatingandifspecified,thepartshallnotexceed
maximum dimension on signiscant surface (see5.3).
NOIE9--The~oftbecoatingcannotbecontrolledinMind
orsmalldiameterdeepholcsorwheresolutioncirculationisrcstricted

used.

7.2.3 Adhesion-The coating shall have sufficient adhe

sion to the hasis metal to pas the specified adhesion test (see
9.4 and Test Methods B 571).
7.2.4 PorositpThe coatings shall be essentiauy porefree
when tested Bccording to one ofthe methods of 9.6. The test
method, the duration of the test, and number of allowable
spots per unit axa shall be specified (see5.10 and 9.6).
7.3 Qual@cation Requirements-These requirements m
placed on the deposit and process and are performed on
specimens to qual@ the deposit and plating process Tbe
tests for these qualification requirementsshall be performed
monthly or more kquentIy.
7.3.1 Conrparition-Tm II, m,IV, V deposits shall be
analyzed far alloy composition by testing for phosphorus(see
9.1). The weight percent of phosphorus shall be in the range
designated by type dassitication (see4.1).
microhardnesp of Class 2 de7.3.2 Mb-me
posits shall be determined by Test Method B 578 (KMIOP).
ForClass2~themim~nessshalleq~orexceed
a minimum of 850 (HK100 (or equivalent Vickers) (see4.3

6.6.I Heat treatment shall be p e r f i i e d preferably within

1 h but not morethan 3 h of platingon plated after plating of
steel parts to redu the risk of hydrogen embrittlement. In
all cases, the durationof the heat treatment shall commence
from the time at which the whole of each part attains the
specified temperature.
6.6.2 High-strength steelpartswith actual t e d e strengths
greater than loo0 MPa (correspondinghardness values 300
HV10,303 HB or 31 HRC) and s d k e hardened parts shall
be pn>cessed after coating in accordance with speciscation
B 850.
6.7 Heat Treatment After Plating to Improve AdhesionTo improve the adhesion of the coating to various substrats,
the heat treatments in Table 3 should be performed as soon
as practical &el plating (see 4.3).
6.8 Heat Treatment ABer Plating to Increase Hurdms:
6.8.1 To increase the hardness of the coating a heat
treatment of over 260.C is requid. Table 3 describes the
heat tnatment for maximumhardness.
4
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and 9.5).The conversion of Vickers to Knoop using Tables

E 140 is not recommended.
7.3.3 Hydrogen Embrittlement-The process
used to deposit a coating ontohigh strength steels shallbe evaluated for
hydrogen embrittlement by Test Method F 5 19.

tion, emission or X-ray fluorescence spectrometry.

N m 12"Inductively coupled plasma techniques can determine the

alloy to within 0.5 Om.The foUowing analysis wavelength lines have bee0
ued with minimum interfaence to determine thealloy.

Ni 216.10 nm
P 215.40 nm
P 213.62 nm

Cd 214.44 nm
CD 238.34 nm
Cr 284.32 om
Cu 324.75 nm

Fe 23820 nm
Pb 283.30 nm
Sn 198.94 nm
Zn 206.20 om

8. Sampling
Al 202.55 nm
8.1 Thepurchaserandproducer
are urged to employ
9.2 Appearance-Examine the coating visually for comstatisticalprocesscontrol 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.
N m 13-Eddy-cummt type instruments give enatic measurements
8.1.1 Sampling plans can only screen out unsatisfactory
due to variations in conductivity of the coatings withchanges in
productswithout assurance thatnone ofthem will be
phosphorus content.
accepted. (7)
9.3.I Microscopicd Method-Measum the coating thick8.2 Thesamplingplan
used for theinspection of a
ness of a cross section accordingto Test Method B 487.
quantity of coated parts (lot) shall be Test Method B 602
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
on
lot 8.2) is examined for compliance with the requirements placedthe
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
mass 96 phosphorus (not ferromagnetic) and that have not
or not complying with the requirements
based on the results of the
been heat-treated The instrument shall be calibrated with
inspection sample.The size of the sample andthe criteria of compliance
deposits plated in the same solution under the same condiare determined by the application of statistics. The procedure is known
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,magneTest Method B 602 contains four sampling plans, three for use with
sium, and titanium. The instrument mustbe calibrated with
tests that are nondestructiveandonefor
use with tests that are
standards having the same compositionas the coating.
destructive. Thepurchaserand prcdur may
on the plants) to be
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 (SeeAppend X2).
on the selection ofa plan. When Guide B 697 is specified, the purchaser
9.3.4 Micrometer Meth0d"Measu-e the part, test
and producer need to agree on the plan to be used.
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
9.3.5 Weigh. Plate, Weigh Meth0d"Using a similar sub
calculating plans to meet s p i a l needs The purchaser and producer
strate material of known surface area, weigh to the neafest
may agree on the plan(s)to be used. If they do not, Test Method B 762
milligram before and after plating makingsure that the part
idenfifies the plan to be used.
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
coating thickness, Fm = 10 W/(A X D)
submitted for aczeptanor rejection as a group.
8.3 All specimens used in the sampling plan for a m p
tance tests shall be made of the same basis material and in
the same metallurgical condition as articles being plated to
this specification.
8.4 AU specimens shall be providedby thepurchaser
unless otherwiseagreed to by the producer.

where:
W = weight gain in milligrams,
A = total swface area in square centimetres, and
D = grams per cubic centimetres(seeAppendix X).
9.3.6 Coulometric Method-Measure thecoatingthickness in accordancewith Test Method B 504.The solutionto
be used shall be in accordanoe with mandachmr's m m mendations. The surface of the coating shall be cleaned prior
to testing (see Note 14).
9.3.6.1 Calibrate standard thickness specimens with de+
posits plated in the same solution under the same conditions.
9.3.7 X-Ray Spectrometry-Measure the coating thickness in accordance withTest Method B 568.The instrument
must be calibrated with standards having the same composition as the coating.

NOTEI I-The autocatalytic nickel pnxzss is dynamic and a daily

sampling is recommended. For h
q
i
tgrequiring alloy analysis and
corrosion testing weekly sampling should be considered as an option.

9. Test Methods
9.1 Deposit Analysis for Phosphorus:
9.l . 1 Phosphorus Determination-Determine mass ?&
phosphoruscontentaccording
to Practice E 60, Test
Methods E 352, or Test Method E 156 on known weight of
deposit dissolved in warm concentrated nitric acid.
9.1.2 Composition can be determined by atomic absorp-

N m I b T h i s method is only realmmended for deposits in the

asplated condition. The phasphorus content of the coating must be
5

COPYRIGHT American Society for Testing and Materials

Licensed by Information Handling Services

~.

~~

~~

S T D - A S T M B733-ENGL 1777 D 0757530 Ob07737 Sb2

B733
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

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

Po=.

9.4 Adhesion:

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-

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 inteda of the coating and basis metal to
determine the adhesion is suggested.

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
llulosein90mLofboilingwatatowhich,afhcooling,
O. 1 g sodium alizarin MOM^, dissolved in 5 mL of ethanol
isadded.After4mincontaa,apply~aticaciduntil
thevioletcdordisappearsAnyredspots~indicate
Po9.6.5 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
Uulosein9OmLofboilingdistilledwater.Theappearan
0fbrownspotsafter2minindicatepores.
9.7 Other Test Method-Test methods which have been
developedthatareequaltoorbetterthanthesemaybe
substituted. The w o n and bias requimnents will vary

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 hicrokrdness-The microhardness of the coating
can be measured by Test Metbod B578 using Knmp
indenter and is reported in Knoop Hardnes Number
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 minimum coating thickness of 75 pm is recommended. Conversions of Vickm or Knoop hardness number to Rockwell C is
not recommended.
NOTE1 8 4 thick (75 Fm+) cuatings on steel a surface

(HK).

foreachtypeoftestIfanalternatetcstisspecifieditshallbe
agreeduponbctwecntheprodurandthcpwchaser.
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

microhardnessdetermination is permissible.

be rejected.

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-Completely immerse the part to be treated in a vessel filled with
aerated water at m m tempemture. Apply heat to the beaker
atsucharatethatthewa~beginstoboilinnotlessthan15

11. c k r t i f i i

contract,areportofthetestresultsshallbefurnished.
12 Keywords
12.1 autmatalytiq chemical nickek coati-,
conductive;
c o d o n resistance; electrolq functional, nickeknickel
Phosphorus;"

6
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services

11.1 Whenspecifedinthepurchaseorderorcontmct,the
purchaser shall be lmished certitication that the samples
representing each lot have b n proased, tested and inspected as directed in this specification and the quirements
been met. When specifiedin the purchase oder or

SUPPLEMENTARY REQUIREMENTS

The following supplementary requirements shall applyonlywhen

contract or order.

S1.1 Shot Peening-When specified by

the purchaser in
the ordering information, the part@) shall be shot peened
prior to plating in accordance with Specification B 85 1 or
MILS13165
S1.2 Composition-When specified by thepurchaserin
the ordering information the phosphorus content shall be
maintainedinthedeposit
to within 1 % . Use the test
methods described in9. l.
S 1.3 Inert Atmosphere-When specified by the purchaser
shall be heat treated
in the ordering information, the coating
in avacuum,inert,
or reducingatmosphere to prevent
surface oxidation of the coating.
S1.4 HydrogenEmbrittlement-Whenspecifiedby
the
purchaser in the ordering information the plating process
shall be evaluated at thetime
of processingpartsfor
hydrogen embrittlement using Test Method F 5 19.
S1.5 Abrasive Wear-When specified by the purchaser in
shall be testedfor
theorderinginformation,thecoating
abrasion wear resistance using the method in Appendix X1
of thisspecification.Thecoating
shall meetamaximum
wear rate which is specified by the purchaser and agreed to
by the producer.
S I .6 Adhesive Wear-When specified by the purchaser in
the orderinginformation,thecoating
shall be testedfor
adhesive wear resistance using Test Method D 27 14or Test
Method D 2670. The wear rate shall bespecified by the
purchaser andagreed to by the producer.

specified by thepurchaser in the

S1.7 Conlact Resistance-When

specified by thepurchaser in the ordering information, the coating shall be tested
for contactresistance using Test MethodB 667.
S1.8 sOldetabi1ity"when specified by the purchaser in
the ordering information, the unaged coating
shall pass Test
Method B 678 on solderability.
S1.9 Corrosion Resistance-When specified
by the purchaser in the ordering information the coating
shall pass any
special corrosion tests agreed to by theproducer. The
corrosion resistance of thecoating to aspecificliquid
medium can be determined by means of immersion tests (see
practice G 3 I ) or electrochemical test (seePractices G 5 and
G 59).
S1.10 Pitting Corrosion Resiszance-Use Method G 85
(aceticacid-saltspraytest),Method
B 368 (copper-accelC M ) , or Method B380
eratedaceticacid-saltspray,
(Corrodkote) to evaluatethe c~rrosionresistance of the
coating to pitting
S l. 11 Special Government Requirements:
Sl. 1 l . 1 Sampling-Part(s) plated for theUS Government
and Military use shall use MILSTD-105 as the sampling
plan.
S1.11.2 Shot P e e n i n g "
strength steel part($ p m
cessed for US Government and Military use shall be shot
peened in acconiance with -13165
orrotary flap
peened in aa;ordancewith Mil-R-8 184l. (seeNote 6).
SI. 1 1.3 Puckugin"parts shall be packaged in accordanq with Practice D 3951.

APPENDIX

(Nonmandatory Information)

XI. TABER ABRASER WEARTEST"I0D

x1.1 scope
X1.2 Apparatus
X l . l. 1 This test methodw
l
ievaluate 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

panel aller each l o 0 0 cycles for weightloss. Duration of the
test is 6000 cycles and itcan be extended to 25 O00 cycles for
more complete results.
NOTEX1.I-Variation in results have been attributed to the hu-

vacuum.
X1.2.2 Abrasion Wheels-Use Cs10 (resilientrubber)
Taber wheels. To reface the wheels use CS-1 1 discs fkom
Taber. The hardness of CS10 wheels can change with time
and can effect thereproducibility of results(seeTest Method
D 4060).
X1.2.3 TestSpecimens-Test
specimens shall be made
fiom 20 gage CR stee.14 by 4 in. (100 by 1 0 0 by 1.3 mm)
with a 0.250 (6.35 mm) hole in the center. Test specimens
are available fiom Taber.
X1.2.4 Analytical Balance-Scalewhich
is capable of
measuring to 150 g k O. 1 mg.

midity in the laboratory and the storage conditions of the CS10 wheels.

Care should be.taken to control the humidity between tests.

X l . 1.2 The w d t s are variable between tests and therefore three plated test specimens should be tested
to 6000
cycles each. The results should be averaged withoutthe lrst
l o 0 0 cycles and the abrasion wear resistance is reported as
the weight loss in mg/1000cycles (Taber Wear Index).
7
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services

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

of 6OOO cycles bave been accomplished for eacb
specimen.
total

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

COPYRIGHT American Society for Testing and Materials

Licensed by Information Handling Services

X3. HARDNESS VERSUS HEAT TREATMENT

HARDNESS OF ELECTROLESS
NICKELvs TEMPERATURE
vs TYPE
1000

900

800

700
600
500
II
t

400

100

200

I
I

300

x4. ALLOY TYPES

9
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services

l
l

!I

400

500

B733
TYPES
HARDNESS MAGNETICS

STRENGTH

"
"
"
"
"
"
"
"

3
4

5
6
P%

P%

7
8
9

IO
II

12

12

13

I3

.-

IL

IL

LOW

HIGH

LOW
NON

FERRO

HIGH
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

10
COPYRIGHT American Society for Testing and Materials
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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 thickness. 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 sequen.

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

1
2
3
4
5
1
2
3
4

1
2
3
4

5
IV

1
2
3
4

5
1
2
3
4
5

IV

IV

IV

IV

2
3
4
5
1
2
3
4
5
1
2
3
4
5
1

smooth
smooth
smooth
smooth

No
No
No

125
25
75

YeS

25
25
12.5

smooth

No
No

smooth

No

smooth
smooth

No

Grand

25
75

smooth
Grand

YeS

smooth
smooth
smooth

No

No
No

25
25
12.5
25
75
25
25
12.5
25
75

smooth
Grand
smooth

YeS

25

smooth

No
No
No
No

smooth

YeS

Grand

No
No
No
No

25
125
25
75
25
25
125
25
75
25
25
12.5
25
75
25
25
125
25
75
25
25
12.5
25
75
25
25

Grand

smaoth
smooth
smooth

smooth

YeS

No
No
No
No
No

smooth
smooth
SnKKml
smooth

YeS

(;rand

No

smooth

No
No
No

smooth

smooth
smooth
oand

smooth
smooth

YeS

No
No
No
No

smooth
smooth

YeS

(jmud

No

smooth

No

srooth

3
4

smooth
smooth

No
No
YeS

m5

105

109

77

10.0

102

46

9.9

10.4

9.0

8.9

79

8.3

77

02

75

80

7.1

9.5

3.6 f 3.0
9 2 f 0.3
10*0
92 f O 3
7.0 f 0.4
0.0 f 0
0.0 f 0
9.8 0.4
8 2 f 0.8
42 fO A
6.8 f 1.3
6 2 f 0-4
8.0 f 1.1
6.8 f 1.3
0.0 f 0
0.0 f o
5.8 f 0.4
9.6 f 1.1
7.0 f o
1.0f2
0.6 f Ob
7-4 f 0 9
10.0 f 0
4.0 f 1.1
0.0 f 0
0.0 f 0
1.8f 1.6
6.0 f 1.0
5.0 f 0
0.0 f 0
0.0 f O
0.0 f 0
5.0 f 1A
5.4 f 0.5
0.0 f 0
0.0 f 0
0.0 f 0
0.6 f 0.8
5.6 f 2.8
0.0 f O
0.0 f o
0 2 f 0.4
0.4 f O 5
4.6 f 0.0

REFERENCES
(1) Symposium on ElectrolessNickel Plating, ASTM STP 265, A S M ,

12644 Raearch Parkway, Orlando, R.32826, 1986 Chapter 23.

(5) Mallory G., and Hajdu J. "
E
k
c
t
r
o
s
l
Phtbg," AESF 12644

1959.
(2) Engineering Properties of Electroless Nickel, The International
Nickel Co., Inc., New York, NY.
(3) Gawrilov, C. G.,Chemical (Electroless) Nickel Plating, Portcullis
ReSS, London, 1974.
(4) Saianek, W. H.,The Properties of Electroakposited Metals Md
Afloys, The American Electroplatersand Sud&ce Finishen Society,

Research Parkway, Orlando, FL 32826,1990.

(6) m,K., "Hardmss and Wear Redan Tests of F i k c t r o I e s
N i Deposi4" W i n g , Vd 61,September 1974.
(7) P
a
r
k
e
r
, K.
of Heat Treatment on thc Ropemes of
Electrokss Nickel
Plating and S@ Finishing, Vol
68,December 1981.

11
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7.3