ASTM B733

ADOPTION NOTICE
custodians:
Navy - AS
Air Force - 11
h y " R
Adopting Activity:
Air Force - 11
(Proj No. MFFP-0565)
Review activity:
Air Force - 99
AREA MFFP
AMSC NIA
DISTRJBUTION STATEMENT A. Approved for public release; distribution is unlimited.
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services
STD-ASTM B733-ENGL 3777 W 0757530 Ob04732 TAU m
4Tb
Designation: B 733 - 97
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken. PA 19428
Repmted froml he Amua1 Book of ASTM StardardS. Copyright ASTM
Standard Specification for
Autocatalytic (Electroless) Nickel-Phosphorus Coatings on
Metal'
1. scope
t. 1 This specification covers requirements for auto-
catalytic (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
produced by autocatalytic chemical reduction with h m
phosphite. Because the deposited nickel alloy is a catalyst for
the reaction, the process is self-sustaining. The chemical and
physical properties of the deposit vary primarily with its
phosphorus content and subsequent heat treatment. The
chemical makeup of the plating solution and the use of the
solution can af f ect 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 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 irregularly shaped parts, provided the plating solution
circulates freely over their surfaces.
1 .5 The coatings have multifunctional properties, such as
hardness, heat hardenability, abrasion, wear and corrosion
resistance, magnetics, electrical conductivity provide di f u-
sion 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 (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
and 3 % phosphorus are al so microcrystalline. These coat-
ings are used in electronic applications pro,yiding solder-
ability, bondability, increased electrical conductivity, 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
parts for low stress properties. Coatings with phosphorus
' 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 Eogi nmi ug coatingr
Current edition approved July IO, 1997. Published October 1997. ori gi oauy
published as B 733 - 84. Last previous edition B 733 - 90 (1994).
The boldface numbm given in parentheses refer to a List of references at the
end of the t ex t
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 responsi-
bility of the user of this standard to establish appropriate
safety and health practices and determine the applicability of
regulatoty limitations prior to use.
2. Ref ered Docoments
2.1 ASTM Standardr:
B 368 Test Method for Copper-Accelerated Acetic Acid-
Salt Spray (Fog) Testing (CAS Testing)3
B 374 Terminology Relating to Electroplating3
B 380 Test Method of Corrosion by the Corrodkote
P r d d
B 487 Test Method for Measurement of Metal and Oxide
Coating Thicknesses by Microscopical Examination of a
Cross Wo n 3
B 499 Test Method for Measurement of Coating Thick-
nesses by the Magnetic Methd 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 Sub
jeCtea to Atmospheric Expos&
B 567 Method for Measurement of Coating Thickness by
the Beta BackscamMethod3
B 568 Method for Measurement of Coating Thicknes by
X-Ray Spectrometry3
B 571 Test Methods for Adhesion of Metallic Coatings3
B 578 Test Method for Microhardness of Electroplated
B 602 Test Method for Attribute Sampling of Metallic and
B 656 Guide for Autocataytic Nickel-Phosphorus Deposi-
B 667 Practice for Construction and Use of a Prok for
B 678 Test Method for Solderability of MetalliGCoated
Coatings3
Inorganic Coating?
tion on Metals for Engineering U&
Measuring Electrical Contact Resistance4
Products3
A d Book ofASTM &anh&, Vd 0205.
A d Bod ofAS7" &anh&, Vol 03.W.
1
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services
B 697 Guide for Selection of Sampling Plans for Inspec-
tion of Electrodeposited Metallic and Inorganic
Coatings3
B 762 Method for Variable Sampling of Metallic and
Inorganic Coatings3
B 849 Specification for Pre-Treatment of Iron or Steel for
Reducing the Risk of Hydrogen Embrittlement3
B 850 Specification for Post-Coating Treatments of
Iron or Steel for Reducing the Risk of Hydrogen
Embrittlement3
B 851 Specification for Automated Controlled Shot
Peening of Metallic Articles Prior to Nickel, Auto-
catalytic Nickel, Chromium, or As A Final F eh3
D 1 193 Specification for Reagent Watd
D 2670 Method for Measuring Wear Roperties of Fluid
D 27 14 Method for Calibration and Operation of an Alpha
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 Photometric Methods for Chemical
Analysis of Metalsg
E 156 Test Method for Determination of Phospho-
NS in High-Phosphorus Brazing Alloys (Photometric
Method)Io
E 352 Test Methods for Chemical Analysis of Tool Steels
and Other Similar Medium-and High-Alloy Steel'
F 519 Test Method for Mechanical Hydrogen Embrit-
tlement I
G5 Practice for Standard Reference Method for Making
Potentiostatic and Potentiodynamic Anodic Polariza-
tion Measurementst2
G 31 Practice for Laboratory Immersion Corrosion
Testing of Metals12
G 59 Practice for Conducting Potentiodynamic Polariza-
tion Resistance Measurements12
G 85 Practice for Modified Salt Spray (Fog) Testing''
2.2 Military Standards:
MLR-81841 Rotary Flap Peening of Metal P ad3
"S13165 Shot Peening of Metal Parts13
"STLl-109 Sampling procedures and Tables for In-
2.3 I S0 Stanazrds:
IS0 4527 Autocatalytc Nickel-Wosphorus Coatings-
Lubricants (Falex Method)'
LFW- 1 Friction and Wear Testing Machin&
spection by Attribute"
Specification and Test Meth0dd4
3. Termindlagy
3.1 DeJirrition:
3. l . 1 significant su$bces-those substrate surfaces which
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the coating must protect fiom corrosion or wear,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.
4. contingchapifuction
4.1 The cuating dadication system provides for a
scheme to select an elechroless nickel coating to meet specific
performance requkments based on alloy composition,
thickness and hardness.
4.1.1 TYPE describes the general composition of the
deposit with respect to 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 analysis methods
a&v1at~mof0.5%hpbeendesigecdintothisdarrificetionscbane.
Roundingoftktcatresultsduttothe~ofthclimitspmrideJ
f o r a n ~ l i m a o f C S a n d 9 . 5 % ~ ~ . F o r Q C a m p k . ~
withatestresultfar~of9.71wouldhaveaclasgificatiollof
TYPE V, stt Appeaaix 4, Mo 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 (see Table 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 requirements for diffusion barrier,
undercoat, electrical conductivity and wear and codon
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 lifeof
the part. Typical environments include light-load lubricated
wear,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 exposure on 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 expo-
sure, 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 tempemmand pressme,
hydrogen diide and carbon dioNde oil service, high-
temperam chloride systems, very severe wear,and marine
i mmersi oa
Nar s 2- "I he ~of t he r ut oc oEl l yt i c ~c aat i ngdb
pendst oa~cxt cot ont besur habi shof t hear r i det obepl et al
TABLE1
TLP.
I No-*-
I 1 (D3
ln 2104
N 510s
V 10"
2
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Licensed by Information Handling Services
B 733
TABLE2 senicecondilions
Coating TNdrnert Requirrnnents
secvicecondipbn Thidcness
v m.(m)
Minmuncoating
specificetan
Sc0 Mi rLnrn- 0.1 o.-( 1
S C 1 Light service 5
SC2
~.oO02 ( 1
hwservi ce 13 o.O@x ( 1
Sc3 Modmatesenice 25
Sc4 severeservice 75 0.m ( )
0.001 ( )
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 beclassified by heat treatment after plating to
increase coating adhesion and or hardness (see Table 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 increase adhesion of heat-treatable (age-hardened)
aluminum alloys and carburized steel (seeNote 3).
4.3.5 Class 5-Heat treatment at 140 to 150C for at least
1 h to improve coating adhesion for aluminum, non age-
hardened aluminum alloys, copper, copper alloys and beryl-
lium.
4.3.6 Class 6-Heat treatment at 300 to 320C for at least
1 h to improve coating adhesion for titanium alloys.
N m 3-Heat-treatable aluminum 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 on the engineering
drawing of the part to be plated:
TABLE 3 ClassilicaiionoiPostHeatTreabnent
CLASS oescription Tm@)
CC)
1 No Heat Treatment, As Plated
2 IieatTrearmentforMaXinun
Hardness
TYPE I 260 20
285 16
320 8
400 1
NP II 350t0380 1
TYPE 111 36ot0390 1
TYPE IV 366to400 1
TYPE V 375 to 400 1
3 HvaogenEmbrittlementand 18oto200 2t o 4
4 A&esim.carbwidsteeland 120t o130 1 - 6
5 AdhesbnmBerycunand 140 to 150 l t o2
Adhes*n on steel
A g e "
6
Aluminum
AdhesanOnTrtaniun 300-320 I 4
5.1.1 Title, ASTM designation number, and year of issue
5. I .2 Classification of the deposit by type,seMce condi-
5.1.3 Specify maximum dimension and tolerance require-
5.1.4 Peening, if required (see 6.5).
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 Supplemental or Special Government Requirements
such as, specific phosphorus content, abrasion wear or
corrosion resistaace of the coatin& solderability, contact
resistance and packaging selected firom Supplemental Re-
quirements.
5.1.9 Requirement for a vacuum, inert or reducing atme
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 corrosion resistance, if re-
quired, selected from those found in Wons 9 and Supple-
mental Requirements.
of this specification.
tion, class, (see 4.1, 4.2 and 4.3).
ments, if any.
5. l . 1 1 Requirements for sampling (see Section 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 observanof the best plating practice.
Any such def 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
may be pmtreated in accordance with Guide B656. A
suitable method shall activate the surface and remove oxide
and foreign materials, which may cause poor adhesion and
coating porosity.
N m 5-Heat treatment of the base material may effect its metal-
lurgical propexti eAn example is leaded steel which may exhibit liquid
or solid embritUement after heat treatment. Careful selection of the pre
and post heat treatmeats are recommended.
6.3 Stress Reli&
6.3.1 Pretreatntent of Iron und Steel for Reducing the Risk
of Hydrogen Embrittlement-Parts that are made of steel
with ultimate tensile strength of greater than IO00 Mpa
(hardness of 31 HRC or greater), that have been machined,
ground, cold formed, or cold straightened subsequent to heat
treatment, shall require stress relief heat treatment when
specified by the purchaser, the tensile strength to 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 requi red
on high-st~~ngth steel parts to induce residual compressive
3
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~~
STD-ASTM B733-ENGL L777 D 0757530 Ob07735 79T
@ B733
stresses in the sudace, which can reduloss of fatigue
strength and improve stress corrosion resistance after plating,
(See Supplementary Requirements).
6.3.3 Steel parts which are designed for unlimited life
under dynamic loads shall be shot peened or rotary flap
peened.
N m bcontroUed shot peening is the ppefkred method because
thereare~~swh~~taryOappeeningisaoteffectimSeeSl11.
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
requi red and all immediate adjacent surf ces when they
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 solution over all surfaces to obtain
uniform coating thickness. The location of rack or wire
marks in the coating shall be agreed upon betwen the
producer and purchaser.
6.5 Plating Process:
6.5.1 To obtain consistent coating properties, the bath
must bemonitored periodically for pH, temperature, nickel
and hypophosphite. Replenishments to the plating solution
should beas frequent as requi redto maintain the concentra-
tion of the nickel and hypophosphite between 90 and 100 %
of set point. The use of a statistical regimen to 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 pitting or StreaLing due to hydrogen
bubbles.
6.6 Post Coating Treatment for Iron and Steel for Re-
ducing 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 requi re post coating hydrogen embrittlement
relef baking when speci f i ed by the purchaser, the tensile
strength to be supplied by the purchaser. Specification B 850
may be consulted for a list of post treatments that are widely
used.
6.6. I Heat treatment shall be per f i i ed preferably within
1 h but not more than 3 h of plating on plated after plating of
steel parts to reduthe risk of hydrogen embrittlement. In
all cases, the duration of the heat treatment shall commence
from the time at which the whole of each part attains the
specified temperature.
6.6.2 High-strength steel partswith actual t ede strengths
greater than loo0 MPa(corresponding hardness 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 Adhesion-
To improve the adhesion of the coating to various substrats,
the heat treatments in Table 3 should be performed as soon
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 maximum hardness.
as practical &el plating (see4.3).
6.8.2 See Appendixes 3 and 4 and Guide B656 Fgs
X1.2 and X1.3.
6.8.3 A heat treatment at 260C for greater than 20 h
sho~dbeusedtoreduthelossofsurfacehardn~and
strength of some ferrous basis metals. Avoid rapid heating
and cooling of plated pouts. Suffiicient time must be allowed
for l argeparts to reach oven temperature.
tbCphosphanucontentOftllCdeposit.Highpbogpbanrs~tS~~
mqui reb~ti mcorahi gbertem~orboth. Iadi vi dual al l oys
should be tested for maximum hardness attainaMe, especially for
COIlditi~Ofandloaggtima.
~8-rncrtorreducingatmosphereor~umsufficientt0
~toxidpoionisrrawmendedforheattreatmentrbovc26oxDo
not us e gas am~hydr oge nwi t hhi gh~s t e dpar t s
NOIE 7-Th~~oftinact0reachmaximumhardaessvarieswah
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
appearanwithout visible def a such as blisters, pits,
pimples, and mks(see 9.2).
7.2.1.2 Imperfctions that arise from surf ace conditions of
the substrate which the producer is unable to remove using
conventional pretreatment techniques and that persist 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 speci-
fied (see 5.9).
7.2.2 Thkksts-The thickness of the coating shall ex-
ceed 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 sur f ace (see 5.3).
NOIE 9--The~oftbecoatingcannotbecontrolledinMind
orsmalldiameterdeepholcsorwheresolutioncirculationisrcstricted
7.2.3 Adhesion-The coating shall have sufficient adhe
sion to the hasis metal to pas the speci fi ed adhesion test (see
9.4 and Test Methods B 571).
7.2.4 PorositpThe coatings shall be essentiauy pore free
when tested Bccording to one of the methods of 9.6. The test
method, the duration of the test, and number of allowable
spots per unit axa shall be specified (see 5.10 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 thesequalification requirements shall 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 (see 4.1).
7.3.2 Mb- me microhardnesp of Class 2 de-
posits shall be determined by Test Method B 578 (KMIOP).
Fo r Cl a s s 2 ~ t h e mi m~ n e s s s h a l l e q ~ o r e x c e e d
a minimum of 850 (HK100 (or equivalent Vickers) (see 4.3
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 de-
posit a coating onto high strength steels shall be evaluated for
hydrogen embrittlement by Test Method F 5 19.
8. Sampling
8.1 The purchaser and producer are urged to employ
statistical process control in the coating process. F'roperly
performed this will ensure mted products of satisfactory
quality and wi l lreduce the amount of acceptance inspection.
8.1.1 Sampling plans can only screen out unsatisfactory
products without assurance that none of them will be
accepted. (7)
8.2 The sampling plan used for the inspection 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 5.1 1 and S. 1 1.1).
NOTE I O-Usually, when a collection of coated parts (the inspection
lot 8.2) is examined for compliance with the requirements placed on the
parts a relatively small number of parts, the sample, is s e l e c t e d at
random and inspected. The inspection lot is then clasifted as compIying
or not complying with the requirements based on the results of the
inspection sample. The si ze of the sample and the criteria of compliance
are determined by the application of statistics. The procedure isknown
as sampling inspection. Three standads Test Method B 602, Guide
B 697, and Test Method B 762 contain sampling plans that are designed
for the sampling inspection of coatings.
Test Method B 602 contains four sampling plans, three for usewith
tests that are nondestructive and one for use with tests that are
destructive. The purchaser and prcdur may on the plants) to be
used.If they do not, Test Method B 602 identifig the plan to beused.
Guide B 697 provides a large number of plans and al so gives guidana
on the selection of a plan. When Guide B 697 is specified, the purchaser
and producer need to agree on the plan to beused.
Test Method B 762 can be used only for coating requirements that
havea numerical limit, such as coating thickness. The last must yield a
numerical value and certain statistical requirements must be met. Test
Method B 762 contains several plans and also gives instructions for
calculating plans to meet spi al needs The purchaser and producer
may agree on the plan(s) to be used. If they do not, Test Method B 762
idenfifies the plan to beused.
An inspection lot shall be defined as a collection of coated parts which
are of the same kind, that have been produced to the same specification,
that have been wated by a single producer at one time or approximately
the same time under essentially identical conditions, and that are
submitted for aczeptanor rejection as a group.
8.3 All specimens used in the sampling plan for a mp
tance tests shall bemade of the same basis material and in
the same metallurgical condition as articles being plated to
this specification.
8.4 AU specimens shall be provided by the purchaser
unless otherwise agreed to by the producer.
NOTE I I-The autocatalytic nickel pnxzss is dynamic and a daily
sampling is recommended. For ht i qgrequiring alloy analysis and
corrosion testing weekly sampling should beconsidered as an option.
9. Test Methods
9.1 Deposit Analysis for Phosphorus:
9. l . 1 Phosphorus Determination-Determine mass ?&
phosphorus content according 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-
tion, emission or X-ray fluorescence spectrometry.
N m 12"Inductively coupled plasma techniques can determine the
alloy to within 0.5 Om.The foUowinganalysis wavelength lines have bee0
ued with minimum interfaence to determine the alloy.
Ni 216.10 nm Cd 214.44 nm Fe 23820 nm
P 215.40 nm CD 238.34 nm Pb 283.30 nm
P 213.62 nm Cr 284.32 om Sn 198. 94 nm
Al 202.55 nm Cu 324.75 nm Zn 206.20 om
9.2 Appearance-Examine the coating visually for com-
9.3 Thickness:
N m 13-Eddy-cummt type instruments giveenatic measurements
due to variations in conductivity of the coatings with changes in
phosphorus content.
9.3. I Microscopicd Method-Measum the coating thick-
ness of a cross section according to Test Method B 487.
N m 14-To protect the edges, electroplate the specimens with a
minimum of 5 pmof nicket or copper prior to c~(lss sectioning.
9.3.2 Magnetic Induction Instrument Method-Test
Methad B 499 is applicable to magnetic substrates plated
withautocatalytic nickel deposits, that contain more than11
mass 96 phosphorus (not ferromagnetic) and that have not
been heat-treated The instrument shall be calibrated with
deposits plated in the same solution under the same condi-
tions on magnetic steel.
9.3.3 Beta Backscatrm Method-Test Method B 567 is
only applicable to coatings on aluminum, beryllium, magne-
sium, and titanium. The instrument must be calibrated with
standards having the same composition as the coating.
phosphorus content (See Append X2).
9.3.4 Micrometer Meth0d"Measu-e the part, test
coupon, or pin in a specific spot before and after plating
using a suitable micrometer. Make sure that the surfaces
measured are smooth, clean, and dry.
9.3.5 Weigh. Plate, Weigh Meth0d"Using a similar sub
strate material of known surf ace area, weigh to the neafest
milligram before and after plating making sur e that the part
or coupon is dry and at room temperature for each measure!-
ment. Calculate the thickness Eromthe increase in weight,
specific gravity, and area as follows:
coating thickness, Fm =10 W/ (A X D)
pliance with the requirements of 7.2. l.
N m 15-The density of the coating vari es with its mass 56
where:
W =weight gain in milligrams,
A =total swface area in square centimetres, and
D =grams per cubic centimetres (see Appendix X).
9.3.6 Coulometric Method-Measure the coating thick-
ness in accordance with Test Method B 504. The solution to
be used shall be in accordanoe with mandachmr's m m -
mendations. The surface of the coating shall be cleaned prior
to testing(seeNote 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 thick-
ness in accordance with Test Method B 568. The instrument
must be calibrated with standards having the same composi-
tion as the coating.
N m I bT hi 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
~. ~ ~~ ~ ~~
STD-ASTM 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&CY and muh that 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 4x 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.
NOTE 17-Appropriate test specimens are strips approximately 25 to
50mmwide,200to300mmloagand3to6mmthick.
9.4.2 Impact Test-A spring-loaded center punch with a
point having 2 to 3 mm 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 for flaking or blistering of the coating, which is
cause for rejection.
9.4.3 Thsnnal Shuck-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 (HK).
It will vary depending on loads, type of indenter, and
operator. A L O O g load is recommended. The rhombic
hoop indenter gives higher hardness readings than the
squarsbase pyramidal Vickm diamond indenter for 100 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.
NOTE 1 8 4 thick (75 Fm+) cuatings on steel a surface
microhardness determination 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 dissolving 25 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 rinsing and air drying, examine the part for blue
spots, which format 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~beginstoboilinnotlessthan 15
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 1 193) at 25 f 2% temperam
andthenexaminethepartforrustspots.
9.6.4 Alizarin Test for AIuminwn Alloys-Wipe the
plated part or specimen with 10mass 48 d u m hydroxide
solution. After 3 min contact, rinse, and apply a solution of
al i zari n sulfonate prepared by dissolving 1.5 g of methyl
llulosein90mLofboilingwatatowhich,afhcooling,
O. 1 g sodiumal i zari n MOM^, dissolved in 5 mL of ethanol
isadded.After4mincontaa,apply~aticaciduntil
t hevi ol et cdordi sappearsAnyredspot s~i ndi cat e
Po-
9.6.5 Porosity Test for Copper Substrutes-Wipe the
platedpartorspecimenwithglacialaceticacid.After3min,
apply a solution of potassium ferrocyanide 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. Thew o n and bias requimnents will vary
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 of dhat i sf b
tionoccurswiththeresultsofatest,theproducermaymake
a claim for a hearing. coatings that show imperfections may
berejected.
11. ckrtifii
11.1 Whenspecifedinthepurchaseorderorcontmct,the
purchaser shall be lmished 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 v e been met. When specifiedin the purchase oder or
contract,areportofthetestresultsshallbefurnished.
12 Keywords
12.1 autmatalytiq chemical nickek coati-, conductive;
c o d o n resistance; electrolq functional, nickek nickel
Phosphorus;"
6
COPYRIGHT American Society for Testing and Materials
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SUPPLEMENTARY REQUIREMENTS
The following supplementary requirements shall apply only when specified by the purchaser in the
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 the purchaser in
the ordering information the phosphorus content shall be
maintained in the deposit to within 1 %. Use the test
methods described in 9. l.
S 1.3 Inert Atmosphere-When specified by the purchaser
in the ordering information, the coating shall be heat treated
in a vacuum, inert, or reducing atmosphere to prevent
surface oxidation of the coating.
S1.4 Hydrogen Embrittlement-When specified by the
purchaser in the ordering information the plating process
shall be evaluated at the time of processing parts for
hydrogen embrittlement using Test Method F 5 19.
S1.5 Abrasive Wear-When specified by the purchaser in
the ordering information, the coating shall be tested for
abrasion wear resistance using the method in Appendix X1
of this specification. The coating shall meet a maximum
wear rate which is specified by the purchaser and agreed to
bythe producer.
S I .6 Adhesive Wear-When speci f i ed by the purchaser in
the ordering information, the coating shall be tested for
adhesive wear resistance using Test Method D 27 14 or Test
Method D 2670. The wear rate shall be specified by the
purchaser and agreed to by the producer.
S1.7 Conlact Resistance-When specified by the pur-
chaser in the ordering information, the coating shall be tested
for contact resistance using Test Method B 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 pur-
chaser in the ordering information the coating shall pass any
special corrosion tests agreed to by the producer. The
corrosion resistance of the 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).
S1.10 Pitting Corrosion Resiszance-Use Method G 85
(acetic acid-salt spray test), Method B 368 (copper-accel-
erated acetic acid-salt spray, CM) , or Method B380
(Corrodkote) to evaluate the c~rrosion resistance of the
coating to pitting
S l. 1 1 Special Government Requirements:
S l. 1 l . 1 Sampling-Part(s) plated for the US Government
and Military use shall use MILSTD-105 as the sampling
plan.
S1.11.2 Shot Peeni ng" strength steel part($ pm
cessed for US Government and Military useshall be shot
peened in acconiance with -13165 or rotary flap
peened in aa; ordance with Mil-R-8 184 l. (see Note 6).
SI. 1 1.3 Puckugin"parts shall be packaged in accor-
danq with Practice D 3951.
APPENDIX
(Nonmandatory Information)
XI. TABER ABRASER
x1.1 scope
X l . l . 1 This test method wi l levaluate the resistance of the
coating to abrasive wear. The test is performed by rotating a
plated panel under rotating rubber wheels and weighing the
panel aller each l o00 cycles for weight loss. Duration of the
test is 6000 cycles and it can be extended to 25 O00 cycles for
more complete results.
NOTE X1. I-Variation in results have been attributed to the hu-
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 wdts are variable between tests and there-
fore three plated test specimens should be tested to 6000
cycles each. The results should be averaged without the lrst
l o00 cycles and the abrasion wear resistance is reported as
the weight loss in mg/1000 cycles (Taber Wear Index).
WEARTEST"I0D
X1.2 Apparatus
X 1.2. I Taber Abraser Wear Testing Unit-The unit must
be capable of loading with I O0 0 g load and operating with a
vacuum.
X 1.2.2 Abrasion Wheels-Use Cs10 (resilient rubber)
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 the reproducibility of results (see Test Method
D 4060).
X1.2.3 Test Specimens-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-Scale which is capable of
measuring to 150 g k O. 1 mg.
7
COPYRIGHT American Society for Testing and Materials
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X13 Procedure X1.3.2.4 Abrasion test the coating with I O00 g load for
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 the following steps:
X1.3.2.1 Run the CS10 wheels on the coating for I O00
cycles to remove any surface rouphness. The wheels shall be
loaddwithIOOOgwithavacuumonhighfortheentiretest.
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.
~Ooo cycles.
X1.3.2.5 Repeat X1.3.2.2, X1.3.2.3 and X1.3.2.4 until a
total of 6OOO cycles bave been accomplished for eacb
specimen.
Xl A Reparthg
X1.4.1 Determine the average weight loss in m@cams
for each specimen per l o00 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
IS04527. Annex C
Vendor, Elnic, unpublished
Rajarn, K. S. Rajam et al. Metal Finishing, Vol 88. No 11 119901
NIST, Fielding Ogburn et 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. Schering KG. Berlin 1982
Mallory, Glenn Mallory et al, Studies and Properties o f Very Hard Electroless Nickel Deposits.
EN' 95. Gardner Management, Cincinnati. OH, 1995
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X3. HARDNESS VERSUS HEAT TREATMENT
HARDNESS OF ELECTROLESS NICKEL vs TEMPERATURE vs TYPE
1000
900
800
700
600
500
I I I l I
400
I
I
I t
I
I I , I l
I
I I l I !
I I
O 100 200 300 400 500
x4. ALLOY TYPES
9
COPYRIGHT American Society for Testing and Materials
Licensed by Information Handling Services
O
I
2
3
4
5
6
P%
7
8
9
IO
II
12
13
IL
B733
HARDNESS STRENGTH MAGNETICS TYPES
""""""""
12
I3
IL
P%
.-
LOW HIGH LOW HIGH NON FERRO
MAGNETIC MAGNETIC
FmX4.1 ~~d A. " Nl d r d ~c o 11Oh o , b y "
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 at the 75 m site at Lame Center for
Corrosion Technology, Wrightsville, NC (Kure Beach). The
program caUdfor the plating of both TypeN and TypeV
deposits on standard smooth and ground steel Q PaneIs.
X5.1.2 There were nine Merent sources of deposits, each
providing five lots of five panels. The program involved
plating 12.5, 25, and 75 Fmthicknesses on smooth and
ground surf ace and one smooth lot heat treated for hardness
at 550'C for 2 h. The heat treatment temperature was
considerably higher than typical processing and was chosen
to evaluate the formation of diffusion products of iron,
nickel and phosphorus
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 interpmtation of the results of these exposure
test should be made on the basis of general performance of
the coating on panels. Base metal condition, undercoats,
surface prcparation, and post processing al l have a signiscant
effect on the performance and should be given mreful
consideraton when designing the part and p&reatment
processing sequen.
10
COPYRIGHT American Society for Testing and Materials
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STD-ASTM B733-ENGL L797 W 0757530 Ob097LI2 72T
V E
V C
IV J
IV
IV
IV
1
2
V G 3
4
5
2
1
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
2
1
3
4
5
IV K
1
2
3
4
5
1
2
3
4
5
1
2
N I 3
4
5
smooth
smooth
smooth
smooth
Grand
smooth
smooth
smooth
smooth
Grand
smaoth
smooth
smooth
smooth
Grand
smooth
smooth
smooth
smooth
Grand
smooth
smooth
smooth
smooth
Grand
smooth
smooth
SnKKml
smooth
(;rand
smooth
smooth
smooth
smooth
oand
smooth
smooth
smooth
smooth
(jmud
smooth
srooth
smooth
smooth
No
No
No
YeS
No
No
No
No
YeS
No
No
No
No
YeS
No
No
No
YeS
No
No
No
No
YeS
No
No
No
No
YeS
No
No
No
No
YeS
No
No
No
No
YeS
No
No
No
No
YeS
No
77 10.0
46 9.9
79
77
125
25
75 m5 105 109
25
25
12.5
25
75 102
25
25
12.5
25
75 10.4
25
25
12.5
25
75
25
25
25
125
75
25
25
125
25
75 7.3
25
25
12.5
25
75
25
25
125
25
75
25
25
12.5
25
75 80 7.1
25
25
9.5
9.0
8.9
8.3
02
7 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
4 2 f O 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
9.6 f 1.1
7.0 f o
1 . 0 f 2
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
5.8 f 0.4
5.0 f 1 A
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 Electroless Nickel Plating, ASTM STP 265, ASM, 12644 Raearch Parkway, Orlando, R. 32826, 1986 Chapter 23.
(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 RedanTests of Fi k c t r o I e s
(3) Gawri l ov, C. G., Chemical (Electroless) Nickel Plating, Portcullis N i Deposi4" Wi ng, Vd 61, September 1974.
ReSS, London, 1974.
( 7) Parker,K. of Heat Treatment on thc Ropemes of
(4) Saianek, W. H., The Properties of Electroakposited Metals Md Electrokss Nickel Plating and S@ Finishing, Vol
Afloys, The American Electroplaters and Sud&ce Finishen Society, 68, December 1981.
1959. (5) Mallory G., and Hajdu J. "Ekctrol sPhtbg," AESF 12644
11
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