ASTM B733 Electroless Nickel Plating
ASTM B733 Electroless Nickel Plating
ASTM B733 Electroless Nickel Plating
'
Thrs standard is lrsued under h e fired deri%mrionB 733: the numbcr irnmcdialcly f o l i o r i n ~!he drri~mationindica~esthe ycnr of
original adoption or, in the case ofrevision, the year of larl revlson. A number in parentheses indicales the year af larl reapproval. A
superscript cprilo~l(E) ind~cvtesan edilorial chanee since Ule l a s ~revision or reapproval.
hl.
1. Scope
' This ipec~ficalionis under the jurisdiction of ASTM Commillce 8-08 on Melal
Pordcrr and Mesa1 Powder Produca and is the direct rcipo~ir~blllry
of Subcommillee B06.08.01 on Englneenng Coatings
C u n m , cdition approved July 10. 1997. Published October 1997. Oiiginally
published as B 713 - 81 Last prevlour edition B 733 - 90 (19941.
'The boldfac, numbrrr
in
rercr lo a lis1 of references 0 , ,hr
end of rhe ex,.
2. Referenced Documents
2.1 ASTM Sra~~dards:
B 368 Test Method for Copper-Accelerated Acetic AcidSalt Spray (Fog) Testing (CASS Testing)'
B 374 Terminology Relating to Electroplating3
B 380 Test Method of Corrosion by the Corrodkote Procedure3
B 487 Test Method for Measurement of Metal and Oxide
Coating Thicknesses by Microscopical Examination of a
Cross Section'
B 199 Test Method for Measurement of Coating Thicknesses by the Magnetic Method: Nonmagnetic Coatings on
Magnetic Basis Metals3
B 504 Test Method for Measurement of Thickness of Metallic Coatings by the Coulometric Method3
B 537 Practice for Rating of Electroplated Panels Subjected
to Atmospheric Exposure'
B 567 Method for Measurement of Coating Thickness by
the Beta Dackscatter ~ e t h o d ~
B 568 Method for Measurement of Coating Thickness by
X-Ray Spectrometry3
'.l!a>i,oIBook
Copyrlghl OASTM International 100 Ban Harbor Dive. PO Box C100. Wart CmnrhMosXen PA 19428-2959, United Slales
Coatings3
B 602 Test Method for Attribute Sampling of Metallic and
Inorganic Coating"
B 656 Guide for Autocatalytic Nickel-Phosphorus Deposition on Metals for Eneineerine Use3
B 667 Practice for Cot%uctio;
and Use o f a Probe for
Measuring Electrical Contact Resistance"
B 678 Test Method for Solderability of Metallic-Coated
Products'
B 697 Guide for Selection of Sampling Plans for Inspection
of Electrodeposited Metallic and lnorganic Coatings"
B 762 Method for Variable Sampling of Metallic and Inorganic Coating?
B 849 Specification for Pre-Treatment of Iron or Steel for
Reducing the Risk of Hydrogen Embrinlement3
B 850 Specification for Post-Coating Treatments of lron or
Steel f i r Reducing the Risk o f Hydrogen Embrittlement3
B 85 1 Specification for Automated Controlled Shot Peening
of Metallic Articles Plior to Nickel, Autocatalytic Nickel.
Chromium. or As A Final Finish3
D 1193 Specification for Reagellt Wale9
D 2 6 7 0 Method for Measuring Wear Properties of Fluid
Luhricants
Methodi6
.~~(Falex
~~
,
D 2714 Method for Calibration and Operation of an Alplia
LFW-I Friction and Wear Testing Machine6
D 1951 Practice for Commercial Packaging'
D 4060 Test Method for Abrasion Resistance of Organic
Coatings by tlie Taber ~ b r a s e r '
E 60 Practice for Photometric h4ethods for Chemical Analysis of Metals9
E 156 Test Metliod for Determinatio~i of Phosphorus in
Higll-Phosphorus Brazing Alloys (Photometric Met11od)'~
E 352 Test Methods for Chemical Analysis of Tool Steels
and Other Similar Medium-and High-Alloy Steel9
F 519 Test Method for Mechanical Hydrogen Embrinlementll
G 5 Practice for Standard Reference Method for Making
Pote~itiostaticand Potentiodynamic Anodic Polarization
Measurements"
G 3 1 Practice for Laboratory l ~ n n ~ e r s i oCorrosion
n
Testing
of Metals"
G 59 Practice for Conducting Potentiodynamic Polarizatio~i
Res~stanceMeasurements"
G 85 Practice for Modified Salt Spray (Fog) Testing"
2.2 144ilira1,~Sta17dar.d~:
MIL-R-81841 Rotary Flap Peening of Metal PartsI3
P h o ~ p h o w%~~t
II
I 103
111
2 io 4
5 to 9
10 and above
IV
Condllon
~rm
in (mm)
SCO
SCI
Minlrnun Thickness
Light Service
0.1
5
0.000004 (
0.0002
(
)
J
SC2
Mild Service
Moderate Service
Severe Service
13
25
75
0.0005
0.001
0003
(
[
)
)
sc3
SC4
'.4nri?rol Book
0J.04.
11.0 1
Val 05.02.
' .4!i??<rI
Book of.4STM Sinndords. \bl
'Aari,ruI
3. Terminology
3.1 D.efini/io~i:
3 1 . 1 significant sur/aces-those
substrate surfaces which
the coating must protect from corrosion or wear, or both, and
that are essential to the perfomlance.
1.2 Orher- DeF~litions-Teminolo B 374 defines most of
the technical terms used in this specification.
4. Coating Classification
"
''A\,ai:abIe
10036.
Oe~cription
CLRSS
Classification of
Temperature
xme (hl
iCl
No HealTrealment. As Plated
Heal Treatment for Maximum Hardness
TYPE I
260
285
320
n nn
TYPE I 1
TYPE I l l
TYPE IV
TYPF V
3
4
180 to 200
12010 130
140 to 150
1 to 2
30C~320
14
Aluminum
6
Adhesion on Xlanium
ro over
~~~
5. Ordering Information
5.1 Tlie following informati011 shall be supplied by The
purchaser in either the purchase order or on the engineering
drawing of the pan to be plated:
5.11 T ~ ~ ~ ~ , Adesignation
STM
number, and year ofissue of
this specification.
5.1.2 Classification of the deposit by type, service condition, class, (see 4.1, 4.2 and 4.3)
5 1 . 3 Specify maximum dimension and tolerance requiremeuts, if any.
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 Embrittlernent Relief after plating, (see
6.6).
5.1.7 Significant surfaces and surfaces not to be plated must
be indicated on drawings or sample.
5 1 . 8 Suppletnental or Special Government Requirements
such as, specific phosphorus content, abrasion wear or corrosion resistance of tlie coating, solderability, contact resistance
and packaging selected from Supplemental Requirements.
5.1.9 Requirement for a vacuum, inert or reducing atmosphere for heat treatment above 260C to prevent surface
oxidation of the coating (see S3).
51.10 Test methods for coating adhesion, composition,
thickness, porosity, wear and corrosion resistance, if required,
selected from those found in Section 9 and Supplemental
Requirements.
5.1.11 Requirements for sampling (see Section 8).
NOTE&The pnrchaser should furnish separate lesl specimens or
coupons of rhe basis metal for lest purposes to be plated coneunentiy with
the artieles la be plated (see 8.4).
NOTE5-Heat
eical
solid
7. Requirements
7.1 Process-The coating shall be produced froni an aqueous solution through chemical reduction reaction.
7.2 Acceprarice Requir-ernenrs-These
requirements are
placed on each lot or batch and can be evaluated by tesling the
plated part.
7.2.1 ilppear-aiice:
7.2.1.1 The coating surface shall have a uniform, metallic
appearance without visible defects such as blisters, pits,
pimples, and cracks (see 9.2).
7.2.1.2 Imperfections that arise froni surface conditions of
the substrate which the producer is unable lo remove using
conventional pretl-eatmcnt tcchniques and that persist in the
coating shall not be cause for rejection (see 6.1). Also,
discoloration due to heat treatment shall not be cause for
rejection unless special heat treatment atmosphere is spccificd
(see section 5.1.9).
7.2.2 Tliicbiess-The thickness of the coating shall exceed
the niiliimuni requirements in Table 2 as specified hy the
service condition agreed to prior to plating (see 9.3). After
coating and if specified, the part shall not exceed maximu111
dimension on sig~iificantsurface (sce section 5.1.3).
UOIE 9-The thickness of the caatms canno1 be canrrolled in blind or
small diameter dcep holes or where salution circulat~anis rcsrricted.
8. Sampling
8.1 The purchaser and producer are urged to employ statistical process control in the coating process. Properly perfomled
this will ensure coated products of satisfactory quality and will
reduce the amount of acceptance inspection.
8.1.1 Sampling plans can only screcn out unsatisfactory
products without assurance that none of them will be accepted.
(7)
. - .
9. Test Methods
9.1 Deposil Anahsis /or Phosphorus:
mass %
9.1.1 Phosphorr~s Dererniinarion-Determine
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 absorption,
emission or X-ray fluorescence spectrometry.
NOTE 12-inductively coupled
plasma techniques can determine the
.
alloy to within 0.5 %.The following analysis wavelength lines have been
used with minimum inteiference to determine the alloy.
Ni 216.10nrn
Cd 214.44 nrn
Fe 238.20 nrn
P 215.40 nrn
CO 238.34 nm
Pb 283.30 nm
P 213.62 nrn
Cr 284.32 nm
Sn 198.94 nm
~
Cu 324.75 nnr
Al 202.55 nrn
Zn 206.20 nrn
9.2 Appenrance-Examine the coating visually for compliance with the requirements of 7.2.1.
9.3 Tltickf~ess:
NOTE13--Eddy-current type insrruments give erraric measurements
due to variarions in conductivity of the coalings with changes in
phaspharur content.
9.3.1 Mio.oscopica1 Merhod-Measure tlie coating thickness of a cross section according to rest Method B 487.
NOTEI L T o protect the edger, elccrroplare the specimens with a
minimum of 5 p of nickel or capper prior to croir sectioning.
".--..
density
where:
It'
=
=
9.4 Adhesion:
9.1.1 Bend Tesl (Test Metliods B 571)-A sample specimen
is bent 180" over a mandrel diameter 4X the thickness (10 mm
minimum) of the specimen and examined at 4X power
magnification for flaking or separation at tlie interface. Fine
cracks in tlie coating on the tension side of the bend are not an
indication of poor adhesion. Insertion of a sharp probe at the
tnterface of the coating and basis metal to detem~ine the
., . 1s
.
,
aoneslon
suggesrea.
Nari 17-Appropnare rest specimens are strips approximately 25
mln wide, 200 lo 300 mm long and 3 to 6 mrn illick.
ta 50
derennination is permissible.
9.6 POI-osih,-There is no universally accepted test for
porosity. When required, one ofthe following tests can be used
on the plated part or specimen.
9.6.1 Ferroxj~lTest for h a n Base Sr~bslrates-Prepare the
test solution by dissolving 25 g of potassium ferricyanide and
15 g of sodium chloride in 1 L of distilled water. After
cleaning, immerse the part for 30 s in the test solution at 25C.
After rinsing and air drying, examine the pan for blue spots,
which form at pore sites.
9.6.2 Boiling Walei- Test for Iron-Base SubstraresCompletely immerse the pan to be treated in a vessel filled
with aerated water at room temperature. Apply heat to the
beaker at such a rate that the water begins to boil in not less
than 15 min, nor more than 20 min after tlie initial application
of heat. Continue to boil the water for 30 min. Then remove the
pan, air dry, and examine for rust spots, wliich indicate pores.
NOTE 19-Aerated water is prepared by bubbling clean compressed air
rhrough disrilled ujater by means of a glass diffusion disk at room
tempemrum for 12 h. The pH of the aerated water should he 6.7 + 0.5.
9.6.3 Aernled N'aler Test for Iron-Base Subsrt-aresImmerse the part for 4 h in vigorously aeratedType 1V or better
water (see Specification D 1193) at 25 t 2C temperature and
then examine the part for rust spots.
9.6.4 Alimriri Tesr for Alrdi~~i~~urn
Allo~,s- Wioe the nlated
part or specime~iwith 10 mass "o sodium hydroxide solution.
After 3 min contact, rinse, and apply a solution of alizarin
sulfonate prepared by dissolving 1.5 g of methyl cellulose in 90
mL of boiling water to which, after cooling. 0.1 g sodium
alizarin sulfonate, dissolved in 5 mL of ethanol is added. After
4 min contact, apply glac~alacetic acid until the violet color
disappears. Any red spots remaining indicate pores.
9.6.5 Porosih Tesr for Copper Subslrares-Wipe the plated
pan or specimen with glacial acetic acid After 3 min, apply a
solution of potassium ferrocyanide prepared by dissolving 1 g
of potassium ferrocyanide and 1.5 g methyl cellulose in 90 mL
of boiling distilled \x8atcr.The appearance of brown spots after
2 min indicate pores.
9.7 Other Tesl Methods-Test methods which have been
developed that are equal to or better than these may be
substituted. The precision and bias requiremetits will vary for
each type of test. If an alternate test is specified it shall be
agreed upon between the producer and the purchaser.
10. Rejection and Rehearing
SUPPLEMENTARY REQUIREMENTS
The following supplementary requirements shall apply only when specified by the purchaser in tlie
contract or order.
S1.l Shot Peening-When specified by the purchaser in the
ordering information, the part(s) shall be shot peened prior to
plating in accordance with Specification B 851 or MIL-S'3165.
S1.2 Con~posifion-When specified by tlie purchaser in the
orderiny information the phosplioms content shall be maintained in the deposit to within 1 %. Use the test methods
described in 9.1.
S l . 3 1rrer.fArmosphere-When specified by the purchaser in
the orderiny information, the coating shall be heat treated in a
vacuum, inert, or reducing am~ospliere to prevent surface
oxidation of tlie coating.
S1.4 Hydrogen Embi-itrlemerzr-When specified by the purchaser in the ordering informatinn tlie plating process shall be
evaluated at the time of processing pans for hydrogen embrittlement using Test Method F 5 19.
S1 5 Abr-orice Wear-When specified by tlic purchaser in
the ordering information, the coating shall be tested for
abrasion wear resistance using the method in Appendix XI of
this specification. Thc coating shall tuect a maximum wear rate
which is specified by the purchaser and agreed to by the
producer.
$1.6 Adhrsi~,eWeor-When specified by tlie purchaser in
5 ordering information, the coating shall be tested for
hdliesive wear resistance usine Test Method D 2714 or Test
Method D 2670. Ihe wear rite shall be specified by the
purchaser and agreed to by the producer.
APPENDIXES
(Nonrnandator! Inlormation)
Care
X1.Z Apparatus
..
X1.2.1 Taber Abi-asei. 14'ear- Testing Unit-The unit must be
capable of loading u'itll 1000 g load and operating with a
vacuum.
X1.2.2 A~I-asior?Wlzeels- Use CS-10 (resilient rubber)
Taber wheels. To reface the wheels use CS-I1 discs from Taber
The hardness of CS-I0 wheels can change with time and call
effect the reproducibility of results (see Test Method D 4060).
~~
~~
cycles.
X1.3.2.4 Abrasion test the coating with 1000 g load for
1000 cycles.
X1.3.2.5 Repeat X1.3.2.2, X1.3.2.3 and Xl.3.2.4 until a
total of 6000 cycles have been accomplished for each speclmen.
X1.4 Reporting
XI .4.1 Determine the average weight loss in milligrams for
each specimen per 1000 cycles Taber Wear Index and the mean
weight loss per 1000 cycles for all specimens. Report the mean
and standard deviation for the coating.
I S 0 152: Annex C
Vendor. Elnlr, u n p u b l l r h e d
Ratam, C
S.Rajam r t
NIST. F ~ e l d ~ nOgburn
g
el a\. P:atlnq and S u r f a c e Flntshlng, V a l 68, No 3 lI'18ll
FIG. X2.1 Density of Autocatalytic Nickel Phosphorus Alloy Summaw of Reported Values
HARDNESS OF ELECTROLESS
NICKELvs TEMPERATURE
vs TYPE
LOO
' I'1
- -
100
200
300
1 1
-
LOO
500
TEMPERATURE
(C) I HOUR
FIG. X3.1 Hardness of Autocatalytic Nickel Phosphorus Versus Heat Treatment Versus Phosphorus
applicarions.
HARDNESS
STRENGTH
MAGNETICS
TYPES
...................
...................
..................
-................
..................
.................
LOW
HIGH
NON
FERRO
MAGNETIC
MAGNETIC
FIG. X4.1 Selected Properties of As Plated Autocatalytic Nickel Phosphorus Coatings by Phosphorus Content
TABLE X5.1 Results o f 110 M o n t h Exposure of Autocatalytic (Electroless) Nickel Deposits a t Kure Beash, N o l t h CarolinaA
P ~ O S D ~ OAlloy
R I S %wf
Deposit Type
Source
Lot
1
Smoolh
Smooth
Smoolh
Smoolh
Heal
Treatment
Thickness,
pm Target
NO
12.5
No
No
12.5
25
75
Thickness,
pm Actual
ICP
EDM
Ractice
B 537
Ralings 110
Months
3.6 1 3 0
Ground
Smaath
Smooth
Smooth
Smooth
Ground
Smoolh
Smoolh
Smooth
Smooth
Ground
Smooth
Smooth
Smooth
Smooth
Ground
Smooth
Smooth
Smaath
Smooth
Ground
Smoolh
Smooth
Smooth
Smooth
Ground
Smoolh
Smooth
Smoolh
Smooth
Ground
Smoolh
Smooth
Smoath
Smooth
Ground
1
2
3
4
5
Smooth
Smooth
Smooth
Smooth
No
Yea
Gro.nJ
'ro
"
80
7.1
.
25
~
23
Te
, ronr .,on$ 'rum i n s mar r e e x v o s ~ r cp o g r m l a . " o w n s.mmanzro o) Dr George ) B a n ol h(:D n
or Slce F r a Reporl un ASTM Fogrl- 14 ho ro has DrcSPnleJ al i h r l (:oo'c.enre ProLr F n s n 1.2
...
CC L O
11 s
caper Mar
(:on05 on
i2etiormnn~r.01 C h (:os.t nq
REFERENCES
(1) Symposium on Elecnolesr Nickel Plating, ASTM STP 265. ASTM,
1959.
(2) D?~i~~rer-i,ig
Pl.oprr-lies q(E1ecnuless Nickei, The lntemarianal Nickel
Ca., Inc., Ncw York, N'i
(3) Gawrilav, C. G., C l ~ e n ~ i c (Elecnulers)
ol
N i d e l Ploting, Pancullis
Press, London. 1974.
(4) Safranek, W H.. Tile P,-oper-ties of Elecnadeposired hf~:Iolr orzd
A/lr,~..<. The American Eleclroplaters and Surface Finishen Society.
ASTM inleroa1,Onal lakes no position respecling lhe validity of any paten1 "ghlr asserted in conneclion wih any rlem mentioned
in his sfanaard. Users of hb sfandaid are expressly adwsed lhal deleiminalion of ihe vaiidily of any such palent rlqhls, and lhe nsk
of infnngemeol of such rights, are enl~relylheii own rerpoosibil,ly
This sleodard K subjecl to revision a1 any time by lhe iesponslbie lechnicai comminee and musl te reviewed eveiy five years and
if no1 revised, either reaowved or wrhdrawr~.Your commenls are invited miher tor revision oi lhis slandaid or for oidditiooal standards
and should be addressed lo ASTM lnlemal~onalHeadquarlers. Youimmmenls Wli receive camfvl mosideiation a1 a meeling of me
iesponsibie lecnnicai cornmillee, whrch you may anend if you feel ihal your mmmeotr have not received a fair heai~ngyou should
make your views known lo the ASTM Commitlee an Standards, a1 the address shown below
This slarldard is copyrighled by ASTM lnternaliononai. 1W Ban Haaoi Drive. PO Box C700, West Cooshohocken,PA 19428-2959,
Uoiled Slales. i,ldivrdual iepi;nls (singie or muiupie copies) of lhrs standard may be oblamed by coolacting ASTM a1 h e above
address or a1 610-832-9585 (phone), 610-832-9555 (fax), or ser/[email protected] (email); or lhmugh lhe ASTM wcbsile
(w.aslm.mg).