ASTM B733 Electroless Nickel Plating

7/24/2019 ASTM B733 Electroless Nickel Plating

1/13

Standard Specification for

Autocatalytic (Electroless) Nickel-Phosphorus Coatings on

Metal '

Thrs s tandard

is

l rsued u n d e r

h e

fired

deri mrionB

733:

the

n u m b c r irnmcdialcly f o l i o r i n ~

he

d r r i ~ ma t i o n

ndica~es

he

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

cpri lo~l

E)

ind~cvtes

n edilorial chanee

since

Ule l a s ~evision

or

reapproval.

Tlii s o rdord hm

bee

,~,~rol.i.dor sc

hl .

ogn~cicr /ihc Dcpornneni o/Defeme

1

Scope

1. I This specification

covers requirements for autocatalytic

(electroless) nickel-phosphorus coat ings applied from aqueous

solutions to metallic products for engineering (functional) uses.

1.2 The coatings are alloys of nickel and phosphorus pro-

-duced by autocatalytic chemical reduction with hypophosphite.

Because the deposited nickel alloy is a catalyst for the reaction,

tlie process is self-sustaining. The chemical and physical

properties of the deposit vary primarily with its phosphorus

content and subseque~it eat treatment. The chemical makeup

of the plating solution and the use of the solution can affect tlie

porosity and col ~os ion esista~iceof the deposit. For more

details, see S T M STP 265 (1) and Refs 2)

3)

(4) and 5 )

also refer to Figs. XI. 1, Figs. X1.2, and Figs. XI.: in the

Appendix of Guide

B

656.

1.3 The coatings are generally deposited from acidic solu-

tions operating at elevated temperatures.

1.4 The process produces coatings of uniform thickness on

il~egular ly haped parts, provided tlie plating solution circu-

lates freely over tlieir surfaces.

1.5 The coatings have multifunctional properties, such as

hardness, heat hardenability, abrasion, wear and col~osion

resistance. magnetics, electrical conductivity p~ ov id e iffusion

barrier, and solderability. They are also used for the salvage of

.om or mismachined parts.

1.6 The low phosphorus (2 to I

P) coatings are microc-

rystalline and possess high as-plated hardness (620 to 750

HK

100). These coatings are used in applications requiring abra-

sion and wear resistance.

1.7 Lower phosphorus deposits in the range between 1 atid

phosphorus are also microcrystalline. These coatings axe

used in electronic applications providing solderability, bond-

ability, increased electrical conductivity, and resistance to

strong alkali solutions.

This

ipec~fica lion

s under the jurisdiction

of

AST M

Commillce

8-08 on Melal

Pordcrr and

Mesa1

Powder

Produca

and is

the

direct

rcipo~ir~blllry

f Subcom-

millee

B06.08.01 on Englneenng Coat ings

C u nm , cdition approved

July

10. 1997.

Published October 1997. Oiiginally

published as

B

713 81 Last prevlour edit ion

B

733

90 (19941.

'The

boldfac,

numbrrr in

rercr lo a

lis1 of references 0

,hr

end of rhe ex, .

l .8 The medium phosphorous coatings (5 to

9

P) are most

widely used to meet the general purpose requirements of wear

and corrosion resistance.

1.9 The high phosphorous (more than 10 P) coatings

have superior salt-spray and acid resistance in a wide range of

applications. They are used on beryllium and titanium parts for

low stress properties. Coatings with phosphorus contents

greater than 11.2 P are not considered to be ferromagnetic.

1.10 The values stated in S1 units are to be regarded as

standard.

1.11 The following precautionary statement pertains only to

the test method ponion, Section 9, of this specification. T11is

s m ~ ~ d a r does norpurp or~o nddress al l o/r he sq/erv concerns.

i/ar??, associo~edwi ih ils use. IS rhe responsibilip o/lhe user

of lhis sla~ldnrd

1

eslnblish appropriare sa/e(v and Ircnlfh

pracrices and delern~inehe applicabil i~y /regula~oo; intira-

rio17s p,- ior lo use.

2

Referenced Documents

2.1

ASTM Sra~~dards:

B 368 Test Method for Copper-Accelerated Acetic Acid-

Salt Spray ( Fog) Testing (CASS Testing)'

B

374 Terminology Relating to Electroplating3

B 380 Test Method of Corrosion by the Corrodkote Proce-

dure3

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 Thick-

nesses by the Magnetic Method: Nonmagnetic Coatings on

Magnetic Basis Metals3

B 504 Test Method for Measurement of Thickness of Me-

tallic 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,oI ook o j l S T A 4 Yundords, Vol 020S

Copyrlghl

OASTM

International 100 Ban Harbor Dive. PO Box C100 Wart CmnrhMosXen PA

19428-2959,

United Slales


2/13

B 571 Test Methods for Adhesion of Metal lic Coatings3

TABLE Deposit Alloy Types

78 Test Metho d for M icrohardne ss of Electroplated Type P h o ~ p h o w ~

~t

Coatings3

Nil

Requi remen1

for

Phosphorus

B 602 Test Method for Attribute Sampling of Metallic and

I I

I 1 0 3

Inorganic Coating"

2

io

4

IV 5 to 9

B 656 Guide for Autocatalytic Nickel-Phosphorus Deposi-

v

10 and

above

tion on Metals for Eneineerine Use3

B

667 Practice for Cot%uctio; and Use o f a Probe for

Measuring Electrical Contact Resistance"

TABLE

2 Service Conditions

B 678 Test Method for Solderability of Metallic-Coated

Coating Thickness Requirements

Products'

Mtn8mum

Coaling

B 697 Guide for Select ion o f Sampling Plans for Inspection

C o n d l l o n Thickness ~ r m in ( m m )

SpeciScauon

of Electrodeposited Metallic and lnorganic Coatings"

SCO Minlrnun Thickness

0.1

0.000004

(

B 762 Method for Variable Samplin g of Metallic and Inor- S C I

Light

Service 5 0.0002

(

ganic Coating?

SC2 Mild Service

13 0.0005

( )

B 849 Specification for Pre-Treatment of Iron or Steel for

sc3 Moderate Service 25 0.001 [ )

SC4

Severe Service 75 0003 (

)

Reducing the Risk of Hydrogen Embrinlement3

B 850 Specification for Post-Coating Treatments of lron or

Steel fi r Reducing the Risk of Hydrogen Em brittlement3

MIL-S-13 165 Shot Peening o f Metal PartsI3

B 85 1 Specification for Autom ated C ontrolled Sho t Peening

MIL-STD-105 Sampling Procedures and Tables for lnspec-

of M etallic Articles Plior to Nickel, Autocatalytic Nickel.

tion by AttributeI3

Chromium. or As A Final Finish3

2.3

IS0

Standards:

D 1193 Specification for Reagellt Wale9

1SO 4527 Autocata lytic Nickel-P hosphoru s Coatings-

D2 67 0 Method for Measur ing Wear Propert ies of Fluid

Specification and Test Methods"

Luhricants (Falex Methodi6

~~

~~ ~ ,

D 2714 Method for Calibration and Operation of an Alplia

LFW-I Fr ict ion and Wear Testing Machine6

D 1951 Practice for Commercial Packaging'

D 4060 Test Method for Abrasion Resistance of Organic

Coat ings by tl ie Taber ~ b ra se r '

E

60 Practice for Photometric h4ethods for Chem ical Analy-

sis of Metals9

E

156 Test Metliod for Det erm inati o~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 Mechan ical H ydrogen Embrinle-

m en t l l

G 5 Practice for Standard Reference Metho d for Making

Pote~itiostatic and Potentiodynamic Anodic Polar izat ion

Measurements"

G

3 1 Practice for Laboratory l~ nn ~e rs io norrosion Testing

of Metals"

G 59 Pract ice for Conducting Potentiodynamic Polar izat io~i

R es ~s t an ceMeasurements"

G 85 Practice for Modified Salt Spray (Fog) Testing"

2.2 144ilira1,~ ta17 dar.d~:

MIL-R-81841 Rotary Flap Peening of Metal PartsI3

.4nri?rol Book o/ASTM Slundords. Vol 0J.04.

4 i??


3/13

include requirements for diffusion barrier, undercoat, electrical

4.3.6 Class 6-Heat treatment at 300 to 320C for at least 1

co~~ductivitynd wear and corrosion protection in specialized

h to improve coating adhesion for titanium alloys.

environments.

NOT -Heal-treatable aluminum alloys such as Type

7075 can

4.2.3 SCl Light Ser?'ice, wpThiss

a

undergo

micrortructu~vl

changes

and

lose strength

=,hen licarcd ro o v e r

minimum coating thickness of 5 pm for extending the life of

130-c

the part. Typical environments include light-load lubricated

wear, indoor corrosion protection to prevent rusting, and for 5. Ordering Information

soldering

and mild abrasive wear.

5.1 Tlie following informati011 shall be supplied by The

4.2.4 SC2 ~ i l dervice, 13 W-This is defined by mild

purchaser in either the purchase order or on the engineering

corrosion and wear environments. It is characterized by indus-

drawing of the pan to be plated:

trial atmosphere exposure on steel substrates in d~ or oiled

5.11 T ~ ~ ~ ~ , A S T Mesignation number, and year ofis sue of

environments.

4.2.5 SC3 Moderare Service, 25 pm-This is defined by

moderate environments such as non marine outdoor exposure,

alkali salts at elevated temperature, and moderate wear.

4.2 .6 SC4 Severe Se n~ ice, 5 pm-This is defined by a very

aggressive enviro~lment.Typical environments would include

acid solutions, elevated temperature and pressure, hydrogen

ulfide and carbon dioxide oil service, liigll-temperature chlo-

ride systems, very severe wear, and marine immersion.

NOTE

?-The

performance

af the autacatalytic nickel coating depends

ra a

large

errent on r be surface finish

of t h e

article to be plated and

lrow

t was prelreated. Rough, non uniform

surfaces

require thicker coutinxs

than smootll surfaces to achieve maximum corrosion res is tance and

minimum porosiry

4.3 Posr Hear Pear1ne111 Class-The nickel-phosphorus

coatings shall be classified by heat treamient after plating to

increase coating adhesion and or hardness (see Table 3).

4.: l Class I-As-deposited, no heat treannent.

4.3.2 Class 2-Heat treatment at 260 to 400C to produce a

minimum hardness of 850 HK100.

4.3.3 C1as.r 3-Heat treatment at

180

to 200C for 2 to 4 11

to improve coating adhesion on steel and to provide for

hydrogen embrittlement relief (see section 6.6).

4.3.4 Class 4-Heat treatment at 120 to 130DC or at least

h to increase adhesion of heat-treatable (age-hardened) alumi-

nun) alloys aud carburized steel (see Note 3).

4.3.5 Class 5-Heat treatment at 110 to 150C for at least I

i to improve coating adhesion for aluminum, non age-

hardened aluminum alloys, copper, copper alloys and beryl-

liutn.

TABLE Classification

of

Post eat

Treatment

LRSS

Oe~cription

Temperature xme hl

iCl

1 No HealTrealment A s Plated

2

Heal Treatment for Maximum Hardness

TYPE

260

285

320

nn

TYPE

I

TYPE I l l

TYPE

IV

TYPF

V

3 Hydmgen

Embriniemenl

and 180 o 200

Adhesion

on

Sleel

4

Adhesion.

Carburized

Steel and 12010 130

this specification.

5.1.2 Classification of the deposit by type, service condi-

tion, class, (see 4.1, 4.2 and 4.3)

51.3 Specify maximum dimension and tolerance require-

meuts, 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.

51.8 Suppletnental or Special Government Requirements

such as, specific phosphorus content, abrasion wear or corro-

sion resistance of tlie coating, solderability, contact resistance

and packaging selected from Supplemental Requirements.

5.1.9 Requirement for a vacuum, inert or reducing atmo-

sphere 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).

NOT &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 .

6 Materials and Manufacture

6.1 S~~bslrare-Defects in the surface of the basis metal

such as scratches, porosity, pits, inclusions, roll and die marks,

laps, cracks, burrs, cold shuts, and roughness may adversely

affect the appearance

and performance of tlie deposit. despite

the obser\.ance of the best plating practice. Any such defects on

significant surfaces shall be brought to the attention of the

purchaser before plating. The producer shall not be responsible

for coatings defects resulting from surface conditions of the

metal, if these conditions have been brought to the attention of

the purchaser.

6.2 P,.er~eamte~il- -Pans o be autocatalytic nickel plated

may be pretreated in accordance with Guide B 656. A suitable

method shall activate tlie surface and remove oxide and foreign

materials, which may cause poor adhesion and coating poros-

ity.

Age Hardened Aluminum

NOT

-Heat

treatment of the base material may effecr its metallur-

5 Adherlo

on

Beryllium and 140 o 150 to 2

Aluminum

eical properties. An example

is l eaded

steel

which

may exhib i t

l iquid or

6 Adhesion on Xlan ium 30C~320 1 4 solid ernbrittlemen1

afrer

heal

treatment.

Careful selection of the

pre

and

past heal treatments are recommended.


4/13

6.3 Su-ess

elief

6.3. l Prerr-ealnienl offron andSleel/or~Reduci iighe Risk of

Hydrogen En~brirllemenl-Parts that are made of steel with

ultimate tensile strength of greater than 1000 Mpa (hardness of

31 HRC or

greater ,

that have been machined, ground, cold

formed, or cold straightened subsequent to heat treatment, shall

require stress relief hear treatment when specified by the

purchaser the tensile srrength to be supplied by the purchascr,

Specification B 849 may be consulted for a list of pre-

treatments that are widely used.

6.3.2 Peening-Peening prior to plating may be required on

liigh-strength steel pans to induce residual conipressive

stresses in the surface, which can reduce loss of fatigue

strength and improve stress corrosion resistalice 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.

Nors Contolled shotpeening

is

the preferred method because rhere

- - a r e

georneoy's where rotary flap peening is not effective.See S11.2.

6.3.3.1 Unless otl icwisc specified, tlie shut peclling shall be

accomplished on all surfaces for which the coating is required

and all immediate adjacent surfaces when they contain notches,

fillets, or other abrupt changes of section size where strcsscs

will be concentrated.

6.4 Racking-Parts should be positioned so as to minimize

trapping of hydrogen gas in cavities and holes, allowing free

circulation of solution over all surfaces to obtain uniforni

coating thickness. The location of rack or wire marks in the

coating shall be agreed upon between the producer and

purchaser.

6.5 Plarirtg Process:

6.5.1 To obtain consistent coating properties, the bath niust

be monttored periodically for pH, tcmperature, nickel and

liypopliosphite. Replenislments to the plating solutioli should

be as fiequent as required to maintain tlie concentration of :lie

nickel and l~ypopl~osphireetween 90 and 100 of set point.

'he use of a statistical regimen to establish tlie control limits

-nd frequency of analysis may be employed to ensure quality

deposits are produced.

6.5.2 Mechanical movement of parts and agitation of tlie

bath is recommended to increase coating smoothness and

uniformity and prevent pitting or streaking due to hydropcn

bubbles.

6.6 Posr Cooririg T,rarn~erif,forrorr arid Sleel/or Redt,cirig

the Risk of HI^-ogen Ei7ibrir/ler1re1ir Partn that are made of

steel with ultimate tensile strengths of 1000 Mpa (hardness of

31 H R C or greater), as well as surface hardened parts, shall

require post coating hydrogen embrittlement relief baking

when specified by the purchaser, the tensile strength to be

supplied by the purchaser. Specification

B

850 may be con-

sulted for a list of post treatments that are widely used.

6.6.1 Heat treatment shall be perfomied prefetably within 1

I1 but not Inore than 3 li of plating on plated afier plating of

steel palis to reduce tlie i s k of hydrogen enibrittlement. In all

cases, the duration of thc hcat trcatment shall cornmetice from

the rime at which the wl~o le f each part attains the specified

temperature.

6.6.2 Higli-strength steel pans with acrual tensile strengths

greater than 1000 MPa (corresponding hardness values 300

HV10,303 HB or 3 HRC) slid surface hardened parts shall be

processed after coating in accordance with Specification B 850.

6.7 Hear Trennnenl Afler- Platir rg ro Intpwve Adhesiort-To

improve the adhesion of the coating to various substrates, the

heat treatments in Table 3 should be perfonned as soon as

practical after plating (see 4.3 .

6.8 Heal T,-ealmenl 4per Pla ti ,~g o Irrcreose Har-drress:

6.8.1 To increase the hardness of the coating a heat treat-

ment of over 2h03C is required. Table 3 describes thc heat

treatment for maximum hardness.

6.8.2 See Appendixes 3 and 4 and Guide B 656; Figs. X1.2

and Figs. X1.3.

6.8.3 A heat treatment at 260C for greater than 20 h should

be used to reduce rhe loss of surface hardness and strength of

some ferrous basis metals. Avoid rapid heating and cooling of

plated parts. Suficient time must be allowed for large parts to

reach oven temperature.

NOTE 7-The length of time to reach maximum hardness vanes with

the phosphorus content of

the deposit.

High phosphorus deposits may

require longer time or

a

higher rempcrarure, or both.

Individual

alloys

should e tested for rnaxinum hardness attainable, especially for condi-

t ons o f lower temperarures an d longer timcs.

NOTE 8-Inerr or rcducing atmosphere or Wacuum rufficienro prevent

oxidation is recamrnendzd for hear treatment above 260C. a not usegas

containing

hydrogen

u,ith

high-srrength steel

parts.

7. Requirements

7.1 Process-The coating shall be produced froni an aque-

ous 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~i ificant urface (sce section 5.1.3).

UOIE 9-The thickness

of

the caatms canno1be canrrolled

in

blind or

small

diameter dcep holes or where salution circulat~ans rcsrricted.

7.2.3 Adl~esion-The coating shall have sufficient adhesion

to the basis metal to pass the specified adhesion test (see 9.4

and Test Methods

B

571).

7.2.4 Porosi+The coatings sliall be essentially pore free

when tested according to one of the methods of 9.6. Tie test

method. the duration of the test, and number of allowable spots

per unit area shall be specified (see section 5. 11 0 and 9.6).


5/13

7.3 Qual~ficaiionRequirentenrs-These requiremetits are 8.3 All specimens used in the sampling plan for acceptance

placed on the deposit and process and are performed on

tests shall be ma de of the sam e basis material and in tlie same

specimens to qualify the deposit and plating process. Tlie tests

metallurgical condition

as

articles being plated to this specifi-

for these qualifica tion requiremelits shall be perform ed cation.

monthly or more frequently. 8.4 All specimens shall be provided by the purchaser unless

7.3.1 Compositiot~-Type 11 111, IV, V deposits shall be

ot he nr ise agreed to by the producer.

analyzed for alloy composition by testins for

P ~ ~ ~ P ~ ~ ~ ~

see

N~~~

1 1 -~ l , ~ au to cawly r ic n ick e l p raccs r i s d mamic an d

a

daily

9.1). The w'e~ghtpercent of pl i os pl lo ~ s hal l be in the range

is recommended.

For

Coatings requiring alloy analysis and

designated by type classification (see 4.1).

corrosion tes t ing w eekly sampling sho uld be considered a s

an

opuon.

7.3.2 Micioho~-dness-The microhardness of Class 2 depos-

its shall be determined by Test Method

B

578 (Knoop). For

Class

coatings, the microhardness sliall equal or exceed a

minimum of 850 (HKLOO (or equivalent Vickers) (see 4.3 and

9.5). Tlie conversion of Vickers to h o o p using Tables

E

140

is not recommetided.

7.3 .3 M ~d ro ge rl E1tibrirrieme17r-TI1e proces s used to de-

posit a coating onto high shength steels shall be evaluated for

'lydrogen embrittlement by Test Method

F

519.

8.

Sampl ing

8.1 The purchaser and producer are urged to employ statis-

tical process control in the coating process. Properly perfomled

this will ensure coated produ cts 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 non e of them will be accepted.

7 )

8.2 The samp ling plan used for the inspectioti of a quantity

of coated parts (lot) shall be Test Method B 602 unless

otherwise specified by purchaser in the purchase order or

contract (see section 5.1.11 and S.Il.1).

NO TE 10-Usually. %.hen

a

collect ion of coated parts ( the

inspection

lot

E.21 is examined for compliance with the requirements placed

a n the parts

a

relatively small number of parrr, the sample, is selected

at

random and

inspected . T he inspection lor is l i~ en classif ied as complying or

no

9

Test Methods

9.1 Deposil An ahs is /or Phosp horus:

9 . 1 . 1 Ph o s p h o r r~s Dererniinarion 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 absorption,

emission or X-ray fluorescence spectrometry.

N O T E

12-inductively

coupled plasma techniques can determine the

.

alloy to with in 0 .5 %.T he fo l lowing analysis wavelength l ines have been

used with min imu m inteiference to determine the alloy.

Ni 216 10

rn

Cd 214 44nrn Fe 238 20 nrn

215 40 nrn O 238 34

nm Pb

283 30nm

213 62

nrn

Cr 284 32 nm Sn 198 94nm

l 202 55

nrn

u 324 75 nnr Zn 206 20

nrn

9.2 Appenrance-Examine the coating visually for compli-

ance with the requirements of 7.2.1.

9.3 Tltickf~ess:

NOTE

13--Eddy-current type insrruments give erraric meas urem ents

d u e to variarions in conductivit y of the coalings with chang es in

phaspharur content .

9.3.1 Mio.os copica 1 Merhod-M easure tlie coating thick-

ness of a cross section according to rest Method

B

487.

NOTE

L T o protect the edger , e lccrroplare the specimens with

a

minimum of f n ickel

or

capper prior to roir sectioning.

com ply ing u.ir11

rbe requirements

bared

on

the results of the inspection

sample,

Ti e

the

sample

and the cr i ter ia of

9.3.2 Mogiiefic Inducfion I~ ~ sl ru i i ~e nfethod-Test Method

.

etermined by the applicat ion of s ta t is t ics . ~h~ ~m c ed u re s known as

B

499 is applicable to magnetic substrates ~I a t e d ith auto-

samolinc insoecrion. Three

standards

Test Method B 602. Guide B 697.

catalvtic nickel deoosits. thar contain more than 11 mass

%

- .

and Test Method B 762 conlain rampling p lans

rhat are

designed

far thc

phosphorus (not ferrom agnetic) and that have not been heat-

sampling inspection of coatings.

treated. The instrument shall be calibrated with deposits plated

Tesr

Method B 602 conrains four sampling p lans, three fa r

use

with tests

in the same under the

same

on magnetic

thal are nondestructive and

one

for use w th tes ts hat

are

destructive. The

.--..

purchaser and produccr may agree an the plan(s) to be used. lf rhe y do not.

Terr Merhod

B

602 identifier th e plan to be used.

9.3.3 Be ta Bac krcalte t, Meihod-Test Method 567 is only

Guide B 6 9 7

a l ye

n u mb er o fp lan s an d piv s guidance to

coatings On magnesium,

an

he selecrion

of a dan. When

Guide

697 is rDccihed, rhc purcl aser

and titan~um. he instrument must be calibrated with standards

and producer need

to a g e e on

the plan to be used.

havitlg the same compositioti as the coating.

Test Method B 762 can be used only for coating requirements that have

15-The density

varier

u , i rh t s

mass

%

a

numerical limir, such as coating th icknerr .

The

last must yield

a

ms

content

See

Appendix X2).

numcncal value and certa in swrirr ica l reauiremeers

must

bc met. Terr

Merhod B 762 contains several p lans and a lso g ives instmclionr for

9.3.4 Micrvtnerer Melhod-M easure the vart, rest coupon,

.

. . .

calculating

plans

to

meet

speeia l needs. The purchaser and producer may

or pin ill a specif ic spot before and after plating using a suitable

n

the to b e

If do

Test 762

micrometer Make sure that the sutiace s measured are smooth,

identifies the plan ro

be

used.

clean, and dry.

An inspection lat shall be defined

as a

collection of coated parts which

are

of the same kind, that Ihave becn produced to th e samc rp ec i f i ca t~o n ,

9.3.5 Weigh, Pia re. Weigh Method-Using a similar sub-

that have been coated by

a

s ingle producer a t one rime

ar

approximately

strate

surface area, weigh the nearest

the same time undcr essentially identical conditions, and thar

are

submit-

milligram before an d after plating making sure that the Part or

ted

for

scceprance

or re ject~on

n

a

group.

coupon is dry and at room ternperamre f i r each measurement.


6/13

Calculate the thickness from the increase in weight, specific

gravity, and area as follows:

where:

It

=

weight gain in milligrams,

1

=

total surface area in squarc centimetres, and

= gram s per cubic centimetres (see Appendix X2 ).

9.3.6 Coulo~aerricMethod-Measure the coating thickness

in accordance with Test Method B 504. The solution to be used

shall be in accordance with manufacturcr's recommendations.

Tlie surface of the coating shall be clea ned prior to testing (see

Note 14).

9.3.6.1 Calibrate standard thickness specimens with depos-

its plated in the same solution under the same conditions.

9 . 3 . 7 X - R a y S p e o r o r n e r ~ ~ M e a s u r ehe coating thickness

in accordance with Test Method B 568. Tlie instrument must be

alibrated with standards having the same composition as the

-coat ing.

NOT l&Ti>is method is only recommended for depasjts in

the

as-plared condition The phosphorus c o n te n t o f t h e coating must

b e

known

to calculare t he

thickness

of the deposit. Mahix effect

d u e

to the

dismbutian

of

phosphoms in layers af t he coating

also

effect the

measurement

accuracy

and

require

t h a ~ a l ib r at io n svrndards be made

under the same conditions as

the

produclion process

9.4 Adhesion:

9.1.1 Be nd Tesl (Test Me tliods 571)-A sam ple specim en

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 d ete m~ ine he

.,

,

derennination is permissible.

9.6 POI-osih,-There is no universally acce pted test for

porosity. When required, one o ft he 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 fo r Iron-B ase Substrares-

Completely 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 m ore than 20 min after tlie initial application

of heat. Continue to boil the water for 30 min. Then rem ove the

pa n, air dry, and exa mine 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. Th e pH of the aerated water should h e 6.7 0.5.

9.6. 3 A er nl ed N'aler Test fo r Iro n- Ba se Su bsrt-ares-

Immerse the part for 4 h in vigorously aera tedT ype 1V or better

water (see Specification D 1193) at 25 C temperature and

then examine the part for rust spots.

9.6.4 Alimriri Tesr for Al rdi ~~ i~~ ur nllo~,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 gl ac ~a l cetic acid until the violet color

disappears. Any red spots remaining indicate pores.

9.6.5 Po ro si h Tesr for Coppe r Subslrares-Wipe the plated

aoneslon 1s suggesrea.

pa n or specimen with glacial acetic acid After 3 min, apply a

ari 17-Appropnare rest specimens

are strips approximately

5 ta 50

mln wide,

200

lo 300

mm

long

and

3 to 6 mrn illick

9.4.2 In ~p nc t Tesl-A spring-loaded ce nter punch with a

\-point having 2 to

3

radius is used to test adhesion of the

coating on nansignificant suifa ces of the plated pa n. Make

three closely spaced tndentations and examine under IOX

~iiagn ificatlon or flaking or blistering o f the coating, w hich is

cause for rejection.

9.4.3 Tl7er-mnlS11ock-The coate d p a n is heated to 200C in

an oven and then que ~ic hed n room temperature w ater. The

coating is examined for blistering or other evidence of poor

adhesion at 4X magnification.

9.5 M~c~ahard,?ess-The microhardness of the coating can

be measured by Test Method B 578 using Knoop indenter and

is reponed in Knoop Hardness Number (HK). It will v a ~ y

depending on loads, type of indenter, and operator. A100 g load

is r ecom m en ded. l l ~ ehombic Knoop indenter gives higher

hardness readings than tlie square-hase pyramidal Vickers

diamond ~n denter or 100 to 300 g loads, see Ref 6). For

~na rim urn ccuracy, a minimum coating thickness of 75 p n is

recommended. Conversions of Vickers or K~ioophardness

number to Rockwell C is not recommended.

Nore 1 8 4 n

hick

(75 pm+)

coatings

on steel a

surface

microhardness

solution of potassium ferrocyanide prepared by dissolving 1 g

of potassium ferrocyanide and 1.5 methyl cellulose in 90 mL

of boiling distilled \x8atcr.The appearance of brown spots after

2 min indicate pores.

9.7 Ot he r Tesl Methods-Test meth ods whic h 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 Rehear ing

10.1 Part(s) that fail to conform to the requuements of this

standard may be rejected. Rejection shall be reponed to tlie

producer promptly in writing. In the case of dissatisfaction

occurs with tlie results of a test, the producer may make a claim

for a hearing Coatings that show imperfections may be

rejected.

11. Cert i f icat ion

11.1 When specified in the purchase order or contract, the

purchaser shall be furnished certification that tlie samples

representing each lot have been processed, tested and inspected

as directed in this specification and the requirem ents have been


7/13

met. When specified in the purchase order or contract, a report

of the test results shall be funislied.

12.1 autocatalytic; chemical nickel; coatings; conductive;

comosion resistance; electroless; functional; nickel: nickel

phosphorus; wear resistance

S U P P L E M E N T A R Y R E Q U I R E M E N T S

The following supplementary requirements shall apply only when specified by the purchaser in tlie

contract or order.

S1 .l Shot Peening-W hen 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~po sifion-When specified by tlie purchaser in the

orderiny information the phosplioms content shall be main-

tained in the deposit to within 1

.

Use the test methods

described in 9.1.

S l .3 1rrer.fArmosphere-When spec ified by the purch aser in

the orderiny information, the coating shall be heat treated in a

vacuum, inert, or reducing am ~os plie re o prevent surface

oxidation of tlie coating.

S1.4 Hy drog en Embi-itrlemerzr-When spec ified by the pur-

chaser in the ordering informatinn tlie plating process shall be

evaluated at the time of processing pans for hydrogen em-

brittlement using Test Metho d

F

5 19.

S1 Abr-orice Wear-When speci fied by tlic purch aser in

the ordering information, the coating shall be tested for

abrasion wear resistance using the method in Appendix XI of

this specification. Thc coating sh all tuect a maxim um wear rate

which is specified by the purchaser and agreed to by the

producer.

1 .6 Adhrs i~ ,eWeor-When spec ified by tlie purc haser in

ordering information, the coating shall be tested for

hd lie siv e wear resistance usine T est Method D 2714 or Test

S1.7 Coi7tacr Resisrance-W hen speci fied by the purch aser

in the ordering information. the coating shall be tested for

contact resistance using Test Method

B

667.

S1.8 Solderabili1)-When specified by the purchaser in the

ordering information, thc unaged coating shall pass Test

Method B 678 on solderability.

S1.9 Corrusiori ResisfanceWhen specif ied 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 tlie coating to a specific liquid medium can be

determined by means of immersion tests (see Practice

G

3 I ) or

electrochemical test (see Practices G 5 and G 59).

S1.10 irling Col.,nsiorl Resbrance-Use Method

G

85

(acetic acid-salt spray test), Method B 368 (copper-accelerated

acetic acid-salt spray, CASS), or Method B 380 (Corrodkote)

lo evaluate the corrosion resistance of the coating to pitting.

S 1. l S pe cioi Go ve n ~ ~ n e n teqlrirernents:

S 1.11.1 Sonipling-Part(s) plated for the US Govcrnrnent

and Militaly use shall us e MIL -STD-105 as tlie sampling plan.

S l .I I. 2 Sl ~o t eening--High strength steel palt(s) pro-

cessed Tor US Government and Mililaty use shall be shot

peened in accordance u.ith M IL-S-13 165 or rotary flap peened

in accordance with MIL-R-81841. (see Note

6).

Method

D

2670. Ih e wea r rite shall be specified by the

S I . 11.3 Packaging--Parts shall be packaged in accord ance

purchaser and agreed to by the producer.

with Practice D 3951.

A P P E N D I X E S

(Nonrnandator Inlormation)

XI

T AHE HAB RAS E R W E AR TEST M E T HOD

Xl . 1

cope

the laboratory and [he storage

conditions o

[he CS-10

WIIPP IP

are

X1.1.1 This test method will evalu ate the resistance of the

be conrrol lhe

J u m i d i v bewee

tests

coating to abrasive wear. The test is performed by rotating a

X1.1.2 The results are variable between tests and therefore

plated panel under rotatins rubber wheels and weighing the

three plated test specimens should be tested to 6000 cycles

panel after each 100 0 cycles for weigh t loss. Duration of the

each. The results should b e averaged w itl~ ou t he first 1000

test is 6000 cycles and it can be extended to 25 000 cycles for

cycles and abrasion wear resistance is reported as the

more complete resnlts.

wetght loss in rngIlOO0 cycles (Taber Wear Index).

NOT ll-Variation in results ha\w been atrributed la the humidiry i n


8/13

X1.Z pparatus X1.3.2 Wear test the specimens. For each of the three

X1.2.1 Taber Abi-asei. 14ear- Tes ting Unit-The un it mu st be

specimens complete the foilowing steps:

capable of loading u itll 1000 g load and operating w ith a

X1.3.2.1 Run the CS-I0 wheels on the coating for 1000

cycles to remove any surface roughness. The wheels shall be

vacuum.

loaded with 100 0 with a vacuum on high for the entire test.

X1.2.2 A~I-asior?Wlzeels- Use CS-10 (resilie nt rubb er)

X1.3.2.2 c o o l weigh (he specimen to the nearest 0.1

Taber wheels. To reface the whe els use

CS-I1

discs from Taber

,-

The hardness of CS-I0 wheels can change with time and call

X1.3.2.3 Dress the CS -I0 w heels with a CS-11 disc for 50

effect the reproducibility o f results (see Test Metho d D 4060 ).

cycles

X1.2.3 k t Specimeiu- Test specimen s shall be made

from 20 gage CR steel 4 by in. (100 by 100 by 1.3 m m) with

a 0.250 (6.35 mm) hole in the center. Test specimens are

available from Taher.

X1.2.4 Ana/lrrcal Balance-Scale which is capable of mea -

suring lo 150 g 0.1 mg .

X1.3 Procedure

X1.3.1 Plate three specimens with 0.001 in. (25 pm) of

-nickel phosphorus coaling.

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 specl-

men.

X1.4 Reporting

XI .4.1 Determine the average weight loss in milligrams for

each sp ecimen per 100 0 cycles Taber Wear Index and the mean

weight loss per 1000 cycles for all specimens. Report the mean

and stand ard deviation fo r the coating.


9/13

XZ

DENSITY O F UTOC T LYTIC NICKEL DEPOSITS

ensity

of

Electroless

Nickel

Deposits

A

R ei de l, Wd fgan g , E l e i t r o l e r r N i ck e l P l a tmg . ASH 1n :er nal l ona l. H e r a l r Pa r k .

OH

1991, p92 DIN 5096 6

+ IS0

52:

Annex

Vendor . E ln l r , unpubl l rhed

Ratam,

C S

ajam r t a 1 M e t a i

Flo\ rh \og.

V o l 88 No 11

119401

N I S T . F ~ e l d ~ n ggburn e l a\ . P:at lnq an d Sur face F lntsh lng, V a l 68, No 3 l I '18 l l

K a n q e n , AS T M S I P

No

265 . i l e r t r o l e s s N l c k e l P l a t ~ n g 959

Oak

Rldse

D Smith, Thermal Condurr iv8ty

o f

E l ec t r a l e r r N l i k e l - Phos phor us A I l c y P l a l lng . N ahana l

Sr lente Foundahon, 1'163

Garbunova. K

M

lorbunova and A A N l k t o roua . Phy s ~ r a c he m~ i a l

Pr lnr lp les a f N i c k e l PIa t8ng. N a t~ a na l oenc e Founda i l an '963

endor S i he rl ng . u i l pub l ~ s hed na l y t~ c a l es u l t s . S r he r mg KG, Be r l ~ n 982

M a ll or y. G l e x Ha: la ry t al , s tudies nd P r o p e r t i e s o f Very H ar d E l ec t r o l es s

Nickel

D e p a i c t r

EN'95. ( lardner Management. Cinclnn at. OH 1995

FIG X2 1

Density

of

Autocatalytic Nickel Phosphorus Alloy Summaw of Reported Values


10/13

X3

H RDNESS VERSUS HE T TRE TMENT

HARDNESS

OF

ELECTROLESSICKEL

v

TEMPERATURE

TYPE

OO

I ' 1

1 2 3 OO 5

TEMPERATUREC) I HOUR

FIG. X3 1 Hardness of Autocatalytic Nickel Phosphorus Versus Heat Treatment Versus Phosphorus

X4

L L OY T Y P E S

NOTE

X?

-lllese d~fferentlloy

TYPES are

produeed from processes point . These di5erences are produced by micro s t ructural

which are specifically formulared and controlled. Additional requirements

d i5 er en ce s b etw een ~i N i 3 p a nd ~ i 3 ph~~~ differences

f r internal mess purity and elong tion

may

be

necessary

for same

applicarions.

also effect non-destmcti\ e thickne ss resting by X-Ray and

magnet ic means . Careful a t tent ion to the select ion of TYPE

X4.1

The physical di fferences of these TYPE S provide for mill insure opt imu m pe rfo nn ai~ ce f the deposi t in the intended

a wide variation in perform ance in wire bonding contac t

application.

resistance machineability lubricity reactivation and melting


11/13

H RDNESS STRENGTH

M GNETICS TYPES

L O W HIGH O F R R O

MAGNETIC MAGNETIC

FIG

X4 1 Selected Properties of s Plated utocatalytic Nickel Phosphorus Coatings by Phosphorus Content

X5 SU MMA R Y PR O G R A M

4

X5.1 Results o 110 Mo17lh Exposrtrr

o f

Aulocatalylic

Nickel Deposits a/ Kurv Beach North Caiolina:

X5.1.1 Program 14 is part of an ongoing marine exposure

testing process at the 75 m site at LaQ ue Ceriter for Corrosion

echnology, Wrightsville, N C (Kure Beach). The program

called for the plating of both Type IV and Type V deposits on

standard smooth and ground steel Q Panels.

X5.1.2 There were nine different sources of deposits, each

providing five lots of five panels. Th e program involved plating

12.5, 25, and 75 pm thicknesses on smooth and ground surface

and one smo oth lot heat treated for hardn ess at 5 50 C for 2 11.

The heat treatment temperature was considerably higher than

typical processing and was chosento 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 thickness.

Panels were rated at Kure Beach each year by a team from

A ST M Committee using Practice B 537.

X5.1.4 Th e interpretation o f the results of these exp osure

test should be made on the basis of general performance of the

coating on panels. Base metal condition, undercoats, surface

preparation, arid post processing all have a significant effect on

the performance and should be given careful consideration

whe n designing the part and pretreatment processing sequence.


12/13

TABLE X5.1 R e s u l t s o f 110 M o n t h E x p o s u r e

of

A u t oc a t a l y ti c (E l ec t ro l es s ) N i c k e l Depo s i t s a t Kure B eas h , No l t h Ca ro li naA

P ~ O S D ~ O R I Slloy

%wf

Ractice

Source Lot

Heal

Thickness, Thickness,

Deposit Type

B 537

Treatment

pm Target

pm

Actual

ICP

Ralings 110

E D M Months

1 Smoolh NO 12.5 3.6

1 3 0

Smooth

Smoolh

Smoolh

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 Smooth

No

12.5

2 Smooth

No

25

3 Smooth

No

75 80 7.1

4

Smooth Yea 25

5 Gro.nJ

ro

23 L O

Te ronr

.,on

'rum in s mar

r e

e x v o s ~ r c o g r m

l a. o w n

s.mmanzro

o)

Dr

George ) B a n

ol h :D

11 s

caper Mar :on05

o

i2etiormnn~r.1

C h :os.t nq

o r

Slce

F

r a Reporl

un

ASTM Fogr l - 14

ho

r h s DrcSPnleJ al i h r l

(:oo c.enre

P r o L r F

n s n

1.2

REFERENCES

(1) Symposium on Elecnolesr Nic ke l Plat ing, AS TM STP 265 ASTM,

12644 Research Parkway, Orlando,

FL

32826, 1986 Chapter 23.

1959.

(5)

M al l a r y

G.

and

Ha jd uI . Elecholess Plaling. . lESF 12644 Research

(2)

D ? ~ i ~ ~ r e r - i , i gl.oprr-lies q(E1ecnuless Nickei, Th e lntem arianal N ick el

Parkway. Orlando, F L 32826. 1990.

Ca.,

Inc.

Ncw York, N'i

(6)

Parker, K,~ ardness and ear Rerirra nce Tests

of

Elecrrolers N ickel

(3) Gawri lav , C. G. C l ~ e n ~ i c o lE lecnu lers ) N i d e l P lo ting , Pancu l l i s

Deposits, P lo r i ,? ~, ol 6 1 September 1971.

Press, London. 1974.

7 )

Parker,

K.,

Effects

of

Hea t Treatment on the Prapenier

of

Eiecrroiess

4)

Safranek,

W

H.. Tile P,-oper-ties

o

Elecnadeposired hf~:Iolr

orzd

Nl cke l Deposits.

Plorisg orzd B,r;/ cr

Fi,iishirrg. Vol 68, Decembe r

A/lr,~..


13/13

ASTM inleroa1,Onal lakes

no

position respecling lhe validity of any paten1 ghlr asserted n conneclion wih any rlem mentioned

in hi s sfanaard. Users of

h

sfandaid are expressly adwsed lhal deleiminalion of ihe vaiidi ly of any su h palent rlqhls, and lhe nsk

of infnngemeol of such rights, are enl~rely heii own rerpoosibil,ly

This sleodard K subjecl to revision a1 any time by lhe iesponslbie lechnicai comminee and musl

t

eviewed eveiy five years and

if no1 revised, either reaowved r wrhdrawr~. our commenls re invited miher t rrevision oi his slandaid r for oidditiooal standards

and should be addressed lo ASTM lnlemal~onalHeadquarlers. Youimm menls Wli receive camfvl mosideiation a1

a

meeling of me

iesponsibie lecnnicai cornmillee, whrch you may anend if you feel ihal your mmmeotr have

ot

received

a

f ir heai~ng ou should

make your views known lo the ASTM Commitlee n Standards, a1 the address shown below

This slarldard is copyrighled by ASTM lnternaliononai. W an aao i Drive. PO

ox

C700, West Cooshohocken, PA 19428-2959,

Uoiled Slales. i,ldivrdual iepi;nls (singie

r

muiupie copies)of lhrs standard may

e

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.as lm.mg) .

ASTM B733 Electroless Nickel Plating

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Transcript of ASTM B733 Electroless Nickel Plating