This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: B733 − 15

Standard Specification for

Autocatalytic (Electroless) Nickel-Phosphorus Coatings on
Metal 1
This standard is issued under the fixed designation B733; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope bondability, increased electrical conductivity, and resistance to

1.1 This specification covers requirements for autocatalytic strong alkali solutions.
(electroless) nickel-phosphorus coatings applied from aqueous 1.8 The medium phosphorous coatings (5 to 9 % P) are most
solutions to metallic products for engineering (functional) uses. widely used to meet the general purpose requirements of wear
1.2 The coatings are alloys of nickel and phosphorus pro- and corrosion resistance.
duced by autocatalytic chemical reduction with hypophosphite. 1.9 The high phosphorous (more than 10 % P) coatings
Because the deposited nickel alloy is a catalyst for the reaction, have superior salt-spray and acid resistance in a wide range of
the process is self-sustaining. The chemical and physical applications. They are used on beryllium and titanium parts for
properties of the deposit vary primarily with its phosphorus low stress properties. Coatings with phosphorus contents
content and subsequent heat treatment. The chemical makeup greater than 11.2 % P are not considered to be ferromagnetic.
of the plating solution and the use of the solution can affect the 1.10 The values stated in SI units are to be regarded as
porosity and corrosion resistance of the deposit. For more standard.
details, see ASTM STP 265 (1)2 and Refs (2) (3) (4) and (5).
1.11 The following precautionary statement pertains only to
1.3 The coatings are generally deposited from acidic solu- the test method portion, Section 9, of this specification. This
tions operating at elevated temperatures. standard does not purport to address all of the safety concerns,
1.4 The process produces coatings of uniform thickness on if any, associated with its use. It is the responsibility of the user
irregularly shaped parts, provided the plating solution circu- of this standard to establish appropriate safety and health
lates freely over their surfaces. practices and determine the applicability of regulatory limita-
tions prior to use.
1.5 The coatings have multifunctional properties, such as
hardness, heat hardenability, abrasion, wear and corrosion 2. Referenced Documents
resistance, magnetics, electrical conductivity provide diffusion
2.1 ASTM Standards:3
barrier, and solderability. They are also used for the salvage of
B368 Test Method for Copper-Accelerated Acetic Acid-Salt
worn or mismachined parts.
Spray (Fog) Testing (CASS Test)
1.6 The low phosphorus (2 to 4 % P) coatings are microc- B374 Terminology Relating to Electroplating
rystalline and possess high as-plated hardness (620 to 750 HK B380 Test Method for Corrosion Testing of Decorative
100). These coatings are used in applications requiring abra- Electrodeposited Coatings by the Corrodkote Procedure
sion and wear resistance. B487 Test Method for Measurement of Metal and Oxide
1.7 Lower phosphorus deposits in the range between 1 and Coating Thickness by Microscopical Examination of
3 % phosphorus are also microcrystalline. These coatings are Cross Section
used in electronic applications providing solderability, B499 Test Method for Measurement of Coating Thicknesses
by the Magnetic Method: Nonmagnetic Coatings on
Magnetic Basis Metals
1
B504 Test Method for Measurement of Thickness of Metal-
This specification is under the jurisdiction of ASTM Committee B08 on
lic Coatings by the Coulometric Method
Metallic and Inorganic Coatings and is the direct responsibility of Subcommittee
B08.03 on Engineering Coatings.
Current edition approved Nov. 1, 2015. Published November 2015. Originally
3
approved in 1984. Last previous edition approved in 2014 as B733 – 09(2014). DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/B0733-15. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers given in parentheses refer to a list of references at the Standards volume information, refer to the standard’s Document Summary page on
end of the text. the ASTM website.

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 B733 − 15
B537 Practice for Rating of Electroplated Panels Subjected G85 Practice for Modified Salt Spray (Fog) Testing
to Atmospheric Exposure 2.2 Military Standards:
B567 Test Method for Measurement of Coating Thickness MIL-R-81841 Rotary Flap Peening of Metal Parts5
by the Beta Backscatter Method MIL-S-13165 Shot Peening of Metal Parts5
B568 Test Method for Measurement of Coating Thickness MIL-STD-105 Sampling Procedures and Tables for Inspec-
by X-Ray Spectrometry tion by Attribute5
B571 Practice for Qualitative Adhesion Testing of Metallic
2.3 ISO Standards:
Coatings
ISO 4527 Autocatalytic Nickel-Phosphorus Coatings—
B578 Test Method for Microhardness of Electroplated Coat-
Specification and Test Methods6
ings
B602 Test Method for Attribute Sampling of Metallic and 3. Terminology
Inorganic Coatings
B667 Practice for Construction and Use of a Probe for 3.1 Definitions:
Measuring Electrical Contact Resistance 3.1.1 significant surfaces—those substrate surfaces which
B678 Test Method for Solderability of Metallic-Coated the coating must protect from corrosion or wear, or both, and
Products that are essential to the performance.
B697 Guide for Selection of Sampling Plans for Inspection 3.2 Other Definitions—Terminology B374 defines most of
of Electrodeposited Metallic and Inorganic Coatings the technical terms used in this specification.
B762 Test Method of Variables Sampling of Metallic and
Inorganic Coatings 4. Coating Classification
B849 Specification for Pre-Treatments of Iron or Steel for 4.1 The coating classification system provides for a scheme
Reducing Risk of Hydrogen Embrittlement to select an electroless nickel coating to meet specific perfor-
B850 Guide for Post-Coating Treatments of Steel for Reduc- mance requirements based on alloy composition, thickness and
ing the Risk of Hydrogen Embrittlement hardness.
B851 Specification for Automated Controlled Shot Peening 4.1.1 TYPE describes the general composition of the de-
of Metallic Articles Prior to Nickel, Autocatalytic Nickel, posit with respect to the phosphorus content and is divided into
or Chromium Plating, or as Final Finish five categories which establish deposit properties (see Table 1).
D1193 Specification for Reagent Water
D2670 Test Method for Measuring Wear Properties of Fluid NOTE 1—Due to the precision of some phosphorus analysis methods a
deviation of 0.5 % has been designed into this classification scheme.
Lubricants (Falex Pin and Vee Block Method) Rounding of the test results due to the precision of the limits provides for
D2714 Test Method for Calibration and Operation of the an effective limit of 4.5 and 9.5 % respectively. For example, coating with
Falex Block-on-Ring Friction and Wear Testing Machine a test result for phosphorus of 9.7 % would have a classification of TYPE
D3951 Practice for Commercial Packaging V, see Appendix X5, Alloy TYPEs.
D4060 Test Method for Abrasion Resistance of Organic 4.2 Service Condition Based on Thickness:
Coatings by the Taber Abraser 4.2.1 Service condition numbers are based on the severity of
E60 Practice for Analysis of Metals, Ores, and Related the exposure in which the coating is intended to perform and
Materials by Spectrophotometry minimum coating thickness to provide satisfactory perfor-
E140 Hardness Conversion Tables for Metals Relationship mance (see Table 2).
Among Brinell Hardness, Vickers Hardness, Rockwell 4.2.2 SC0 Minimum Service, 0.1 µm—This is defined by a
Hardness, Superficial Hardness, Knoop Hardness, Sclero- minimum coating thickness to provide specific material prop-
scope Hardness, and Leeb Hardness erties and extend the life of a part or its function. Applications
E156 Test Method for Determination of Phosphorus in include requirements for diffusion barrier, undercoat, electrical
High-Phosphorus Brazing Alloys (Photometric Method) conductivity and wear and corrosion protection in specialized
(Withdrawn 1993)4 environments.
E352 Test Methods for Chemical Analysis of Tool Steels and
Other Similar Medium- and High-Alloy Steels
F519 Test Method for Mechanical Hydrogen Embrittlement
Evaluation of Plating/Coating Processes and Service En- 5
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
vironments Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
G5 Reference Test Method for Making Potentiodynamic 6
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Anodic Polarization Measurements 4th Floor, New York, NY 10036, http://www.ansi.org.
G31 Guide for Laboratory Immersion Corrosion Testing of
Metals TABLE 1 Deposit Alloy Types
G59 Test Method for Conducting Potentiodynamic Polariza- Type Phosphorus % wt
tion Resistance Measurements I No Requirement for Phosphorus
II 1 to 3
III 2 to 4
IV 5 to 9
4
The last approved version of this historical standard is referenced on V 10 and above
www.astm.org.

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 B733 − 15
TABLE 2 Service Conditions 4.3.4 Class 4—Heat treatment at 120 to 130°C for at least 1
Coating Thickness Requirements h to increase adhesion of heat-treatable (age-hardened) alumi-
Minimum Coating num alloys and carburized steel (see Note 3).
Service Condition Thickness µm in.
Specification 4.3.5 Class 5—Heat treatment at 140 to 150°C for at least 1
SC0 Minimum Thickness 0.1 0.000004
h to improve coating adhesion for aluminum, non age-
SC1 Light Service 5 0.0002 hardened aluminum alloys, copper, copper alloys and beryl-
SC2 Mild Service 13 0.0005 lium.
SC3 Moderate Service 25 0.001
SC4 Severe Service 75 0.003 4.3.6 Class 6—Heat treatment at 300 to 320°C for at least 1
h to improve coating adhesion for titanium alloys.
NOTE 3—Heat-treatable aluminum alloys such as Type 7075 can
4.2.3 SC1 Light Service, 5 µm—This is defined by a undergo microstructural changes and lose strength when heated to over
130°C.
minimum coating thickness of 5 µm for extending the life of
the part. Typical environments include light-load lubricated
5. Ordering Information
wear, indoor corrosion protection to prevent rusting, and for
soldering and mild abrasive wear. 5.1 The following information shall be supplied by the
4.2.4 SC2 Mild Service, 13 µm—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 part to be plated:
trial atmosphere exposure on steel substrates in dry or oiled 5.1.1 Title, ASTM designation number, and year of issue of
environments. this specification.
4.2.5 SC3 Moderate Service, 25 µm—This is defined by 5.1.2 Classification of the deposit by type, service
moderate environments such as non marine outdoor exposure, condition, class, (see 4.1, 4.2 and 4.3).
alkali salts at elevated temperature, and moderate wear. 5.1.3 Specify maximum dimension and tolerance
4.2.6 SC4 Severe Service, 75 µm—This is defined by a very requirements, if any.
aggressive environment. Typical environments would include 5.1.4 Peening, if required (see 6.5).
acid solutions, elevated temperature and pressure, hydrogen 5.1.5 The tensile strength of the material in MPa (see 6.3.1
sulfide and carbon dioxide oil service, high-temperature chlo- and 6.6).
ride systems, very severe wear, and marine immersion. 5.1.6 Stress relief heat treatment before plating, (see 6.3).
5.1.7 Hydrogen Embrittlement Relief after plating, (see
NOTE 2—The performance of the autocatalytic nickel coating depends 6.6).
to a large extent on the surface finish of the article to be plated and how
it was pretreated. Rough, non uniform surfaces require thicker coatings 5.1.8 Significant surfaces and surfaces not to be plated must
than smooth surfaces to achieve maximum corrosion resistance and be indicated on drawings or sample.
minimum porosity. 5.1.9 Supplemental or Special Government Requirements
4.3 Post Heat Treatment Class—The nickel-phosphorus such as, specific phosphorus content, abrasion wear or corro-
coatings shall be classified by heat treatment after plating to sion resistance of the coating, solderability, contact resistance
increase coating adhesion and or hardness (see Table 3). and packaging selected from Supplemental Requirements.
4.3.1 Class 1—As-deposited, no heat treatment. 5.1.10 Requirement for a vacuum, inert or reducing atmo-
4.3.2 Class 2—Heat treatment at 260 to 400°C to produce a sphere for heat treatment above 260°C to prevent surface
minimum hardness of 850 HK100. oxidation of the coating (see S3).
4.3.3 Class 3—Heat treatment at 180 to 200°C for 2 to 4 h 5.1.11 Test methods for coating adhesion, composition,
to improve coating adhesion on steel and to provide for thickness, porosity, wear and corrosion resistance, if required,
hydrogen embrittlement relief (see section 6.6). selected from those found in Section 9 and Supplemental
Requirements.
5.1.12 Requirements for sampling (see Section 8).
TABLE 3 Classification of Post Heat Treatment
Temperature NOTE 4—The purchaser should furnish separate test specimens or
CLASS Description Time (h) coupons of the basis metal for test purposes to be plated concurrently with
(°C)
the articles to be plated (see 8.4).
1 No Heat Treatment, As Plated
2 Heat Treatment for Maximum Hardness
TYPE I 260 20 6. Materials and Manufacture
285 16
320 8 6.1 Substrate—Defects in the surface of the basis metal such
400 1 as scratches, porosity, pits, inclusions, roll and die marks, laps,
TYPE II 350 to 380 1
TYPE III 360 to 390 1 cracks, burrs, cold shuts, and roughness may adversely affect
TYPE IV 365 to 400 1 the appearance and performance of the deposit, despite the
TYPE V 375 to 400 1 observance of the best plating practice. Any such defects on
3 Adhesion on Steel 180 to 200 2 to 4
4 Adhesion, Carburized Steel and 120 to 130 1 to 6 significant surfaces shall be brought to the attention of the
Age Hardened Aluminum purchaser before plating. The producer shall not be responsible
5 Adhesion on Beryllium and 140 to 150 1 to 2 for coatings defects resulting from surface conditions of the
Aluminum
6 Adhesion on Titanium 300–320 1–4 metal, if these conditions have been brought to the attention of
the purchaser.

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 B733 − 15
6.2 Pretreatment—A suitable method shall activate the sur- purchaser. Guide B850 contains a list of post treatments,
face and remove oxide and foreign materials, which may cause procedures, limitations, and guidelines that are permitted to be
poor adhesion and coating porosity. used to reduce the effects of hydrogen embrittlement.
NOTE 5—Heat treatment of the base material may effect its metallur-
6.6.1 Heat treatment shall be performed preferably within 1
gical properties. An example is leaded steel which may exhibit liquid or h but not more than 3 h of plating unless the size or weight of
solid embrittlement after heat treatment. Careful selection of the pre and the part prevents the initiation of heart treatment within 3 h. In
post heat treatments are recommended. this case, the part shall be heat treated as soon as possible. In
6.3 Stress Relief: all cases, the duration of the heat treatment shall commence
6.3.1 Pretreatment of Iron and Steel for Reducing the Risk of from the time at which the whole of each part attains the
Hydrogen Embrittlement—Parts that are made of steel with specified temperature.
ultimate tensile strength of greater than 1000 MPa (hardness of 6.7 Heat Treatment After Plating to Improve Adhesion—To
31 HRC), that have been machined, ground, cold formed, or improve the adhesion of the coating to various substrates, the
cold straightened subsequent to heat treatment require stress heat treatments in Table 3 should be performed as soon as
relief heat treatment when specified by the purchaser. The practical after plating (see 4.3).
tensile strength of the material shall be supplied by the
purchaser. Specification B849 contains a list of pre-treatments, 6.8 Heat Treatment After Plating to Increase Hardness:
precautions, procedures, and caveats that shall be used. 6.8.1 To increase the hardness of the coating a heat treat-
6.3.2 Peening—Peening prior to plating may be required on ment of over 260°C is required. Table 3 describes the heat
high-strength steel parts to induce residual compressive treatment for maximum hardness.
stresses in the surface, which can reduce loss of fatigue 6.8.2 See Appendix X3 and Appendix X5.
strength and improve stress corrosion resistance after plating. 6.8.3 A heat treatment at 260°C for greater than 20 h should
(See Supplementary Requirements). be used to reduce the loss of surface hardness and strength of
6.3.3 Steel parts which are designed for unlimited life under some ferrous basis metals. Avoid rapid heating and cooling of
dynamic loads shall be shot peened or rotary flap peened. plated parts. Sufficient time must be allowed for large parts to
reach oven temperature.
NOTE 6—Controlled shot peening is the preferred method because there
are geometry’s where rotary flap peening is not effective. See S11.2. NOTE 7—The length of time to reach maximum hardness varies with the
6.3.3.1 Unless otherwise specified, the shot peening shall be phosphorus content of the deposit. High phosphorus deposits may require
longer time or a higher temperature, or both. Individual alloys should be
accomplished on all surfaces for which the coating is required tested for maximum hardness attainable, especially for conditions of lower
and all immediate adjacent surfaces when they contain notches, temperatures and longer times.
fillets, or other abrupt changes of section size where stresses NOTE 8—Inert or reducing atmosphere or vacuum sufficient to prevent
will be concentrated. oxidation is recommended for heat treatment above 260°C. Do not use gas
containing hydrogen with high-strength steel parts.
6.4 Racking—Parts should be positioned so as to minimize
trapping of hydrogen gas in cavities and holes, allowing free 7. Requirements
circulation of solution over all surfaces to obtain uniform
coating thickness. The location of rack or wire marks in the 7.1 Process—The coating shall be produced from an aque-
coating shall be agreed upon between the producer and ous solution through chemical reduction reaction.
purchaser. 7.2 Acceptance Requirements—These requirements are
6.5 Plating Process: placed on each lot or batch and can be evaluated by testing the
6.5.1 To obtain consistent coating properties, the bath must plated part.
be monitored periodically for pH, temperature, nickel and 7.2.1 Appearance:
hypophosphite. Replenishments to the plating solution should 7.2.1.1 The coating surface shall have a uniform, metallic
be as frequent as required to maintain the concentration of the appearance without visible defects such as blisters, pits,
nickel and hypophosphite between 90 and 100 % of set point. pimples, and cracks (see 9.2).
The use of a statistical regimen to establish the control limits 7.2.1.2 Imperfections that arise from surface conditions of
and frequency of analysis may be employed to ensure quality the substrate which the producer is unable to remove using
deposits are produced. conventional pretreatment techniques and that persist in the
6.5.2 Mechanical movement of parts, agitation of the bath, coating shall not be cause for rejection (see 6.1). Also,
and filtration is recommended to increase coating smoothness discoloration due to heat treatment shall not be cause for
and uniformity and prevent pitting or streaking due to hydro- rejection unless special heat treatment atmosphere is specified
gen bubbles. (see 5.1.10).
6.6 Post Coating Treatment for Iron and Steel for Reducing 7.2.2 Thickness—The thickness of the coating shall exceed
the Risk of Hydrogen Embrittlement—Parts that are made of the minimum requirements in Table 2 as specified by the
steel with ultimate tensile strengths of 1000 MPa (correspond- service condition agreed to prior to plating (see 9.3). After
ing hardness values 300 HV10, 303 HB, or 31 HRC or greater), coating and if specified, the part shall not exceed maximum
as well as surface hardened parts, shall require post coating dimension on significant surface (see 5.1.3).
hydrogen embrittlement relief baking when specified by the NOTE 9—The thickness of the coating cannot be controlled in blind or
purchaser. The tensile strength shall be supplied by the small diameter deep holes or where solution circulation is restricted.

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 B733 − 15
7.2.3 Adhesion—The coating shall have sufficient adhesion agree on the plan(s) to be used. If they do not, Test Method B762 identifies
to the basis metal to pass the specified adhesion test (see 9.4 the plan to be used.
An inspection lot shall be defined as a collection of coated parts which
and Practice B571). are of the same kind, that have been produced to the same specification,
7.2.4 Porosity—The coatings shall be essentially pore free that have been coated by a single producer at one time or approximately
when tested according to one of the methods of 9.6. The test the same time under essentially identical conditions, and that are submit-
method, the duration of the test, and number of allowable spots ted for acceptance or rejection as a group.
per unit area shall be specified (see 5.1.11 and 9.6). 8.3 All specimens used in the sampling plan for acceptance
tests shall be made of the same basis material and in the same
7.3 Qualification Requirements—These requirements are
metallurgical condition as articles being plated to this specifi-
placed on the deposit and process and are performed on
cation.
specimens to qualify the deposit and plating process. The tests
for these qualification requirements shall be performed 8.4 All specimens shall be provided by the purchaser unless
monthly or more frequently. otherwise agreed to by the producer.
7.3.1 Composition—Type II, III, IV, V deposits shall be NOTE 11—The autocatalytic nickel process is dynamic and a daily
analyzed for alloy composition by testing for phosphorus (see sampling is recommended. For coatings requiring alloy analysis and
9.1). The weight percent of phosphorus shall be in the range corrosion testing weekly sampling should be considered as an option.
designated by type classification (see 4.1). 9. Test Methods
7.3.2 Microhardness—The microhardness of Class 2 depos- 9.1 Deposit Analysis for Phosphorus:
its shall be determined by Test Method B578 (Knoop). For 9.1.1 Phosphorus Determination—Determine mass % phos-
Class 2 coatings, the microhardness shall equal or exceed a phorus content according to Practice E60, Test Methods E352,
minimum of 850 (HK100 (or equivalent Vickers) (see 4.3 and or Test Method E156 on known weight of deposit dissolved in
9.5). The conversion of Vickers to Knoop using Tables E140 is warm concentrated nitric acid.
not recommended. 9.1.2 Composition can be determined by atomic absorption,
7.3.3 Hydrogen Embrittlement—The process used to deposit emission or X-ray fluorescence spectrometry.
a coating onto high strength steels shall be evaluated for
NOTE 12—Inductively coupled plasma techniques can determine the
hydrogen embrittlement by Test Method F519. alloy to within 0.1 %. The following analysis wavelength lines have been
used with minimum interference to determine the alloy.
8. Sampling Ni 216.10 nm Cd 214.44 nm Fe 238.20 nm
P 215.40 nm Co 238.34 nm Pb 283.30 nm
8.1 The purchaser and producer are urged to employ statis- P 213.62 nm Cr 284.32 nm Sn 198.94 nm
tical process control in the coating process. Properly performed Al 202.55 nm Cu 324.75 nm Zn 206.20 nm
this will ensure coated products of satisfactory quality and will 9.2 Appearance—Examine the coating visually for compli-
reduce the amount of acceptance inspection. ance with the requirements of 7.2.1.
8.1.1 Sampling plans can only screen out unsatisfactory 9.3 Thickness:
products without assurance that none of them will be accepted.
(6) NOTE 13—Eddy-current type instruments give erratic measurements
due to variations in conductivity of the coatings with changes in
8.2 The sampling plan used for the inspection of a quantity phosphorus content.
of coated parts (lot) shall be Test Method B602 unless 9.3.1 Microscopical Method—Measure the coating thick-
otherwise specified by purchaser in the purchase order or ness of a cross section according to Test Method B487.
contract (see 5.1.12 and S.11.1).
NOTE 14—To protect the edges, electroplate the specimens with a
NOTE 10—Usually, when a collection of coated parts (the inspection lot minimum of 5 µm of nickel or copper prior to cross sectioning.
8.2) is examined for compliance with the requirements placed on the parts 9.3.2 Magnetic Induction Instrument Method—Test Method
a relatively small number of parts, the sample, is selected at random and B499 is applicable to magnetic substrates plated with autocata-
inspected. The inspection lot is then classified as complying or not
complying with the requirements based on the results of the inspection lytic nickel deposits, that contain more than 11 mass %
sample. The size of the sample and the criteria of compliance are phosphorus (not ferromagnetic) and that have not been heat-
determined by the application of statistics. The procedure is known as treated. The instrument shall be calibrated with deposits plated
sampling inspection. Three standards Test Method B602, Guide B697, and in the same solution under the same conditions on magnetic
Test Method B762 contain sampling plans that are designed for the
steel.
sampling inspection of coatings.
Test Method B602 contains four sampling plans, three for use with tests 9.3.3 Beta Backscatter Method—Test Method B567 is only
that are nondestructive and one for use with tests that are destructive. The applicable to coatings on aluminum, beryllium, magnesium,
purchaser and producer may agree on the plan(s) to be used. If they do not, and titanium. The instrument must be calibrated with standards
Test Method B602 identifies the plan to be used. having the same composition as the coating.
Guide B697 provides a large number of plans and also gives guidance
on the selection of a plan. When Guide B697 is specified, the purchaser NOTE 15—The density of the coating varies with its mass % phosphorus
and producer need to agree on the plan to be used. content (See Appendix X2).
Test Method B762 can be used only for coating requirements that have 9.3.4 Micrometer Method—Measure the part, test coupon,
a numerical limit, such as coating thickness. The last must yield a
numerical value and certain statistical requirements must be met. Test or pin in a specific spot before and after plating using a suitable
Method B762 contains several plans and also gives instructions for micrometer. Make sure that the surfaces measured are smooth,
calculating plans to meet special needs. The purchaser and producer may clean, and dry.

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 B733 − 15
9.3.5 Weigh, Plate, Weigh Method—Using a similar sub- maximum accuracy, a minimum coating thickness of 75 µm is
strate material of known surface area, weigh to the nearest recommended. Conversions of Vickers or Knoop hardness
milligram before and after plating making sure that the part or number to Rockwell C is not recommended.
coupon is dry and at room temperature for each measurement.
Calculate the thickness from the increase in weight, specific NOTE 18—On thick (75 µm+) coatings on steel a surface microhardness
determination is permissible.
gravity, and area as follows:
coating thickness, µm 5 10 W/ ~ A 3 D ! (1)
9.6 Porosity—There is no universally accepted test for
porosity. When required, one of the following tests can be used
where: on the plated part or specimen.
W = weight gain in milligrams, 9.6.1 Ferroxyl Test for Iron Base Substrates—Prepare the
A = total surface area in square centimetres, and test solution by dissolving 25 g of potassium ferricyanide and
D = grams per cubic centimetres (see Appendix X2). 15 g of sodium chloride in 1 L of distilled water. After
9.3.6 Coulometric Method—Measure the coating thickness cleaning, immerse the part for 30 s in the test solution at 25°C.
in accordance with Test Method B504. The solution to be used After rinsing and air drying, examine the part for blue spots,
shall be in accordance with manufacturer’s recommendations. which form at pore sites.
The surface of the coating shall be cleaned prior to testing (see 9.6.2 Boiling Water Test for Iron-Base Substrates—
Note 14). Completely immerse the part to be treated in a vessel filled
9.3.6.1 Calibrate standard thickness specimens with depos- with aerated water at room temperature. Apply heat to the
its plated in the same solution under the same conditions. beaker at such a rate that the water begins to boil in not less
9.3.7 X-Ray Spectrometry—Measure the coating thickness than 15 min, nor more than 20 min after the initial application
in accordance with Test Method B568. The instrument must be of heat. Continue to boil the water for 30 min. Then remove the
calibrated with standards having the same composition as the part, air dry, and examine for rust spots, which indicate pores.
coating.
NOTE 19—Aerated water is prepared by bubbling clean compressed air
NOTE 16—This method is only recommended for deposits in the through distilled water by means of a glass diffusion disk at room
as-plated condition. The phosphorus content of the coating must be known temperature for 12 h. The pH of the aerated water should be 6.7 + 0.5.
to calculate the thickness of the deposit. Matrix effect due to the
distribution of phosphorus in layers of the coating also effect the 9.6.3 Aerated Water Test for Iron-Base Substrates—
measurement accuracy and require that calibration standards be made Immerse the part for 4 h in vigorously aerated Type IV or better
under the same conditions as the production process. water (see Specification D1193) at 25 6 2°C temperature and
9.4 Adhesion: then examine the part for rust spots.
9.4.1 Bend Test (Practice B571)—A sample specimen is 9.6.4 Alizarin Test for Aluminum Alloys—Wipe the plated
bent 180° over a mandrel diameter 4× the thickness (10 mm part or specimen with 10 mass % sodium hydroxide solution.
minimum) of the specimen and examined at 4× power magni- After 3 min contact, rinse, and apply a solution of alizarin
fication for flaking or separation at the interface. Fine cracks in sulfonate prepared by dissolving 1.5 g of methyl cellulose in 90
the coating on the tension side of the bend are not an indication mL of boiling water to which, after cooling, 0.1 g sodium
of poor adhesion. Insertion of a sharp probe at the interface of alizarin sulfonate, dissolved in 5 mL of ethanol is added. After
the coating and basis metal to determine the adhesion is 4 min contact, apply glacial acetic acid until the violet color
suggested. disappears. Any red spots remaining indicate pores.
9.6.5 Porosity Test for Copper Substrates—Wipe the plated
NOTE 17—Appropriate test specimens are strips approximately 25 to 50
mm wide, 200 to 300 mm long and 3 to 6 mm thick. part or specimen with glacial acetic acid. After 3 min, apply a
solution of potassium ferrocyanide prepared by dissolving 1 g
9.4.2 Impact Test—A spring-loaded center punch with a of potassium ferrocyanide and 1.5 g methyl cellulose in 90 mL
point having 2 to 3 mm radius is used to test adhesion of the of boiling distilled water. The appearance of brown spots after
coating on nonsignificant surfaces of the plated part. Make 2 min indicate pores.
three closely spaced indentations and examine under 10×
magnification for flaking or blistering of the coating, which is 9.7 Other Test Methods—Test methods which have been
cause for rejection. developed that are equal to or better than these may be
9.4.3 Thermal Shock—The coated part is heated to 200°C in substituted. The precision and bias requirements will vary for
an oven and then quenched in room temperature water. The each type of test. If an alternate test is specified it shall be
coating is examined for blistering or other evidence of poor agreed upon between the producer and the purchaser.
adhesion at 4× magnification.
10. Rejection and Rehearing
9.5 Microhardness—The microhardness of the coating can
be measured by Test Method B578 using Knoop indenter and 10.1 Part(s) that fail to conform to the requirements of this
is reported in Knoop Hardness Number (HK). It will vary standard may be rejected. Rejection shall be reported to the
depending on loads, type of indenter, and operator. A100 g load producer promptly in writing. In the case of dissatisfaction
is recommended. The rhombic Knoop indenter gives higher occurs with the results of a test, the producer may make a claim
hardness readings than the square-base pyramidal Vickers for a hearing. Coatings that show imperfections may be
diamond indenter for 100 to 300 g loads, see Ref (7). For rejected.

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 B733 − 15
11. Certification 12. Keywords
11.1 When specified in the purchase order or contract, the 12.1 autocatalytic; chemical nickel; coatings; conductive;
purchaser shall be furnished certification that the samples corrosion resistance; electroless; functional; nickel; nickel
representing each lot have been processed, tested and inspected phosphorus; wear resistance
as directed in this specification and the requirements have been
met. When specified in the purchase order or contract, a report
of the test results shall be furnished.

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 S1.7 Contact Resistance—When specified by the purchaser
ordering information, the part(s) shall be shot peened prior to in the ordering information, the coating shall be tested for
plating in accordance with Specification B851 or MIL-S- contact resistance using Practice B667.
13165. S1.8 Solderability—When specified by the purchaser in the
S1.2 Composition—When specified by the purchaser in the ordering information, the unaged coating shall pass Test
ordering information the phosphorus content shall be main- Method B678 on solderability.
tained in the deposit to within 1 %. Use the test methods S1.9 Corrosion Resistance—When specified by the pur-
described in 9.1. chaser in the ordering information the coating shall pass any
S1.3 Inert Atmosphere—When specified by the purchaser in special corrosion tests agreed to by the producer. The corrosion
the ordering information, the coating shall be heat treated in a resistance of the coating to a specific liquid medium can be
vacuum, inert, or reducing atmosphere to prevent surface determined by means of immersion tests (see Practice G31) or
oxidation of the coating. electrochemical test (see Test Method G5 and Practice G59).
S1.4 Hydrogen Embrittlement—When specified by the pur- S1.10 Pitting Corrosion Resistance—Use Practice G85
chaser in the ordering information the plating process shall be (acetic acid-salt spray test), Test Method B368 (copper-
evaluated at the time of processing parts for hydrogen em- accelerated acetic acid-salt spray, CASS), or Test Method B380
brittlement using Test Method F519. (Corrodkote) to evaluate the corrosion resistance of the coating
S1.5 Abrasive Wear—When specified by the purchaser in to pitting.
the ordering information, the coating shall be tested for
S1.11 Special Government Requirements:
abrasion wear resistance using the method in Appendix X1 of
this specification. The coating shall meet a maximum wear rate S1.11.1 Sampling—Part(s) plated for the US Government
which is specified by the purchaser and agreed to by the and Military use shall use MIL-STD-105 as the sampling plan.
producer. S1.11.2 Shot Peening—High strength steel part(s) pro-
S1.6 Adhesive Wear—When specified by the purchaser in cessed for US Government and Military use shall be shot
the ordering information, the coating shall be tested for peened in accordance with MIL-S-13165 or rotary flap peened
adhesive wear resistance using Test Method D2714 or Test in accordance with MIL-R-81841. (see Note 6).
Method D2670. The wear rate shall be specified by the S1.11.3 Packaging—Parts shall be packaged in accordance
purchaser and agreed to by the producer. with Practice D3951.

APPENDIXES

(Nonmandatory Information)

X1. TABER ABRASER WEAR TEST METHOD

X1.1. Scope NOTE X1.1—Variation in results have been attributed to calibration of

the instrument, the humidity in the laboratory, and the storage conditions
X1.1.1 This test method will evaluate the resistance of the of the CS-10 wheels.
coating to abrasive wear. The test is performed by rotating a X1.1.2 The results may be variable between tests and
plated panel under weighted abrasive wheels. Abrasion resis- therefore three plated test specimens should be tested to 6000
tance is calculated as loss in weight by weighing the panel after cycles each. The results should be averaged without the first
each 1000 cycles. Duration of the test is 6000 cycles and it can 1000 cycles and the abrasion wear resistance is reported as the
be extended to 25 000 cycles for more complete results. weight loss in mg/1000 cycles (Taber Wear Index).

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 B733 − 15
X1.2. Apparatus X1.4.2 Prepare the Taber Abraser such that a load of 1000 g
X1.2.1 Taber Abraser Wear Testing Unit—As described in (per wheel) is used. Adjust the vacuum nozzle gap to 3 61 mm
Test Method D4060, the unit must be capable of loading each above the specimen surface. Set the vacuum suction force to
wheel with 1000 g load and operating with a vacuum. 100.
X1.2.2 Abrasion Wheels7—Use CS-10 (resilient rubber) X1.4.3 Subject each of the three specimens to abrasion
Taber wheels. The wheels shall be 12.7 6 0.3 mm thick and using the following steps:
have an external diameter of 51.9 6 0.5 mm when new, and in X1.4.3.1 Run the CS-10 wheels on the coating for 1000
no case less than 44.4 mm. The hardness of CS-10 wheels can cycles to remove any surface roughness.
change with time and can affect the reproducibility of results X1.4.3.2 Weigh the specimen to the nearest 0.1 mg.
(see Test Method D4060). Wheels should not be used after the X1.4.3.3 Resurface the CS-10 wheels with a new S-11
date marked on them. refacing disc for 50 cycles.
X1.4.3.4 Abrasion test the coating with 1000 g load for
X1.2.3 Refacing Medium—Taber S-11 abrasive disc, used 1000 cycles.
for resurfacing the CS-10 wheels. X1.4.3.5 Repeat X1.4.3.2, X1.4.3.3 and X1.4.3.4 until a
X1.2.4 Test Specimens—Test specimens shall be made from total of 6000 cycles, or more if desired, have been accom-
20 gage CR steel 4 by 4 in. (100 by 100 by 1.3 mm) with a plished for each specimen.
0.250 (6.35 mm) hole in the center. Test panels must have both X1.5 Calculation
surfaces substantially plane and parallel, and are available from
Taber. X1.5.1 Wear Index—Compute the wear index, I, of a test
specimen as follows:
X1.2.5 Analytical Balance—Scale which is capable of mea-
suring to 150 g 6 0.1 mg. ~ A 2 B ! 1000
I5 (X1.1)
C
X1.3. Conditioning where:
X1.3.1 Condition the plated panel under settings of humid- A = weight of test specimen before abrasion, mg,
ity and temperature as agreed upon between the interested B = weight of test specimen after abrasion, mg, and
parties. If no settings are specified, condition the coated panel C = number of cycles of abrasion recorded.
for at least 24 h at 23 6 2°C and 50 6 5 % relative humidity. X1.5.2 Weight Loss—Compute weight loss, L, of the test
Conduct the test in the same environment or immediately on specimen as follows:
removal therefrom.
L5A2B (X1.2)
X1.4. Procedure where:
X1.4.1 Plate three specimens with 0.001 in. (25 µm) of A = weight of test specimen before abrasion, mg, and
nickel phosphorus coating. B = weight of test specimen after abrasion, mg.
X1.6. Reporting
7
The sole source of supply known to the committee at this time is Taber X1.6.1 Determine the average weight loss in milligrams for
Industries, North Tonawanda, NY. If you are aware of alternative suppliers, please
provide this information to ASTM International Headquarters. Your comments will
each specimen per 1000 cycles Taber Wear Index and the mean
receive careful consideration at a meeting of the responsible technical committee, weight loss per 1000 cycles for all specimens. Report the mean
which you may attend. and standard deviation for the coating.

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 B733 − 15

X2. DENSITY OF AUTOCATALYTIC NICKEL DEPOSITS

FIG. X2.1 Density of Autocatalytic Nickel Phosphorus Alloy Summary of Reported Values

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 B733 − 15

X3. HARDNESS VERSUS 1 H HEAT TREATMENT

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

X3.1 This graph information on the relationship of hardness X3.2 The ultimate hardness of the deposit is dependent on
and heat treatment for 1 h for different phases which approxi- the time and temperature of heat treatment as well as the
mate the TYPEs. Deposits that are low in phosphorus (β) are phosphorus content, age of the solution, concentration of
harder as plated and will transition between 200 and 400°C, hypophosphite, and type of additive system used. Type I and
producing a mixture of fcc Ni and Ni3P. Deposits that are high IV deposits are subject to greater structural variation and their
in phosphorus (γ) are softer in the as plated condition and will properties are less predictable.
also transition between 275 and 350°C, producing a mixture of
fcc Ni and Ni3P. Deposits in the range of 4 to 8 % are a mixture X3.3 Fig. X3.1 and Appendix X4 can be used to approxi-
of both β and γ and have properties that are less predictable mate the hardness after heat treatment.
after heat treatment.

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 B733 − 15

X4. HARDNESS VERSUS TIME AND TEMPERATURE

NOTE 1—These graphs are average and may vary with deviations from normal practice.
FIG. X4.1 Hardness and Annealing Time Versus Temperature
9 % Phosphorus Deposit

X4.1 Fig. X4.1 provides information on the effect of anneal- tation hardening at 200°C. Deposits higher than 7.5 % will be
ing time on the precipitation of nickel and 9 % phosphorus to stronger and when the deposit reaches around 11.2 % will be
Ni3P and fcc Ni. Alloys of other phosphorus contents have saturated with phosphorus. The precipitation of these high
differing hardness versus time and temperature. Deposits that phosphorus deposits may be delayed for several minutes in the
are less than 7.5 % will have lower strength and start precipi- mid-range temperatures.

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 B733 − 15

X5. ALLOY TYPES

FIG. X5.1 Selected Properties of As Plated Autocatalytic Nickel Phosphorus Coatings by Phosphorus Content

NOTE X5.1—These different alloy TYPEs are produced from processes point. These differences are produced by micro structural
which are specifically formulated and controlled. Additional requirements differences between Ni + Ni3P and Ni3P. These differences
for internal stress, purity, and elongation may be necessary for some
applications. also effect non-destructive thickness testing by X-Ray and
magnetic means. Careful attention to the selection of TYPE
X5.1 The physical differences of these TYPEs provide for a will insure optimum performance of the deposit in the intended
wide variation in performance in wire bonding, contact application.
resistance, machineability, lubricity, reactivation and melting

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 B733 − 15

X6. SUMMARY PROGRAM 14

TABLE X6.1 Results of 110 Month Exposure of Autocatalytic (Electroless) Nickel Deposits at Kure Beach, North CarolinaA
Phosphorus Alloy % wt Practice
Heat Thickness, Thickness,
Deposit Type Source Lot Surface B537 Ratings
Treatment µm Target µm Actual ICP EDAX 110 Months
1 Smooth No 12.5 3.6 ± 3.0
2 Smooth No 25 9.2 ± 0.3
V G 3 Smooth No 75 80.5 10.5 10.9 10 ± 0
4 Smooth Yes 25 9.2 ± 0.3
5 Ground No 25 7.8 ± 0.4
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 8.0 ± 0
V E 3 Smooth No 75 77 10.0 10.2 9.8 ± 0.4
4 Smooth Yes 25 8.2 ± 0.8
5 Ground No 25 4.2 ± 0.4
1 Smooth No 12.5 6.8 ± 1.3
2 Smooth No 25 6.2 ± 0.4
V C 3 Smooth No 75 46 9.9 10.4 8.8 ± 1.1
4 Smooth Yes 25 6.8 ± 1.3
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 5.8 ± 0.4
IV J 3 Smooth No 75 9.0 9.6 ± 1.1
4 Smooth Yes 25 7.0 ± 0
5 Ground No 25 1.0 ± 2
1 Smooth No 12.5 0.6 ± 0.5
2 Smooth No 25 7.4 ± 0.9
IV H 3 Smooth No 75 8.9 10.0 ± 0
4 Smooth Yes 25 4.8 ± 1.1
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 1.8 ± 1.6
IV B 3 Smooth No 75 79 8.3 7.3 6.0 ± 1.0
4 Smooth Yes 25 5.0 ± 0
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.0 ± 0
IV D 3 Smooth No 75 77 8.2 9.5 5.0 ± 1.4
4 Smooth Yes 25 5.4 ± 0.5
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.0 ± 0
IV K 3 Smooth No 75 7.5 0.6 ± 0.8
4 Smooth Yes 25 5.6 ± 2.8
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.2 ± 0.4
IV I 3 Smooth No 75 80 7.1 0.4 ± 0.5
4 Smooth Yes 25 4.6 ± 0.8
5 Ground No 25 0.0 ± 0
A
The conclusions from this marine exposure program have been summarized by Dr. George DiBari of INCO in his paper Marine Corrosion Performance of EN Coating
on Steel, Final Report on ASTM Program 14 which was presented at EN91 Conference, Product Finishing.

X6.1 Results of 110 Month Exposure of Autocatalytic typical processing and was chosen to evaluate the formation of
Nickel Deposits at Kure Beach, North Carolina: diffusion products of iron, nickel and phosphorus.
X6.1.1 Program 14 is part of an ongoing marine exposure X6.1.3 The following matrix of test panels were prepared
testing process at the 75 m site at LaQue Center for Corrosion and exposed with subsequent analysis for alloy and thickness.
Technology, Wrightsville, NC (Kure Beach). The program Panels were rated at Kure Beach each year by a team from
called for the plating of both Type IV and Type V deposits on ASTM Committee B08 using Practice B537.
standard smooth and ground steel Q Panels. X6.1.4 The interpretation of the results of these exposure
X6.1.2 There were nine different sources of deposits, each test should be made on the basis of general performance of the
providing five lots of five panels. The program involved plating coating on panels. Base metal condition, undercoats, surface
12.5, 25, and 75µ m thicknesses on smooth and ground surface preparation, and post processing all have a significant effect on
and one smooth lot heat treated for hardness at 550°C for 2 h. the performance and should be given careful consideration
The heat treatment temperature was considerably higher than when designing the part and pretreatment processing sequence.

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 B733 − 15

X7. STRIPPING AND REWORK

X7.1 The stripping of electroless nickel deposits requires These solutions are heated and generally remove the deposit at
the use of aggressive chemical or mechanical systems that may a slower rate than nitric acid. As the stripping process proceeds,
damage the base material. Consideration of the risk of stripping a corrosion product may form on the surface which will slow
the deposit should always be considered when selecting this the stripping. When this occurs, the steel or copper plated
coating. Undercoats may be required to facilitate rework. The article is removed, rinsed, electrocleaned, rinsed, and returned
commercially available strippers that have minimal attack of to the stripper. As the deposit nears complete removal, it is
the substrate are available to minimize the risk of etching or common for a slight etch of the substrate to occur. The amount
pitting of the substrate. of material removed varies from nothing to 0.0003 in.
X7.2 Nitric acid is recommended to strip electroless nickel
X7.4 Mechanical peening with a grit is effective in remov-
deposits from aluminum. A solution of between 20 to 30 % by
ing electroless nickel from hard steel parts with non-critical
weight nitric acid should be prepared. After mixing, let stand
tolerances. The article is placed in a chamber and blasted with
until the temperature reaches ambient. If significant area is to
a heavy grit until all the deposit is removed. This method is
be stripped, the solution should be cooled. Articles to be
effective when parts are large and stripping solutions would be
stripped should be clean and free of oils and surface debris that
difficult to manage.
may interfere with the stripping process. Racks and fixtures
made with nylon and drylen are not recommended and are not X7.5 Generally the rework process is limited to less than
compatible with nitric acid and will decompose to a sticky tar
three times. This is because there is some substrate removal
in the stripper. This tar will be difficult to remove from the
each time the article is stripped. When processing some copper
article after stripping. After all the electroless nickel is
or steel alloys, it is advisable to apply a copper undercoat that
removed, the part should be rinsed in clean rinse water.
will prevent the attack of the substrate was the stripping nears
X7.3 Highly alkaline solutions using nitro benzoic acids are completion. This is always a good practice when dealing with
used to remove electroless nickel from steels and coppers. high value copper alloy articles.

REFERENCES

(1) Symposium on Electroless Nickel Plating, ASTM STP 265, ASTM, 12644 Research Parkway, Orlando, FL 32826, 1986 Chapter 23.
1959. (5) Mallory, G., and Hajdu, J. “Electroless Plating,” AESF 12644
(2) Engineering Properties of Electroless Nickel, The International Nickel Research Parkway, Orlando, FL 32826, 1990.
Co., Inc., New York, NY. (6) Parker, K., “Effects of Heat Treatment on the Properties of Electroless
(3) Gawrilov, C. G., Chemical (Electroless) Nickel Plating, Portcullis Nickel Deposits,” Plating and Surface Finishing, Vol 68, December
Press, London, 1974. 1981.
(4) Safranek, W. H., The Properties of Electrodeposited Metals and (7) Parker, K.,“ Hardness and Wear Resistance Tests of Electroless Nickel
Alloys, The American Electroplaters and Surface Finishers Society, Deposits,” Plating, Vol 61, September 1974 .

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