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Iso 2819 1980

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International Standard

INTERNATIONAL ORGANIZATION FOR STANDARDIZATlON.MEX,QYHAPO~HAR OPTAHM3AL&lR fl0 CTAH~APTM3A~MM.ORGANlSATlON INTERNATIONALE DE NORMALISATION

Metallic coatings on metallic substrates -


Electrodeposited and chemically deposited coatings -
Review of methods available for testing adhesion
Revgtements mt?talliques sur bases m&al/iques - DdpSts 6lectrolytiques et d&p&s par voie chimique - Liste des diffkentes
m&hodes d’essai d’adhkence

Second edition - 1980-08-01

UDC 669.058 : 620.179.4 Ref. No. IS0 2819-1980 (E)


Descriptors : metal coatings, electrodeposited coatings, chemical plating, tests, adhesion tests, adhesion, mechanical tests, quality contra;.
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FOREWORD

IS0 (the International Organization for Standardization) is a worldwide federation


of national standards institutes (IS0 member bodies)., The work of developing
International Standards is carried out through IS0 technical committees. Every
member body interested in a subject for which a technical committee has been set
up has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work.

Draft International Standards adopted by the technical committees are circulated


to the member bodies for approval before their acceptance as International
Standards by the IS0 Council.

International Standard IS0 2819 was developed by Technical Committee


ISO/TC 107, Metallic and other non-organic coatings.

It was submitted directly to the IS0 Council, in accordance with clause 5.10.1 of
the Directives for the technical work of ISO. It cancels and replaces the first edition
(i.e. IS0 2819/l-1973), which had been approved by the member bodies of the
following countries :

Egypt, Arab Rep. of Italy Sweden


France Japan Switzerland
Germany, F. R. New Zealand Thailand
Hungary Poland Turkey
India Portugal United Kingdom
Ireland Romania USSR
Israel South Africa, Rep. of

The Member Body of the following country had expressed disapproval of the
document on technical grounds :

Netherlands

0 International Organization for Standardization, 1980 l

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INTERNATIONAL STANDARD IS0 2819-1980(E)

Metallic coatings on metallic substrates -


Electrodeposited and chemically deposited coatings -
Review of methods available for testing adhesion

1 SCOPE AND FIELD OF APPLICATION adhesion is indicated by the appearance of a blister which
grows as the rubbing is continued.
This International Standard describes methods of checking
the adhesion of electrodeposited and chemically deposited If the mechanical properties of the coating are poor, the
coatings. It is limited to tests of a qualitative nature. blister may crack and the coating will peel from the basis
Table 2 indicates the suitability of each test for some of metal. This test shall be limited to relatively thin deposits.
the most usual types of metallic coatings. Most of the tests
described are capable of destroying both the coating and 2.2 Ball burnishing test
the article being tested, but some destroy the coating only.
Even if the adhesion of the coating is found to be satis- Ball burnishing is frequently used for polishing, but it can
factory on articles not destroyed in testing, it should not be be used also to test adhesion. Using a barrel or vibratory
assumed that the articles are undamaged. For example, the burnisher with steel balls about 3 mm in diameter and soap
burnishing test (see 2.1) may render an article unacceptable solution as lubricant, it is possible to produce blisters when
and the thermal shock test (see 2.12) may produce un- the adhesion is very poor. The method is suitable for
acceptable metallurgical changes. relatively thin deposits.

This International Standard does not describe certain tests


2.3 Shot peening test
which have been developed at various times to give a quan-
titative measure of adhesion of metallic coating to a sub- There are some variations of the principle by which the
strate since such tests require special apparatus and con- hammering action of iron or steel balls, allowed to fall by
siderable skill in their performance which renders them gravity or forced by means of a pressure air stream onto the
unsuitable as quality control tests for production parts. surface to be tested, produces deformation of the deposit.
Some of these quantitative tests may, however, be useful
in research and development work. If the coating is poorly bonded, it will become blistered.
Usually, the intensity of peening necessary to cause non-
When particular methods of adhesion testing are included adherent coatings to blister varies with the coating thick-
in International Standards for individual coatings, they ness, thin coatings requiring less than thick coatings.
should be used in preference to the methods described in
this International Standard and should be agreed upon One test can be performed using a tube 150 mm long,
beforehand by the supplier and the purchaser. 19 mm internal diameter, as the reservoir for round iron or
steel shot (0,75 mm diameter approximately) connected to
a nozzle. Compressed air is brought to the apparatus with a
pressure of 0,07 to 0,21 MPa’ ) and the distances between
2 METHODS OF TEST nozzle and specimen are 3 to 12 mm.

.Another test, that appears to be the most suitable for


2.1 Burnishing test checking the adhesion of electroplated coatings of silver
If plated parts are subjected to burnishing in a localized during production of coatings from 100 to 600 pm in
area, the deposit will tend to work-harden and absorb thickness, is described in the annex and employs a standard
frictional heat. If the coating is thin, separation of the air-operated cabinet of the type used for shot-peening steel
coating from the basis metal as blisters will occur under parts.
these conditions in areas of poor adhesion. If the silver is poorly bonded, it will extend or flow and
When the shape and size of the part permit, an area of not become blistered.
more than 6 cm2 of the plated surface should be rubbed
with a smooth implement for about 15 s. A suitable 2.4 Peel test
implement is a steel rod 6 mm in diameter with a smooth
hemispherical end. This test is suitable for coatings less than 125 pm thick on
substantially flat surfaces. A strip of tinned mild steel or
The pressure shall be sufficient to burnish the coating at brass, approximately 75 mm long x 10 mm wide x 0,5 mm
every stroke but not so great as to cut the coating. Poor thick, is bent at right angles 10 mm from one end and the
I) 1 MPa=l MN/m2
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IS0 2819-1980(E) ,

shorter limb soldered flat to the coated surface. A load is appears to be PO separation at the fracture, a sharp chisel
applied to the free limb and normal to the soldered surface. is used to try to raise the coating at the edge. If the coating
The coating will be detached from the substrate if the can be peeled from the edge for an appreciable distance,
adhesion is weaker than the soldered joint. If the adhesion poor or weak adhesion is indicated. The cutting edge of
of the coating is greater than this, however, failure will the chisel shall be sharpened prior to each test.
occur in the soldered joint or within the thickness of the
coating. Thinner coatings can be tested by substituting a knife for
the chisel and light tapping with a hammer may or may not
This method is not widely used because the temperature be used. The chisel test is not suitable for soft coatings such
reached during the soldering operation might alter the as zinc or cadmium.
adhesion. Alternatively, the test can be performed using an
adhesive of hard-setting synthetic resin of adequate tensile 2.8 Scribe and grid test
strength in place of solder.
Using a hardened steel scribe which has been ground to a
Another test (the tape test) employs an adhesive cellulose sharp 30’ point, two parallel lines are scribed at a distance
tape, with an adhesion value of approximately 8 N per apart of about 2 mm. In scribing the two lines, enough
25 mm width, whose adhesive side is applied to the coating pressure shall be applied to cut through the coating to the
under test, using a fixed-weight roller, care being taken to basis metal in a single stroke. If any part of the coating
exclude all air bubbles. After an interval of 10 s, the tape is between the lines breaks away from the basis metal, the
removed by applying a steady pulling force to the tape, coating shall be deemed to have failed the test.
perpendicular to the surface of the coating. The adhesion of
the coating shall be such that there is no evidence of One variation of the test is to draw a square with a grid of
detachment of the coating. This test is particularly used for 1 mm side and observe whether the coating peels from the
testing adhesion of coatings on the conductors and contacts basis metal within this area.
of printed circuits. Coated conductors shall be tested over
an area of at least 30 mm2. 2.9 Bending test

2.5 File test The bend test consists in bending or flexing the coated
products. The extent and nature of the distortion will vary
A piece sawn off a coated article is held in a vice and a with the basis metal, the shape, the nature of the coating
coarse mill file (one set of serrations only) is applied to the and the relative thickness of the two layers.
cut in such a manner as to attempt to raise the coating. The
file is used in the direction from the basis metal to the The test is usually carried out by hand or with pliers,
coating at an angle of approximately 45’ to the coated bending the specimen as sharply as possible first to one side
surface. No detachment of the coating shall occur. This test then to the other, until the specimen breaks. The rate and
is not suitable for very thin coatings and for soft coatings the radius of bending can be controlled using suitable mach-
such as zinc or cadmium. ines. The test produces a shearing stress between the basis
metal and the deposit; if the deposit is ductile, the shearing
force is much reduced because the coating flows and the
2.6 Grinding and sawing tests
basis metal can even break without the coating loosening.
Grind an edge of the coated specimen with a grinding wheel
A brittle deposit can crack but even so the test can give
with the direction of cutting from the basis metal to the
some information about the adhesion; the fracture must be
deposit. If adhesion is poor, the deposit is torn from the
inspected to determine whether the deposit peeled or can
base. A hacksaw can be substituted for the grinder. It is
be removed with a knife or chisel.
important to saw in such a direction that a force is applied
that tends to separate the coating from the basis metal. Any sign of peeling, ch i PPin g or flaking is taken as indi-
Grinding and sawing tests are especially effective on harder cation of PO0 r adhesion.
coatings such as nickel and chromium.
The coated specimen can be distorted with the coating on
either the inside or the outside of the specimen. The
2.7 Chisel test
behaviour of the coating is normally observed on the
The chisel test is normally used on coatings of considerable outside layer, although in some cases further information
thickness (greater than 125 urn). may be gained by examining the inside of the bend.

One variation of the test is to place a sharp chisel at the 2.10 Twisting (winding) test
back of a coating overhang, and give it a sharp hammer
blow. If the adhesion is good, the coating will break away In this test the specimens (normally strips and wires) are
or be cut through without the bond between basis metal twisted around a mandrel. Each part of the test can be
and coating being affected. standardized : the length and width of the strip, the rate of
bending, the uniformity of bending movement and the
Another type of “chisel test” is combined with the “saw
diameter of the rod around which the piece is twisted.
test”. The test is made by sawing the specimen perpen-
dicular to the coating; if the adhesion is not very good, Any sign of peeling, ch ippin g or flaking is taken as indi-
failure immediately becomes evident. In cases where there cation of poor adhesion.
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IS0 28194980 (E)

The coated specimen can be distorted with the coating on 2.13 Drawing test
either the inside or the outside of the specimen. The
Drawing tests are most generally used on coated sheet
behaviour of the coating is normally observed on the
metal. The most common are the “Erichsen cupping
outside layer, although in some cases further information
test’12) and the “Romanoff flanged cap test”.
may be gained by examining the inside of the bend,
They produce a deformation of the deposit and basis metal
2.11 Tensile test into a cup or flanged depression by means of some sort of
plunger.
This is suitable only for certain types of coated article. The
article is stressed in tension until it breaks. Some cracking In the Erichsen test, a ball-shaped plunger 20 mm in
of the coating will normally be evident near to the fracture, diameter is pushed into the specimen with a speed of 0,2 to
but no detachment of the coating from the basis metal shall 6 mm/s to a desired depth with a suitable hydraulic device.
be visible. Poorly adherent deposits peel or flake from the basis metal
after a few millimetres’ distortion, while adherent deposits
2.12 Thermal shock test exhibit no peeling, even when the basis metal has been
cracked by the penetrating mandrel.
The adhesion of many deposits can be determined by
heating the coated specimen and then suddenly cooling it. The apparatus for the Romanoff test consists of an
The principle involved in this test is the difference in ordinary press with a set of adjustable dies for drawing a
coefficient of expansion between the coating and the basis flanged cap. The flange is 63,5 mm in diameter and the cap
metal. 38 mm in diameter. The depth of the cap is adjustable
from 0 to 12,7 mm. The specimens are usually tested to a
It is therefore applicable when the coefficient of expansion point which will fracture the cap. The intact part of the
of a coating is appreciably different from that of the basis draw shows how drawing affects the structure of the
metal. The test is performed by heating the specimen in an deposit. These methods are used specially for deposits of
oven for a sufficient time to achieve the appropriate the harder metals, such as nickel or chromium.
temperature shown in table 1. The temperature shall be
maintained within + 10 “C. Metals that are sensitive to In all cases, the results must be cautiously interpreted since
oxidation shall be heated in an inert or reducing the ductilities of both the deposit and basis metal are
atmosphere or in suitable liquids. involved.

TABLE 1 - Thermal shock test temperatures


2.14 Cathodic test

Chromium, nickel, The coated part is made cathodic in a solution from which
nickel + chromium, Tin only hydrogen is evolved. Blistering of the coating may take
copper and tin-nickel place due to pressure of gaseous hydrogen which diffuses
through certain coatings and accumulates at the site of any
discontinuities between the coating and the basis metal.
Steel 300 (’c 150°C

Zinc alloys 150°C 150°c


The test is performed using a 5 % solution of sodium
hydroxide (p 1,054 g/ml) and treating the specimen for
Copper and copper alloys 250 ” C 150°C 2 min with a current density of 10 A/dm2 at 90 “C. Small
Aluminium and aluminium blisters form at points where adhesion is poor. If the
220°C 150°C
al lays coating is still free from blisters 15 min afterwards, the
adhesion may be regarded as good. Alternatively, a solution
of sulphuric acid [5 % (m/m)] can be used at 60 “C with a
The specimen shall then be quenched in water at room current density of 10 A/dm 2. Weakly adherent coatings
temperature. No separation, for example by blistering, develop blisters in 5 to 15 min under these conditions.
flaking or exfoliation, of the coating from the basis metal
shall occur. The electrolytic test is limited in application to coatings
which are permeable to cathodically discharged hydrogen.
It should be mentioned that heating generally improves the Nickel or nickel-chromium coatings react satisfactorily to
bond strength of electrodepositsl) so that any test method the test if they are weakly adherent. Coatings of metals
which requires heating of the test piece does not give a such as lead, zinc, tin, copper or cadmium are not suitable
correct indication of the bond strength “as plated”. for testing by this method.

1) In other cases, the diffusion of the coating into the basis metal can create a brittle layer so that the peeling of the coating is caused by
fracture rather than non-adhesion l

2) For a full description of the method, see IS0 1520, Paints and varnishes - Cupping test.
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ISO2819-1980(E)

TABLE 2 - Adhesion tests appropriate for various coating metals

Coating metal Nickel


Tin-nickel
Cadmium Chromium Copper Nickel + Silver Tin __ Zinc Gold
Adhesion test alloy
chromium

Burnishing * * * * * * * * *

Ball burnishing * * * * * * + * * *

Peeling (soldering method) * * * *

Peeling (adhesive method) + * * * * * * *

File * + * *
---
Chisel * * * * *
-
Scribe * + * * * * * *

Bending and twisting * * * + *

Grinding and sawing + * * *


------_
Tension + * * * * * +

Thermal shock * * * * 3 *

Extrusion (Erichsen) * + * + *

Extrusion (Flanged cap) * * * * * *


.
J
Shot-peening * a

Cathodic treatment + * *
, l

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IS0 28194980(E)

ANNEX

DETERMINATION OF ADHESION OF SILVER DEPOSITS (100 to 600 urn) -


SHOT-PEENING METHOD

A.1 SCOPE group them in lots in which the difference in maximum


thickness is 125 pm or less.
This test method is used to evaluate the adhesion on steel
of silver deposits of thicknesses between 100 and 600 urn. Peen the silver-plated surfaces at the minimum peening
The results refer to qualitative tests only. The method does intensity shown in the diagram relative to the maximum
not destroy the parts on which the adhesion of the coating measured thickness. Peening intensity must be regulated by
is satisfactory. tests on an Almen A specimenl) before beginning treat-
ment of each lot.

A.2 REFERENCE Control of peening intensity shall be done on an


Almen A specimen at least once an hour.
IS0 2 178, Metallic and vitreous or porcelain enamel
coatings - Measurement of coating thickness - Magnetic Remove the mask from the surfaces that have not been
method - Non-magnetic coating on magnetic basis metal. peened.
Inspect the peened surface visually; it should be completely
A.3 TEST EQUIPMENT peened. If there are non-peened areas, treatment must be
repeated.
A.3.1 Peening equipment Check that no steel shot has been trapped in the coating-
Remove any residual shot by means of air blowing.
Normal compressed air or centrifugal-type shot-peening
equipment.

A.3.2 Shot
A.5 EVALUATION
Spherical steel shot of average diameter 0,4 mm and hard-
Examine the silver-plated surface carefully with the naked
ness not less than 350 HV. Dimensions are determined by
eye. Where adhesion has been poor, bubbles or blisters will
screening and must correspond to those given in the
form during the test on the silver deposit or the coating
following table.
itself will be detached.

Screen mesh (mm) % shot held

0,707 Q 10
A.6 REGULATION OF PEENING INTENSITY
0,420 2 85
Use a test specimen from carbon steel sheet, hardness range
0,354 2 97
400 HV 30 to 500 HV 30 and thickness of I,6 mm, which
has been cut to a size of 76 f 0,2 mm x 19 f 0,l mm and
Inspection of shot dimensions must be performed by ground to a thickness of I,30 + 0,02 mm (Almen A specimen).
screening at least once a week on a sample of 100 g of shot The deviation from flatness shall not exceed an arc height
taken from the peening nozzles.
of 38 pm when measured as specified below.
With the specimen rigidly held in the fixture shown in the
A.4 PROCEDURE , figure, peen it on the exposed side.
Before peening, submit all parts to stress relieving by After peening, remove the specimen from the fixture and
heating at 190 + 10 “C for 2 h. measure the curvature of the unpeened surface with a depth
Mask all surfaces that are not to be peened. WJW, the specimen b,eing supported on four 5 mm
diameter balls forming a rectangle 32 mm x 16 mm. Align
Measure the thickness of the silver using a nondestructive the gauge symmetrically on the specimen with its centre
method (for example according to IS0 2178). Discard the stylus at the centre of the specimen. Measure the arc height
parts where silver thickness is less than 100 pm or greater at the centre of the specimen over the gauge length of
than 600 urn and those where the difference between the 32 mm, measuring to the nearest 25 urn. The conditions of
maximum and minimum thickness is 125 urn or more. Mark peening are then adjusted, if necessary, to give the required
all acceptable parts with their maximum thickness and arc height.

1) See clause k6.


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ISO2819-1980(E)

Peening intensity as a function of silver thickness

22
21
0,50 20
19
0,45, 18 A
F
17 F
ci 5
0,40 16 i
8
15 3
8
0,35 14 %
E
13
;ii
0,30 12
.-i
v)
11
i
10 .-c
0,25
9 .-F
5
0,20 8 t?

7
0,15 6
5
0,lO 4
3
0,05 2
1
0

Silver thickness, mm

Dimensions in millimetres

Steel set screws, @ 4 to 5 Body, tool steel

FIGURE - Fixture for peening test specimen

I) For further explanation, see Society of Automotive Engineers (USA) Standard SAE J 442 a, Test strip, holder andgage for shot Peening.
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