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Coatings N02 207

Textile Systems 001-en


Technical Design Manual Browning DIN 50938 Page 1/1

The following standard is used at Rieter:

DIN 50938: April 2000, pages 1 - 5

Black Oxide Treatment of Steel Components


Requirements and Testing

Recommendations and Engineering Drawing Notation:

Designation for a black oxide coating following DIN 50 938 on a steel (Fe) part, process group (A) bath black
oxide and post-treatment by greasing, oiling or other lubricants (T4).

Release: S. Liefert DTTNS 2003-10-21 Change:


D EUTSCHE NORM April 2000

Black oxide treatment of ferrous products {


Requirements and testing
50938
ICS 25.220.20 Supersedes
November 1987 edition.
Brünieren von Bauteilen aus Eisenwerkstoffen – Anforderungen und
Prüfverfahren

In keeping with current practice in standards published by the International Organization for Standardization
(ISO), a comma has been used throughout as the decimal marker.

Foreword
This standard has been prepared by Technical Committee Chemische und elektrochemische Überzüge of
the Normenausschuss Materialprüfung (Materials Testing Standards Committee).

Amendments
This standard differs from the November 1987 edition in that it has been harmonized with DIN EN 1403 and
DIN 50960-1, and it has been editorially revised.

Previous editions
DIN 50938: 1973-12, 1987-11.

1 Scope
This standard specifies requirements for and methods of testing black oxide coatings produced on ferrous
components by a chemical reaction during an immersion process. This process provides iron and steel (i.e.
cast iron, unalloyed and low-alloy steel) components with uniform black coatings while substantially retain-
ing their dimensional accuracy. The purpose of this treatment is to give the material a particular appearance
and to increase its corrosion resistance even without aftertreatment. The degree of protection provided is,
however, low.
The standard does not cover semi-finished products and fasteners. Threaded articles shall be coated as
agreed.

2 Normative references
This standard incorporates, by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text, and the titles of the publications are
listed below. For dated references, subsequent amendments to or revisions of any of these publications
apply to this standard only when incorporated in it by amendment or revision. For undated references, the
latest edition of the publication referred to applies.
DIN 50017 Artificial climates in technical applications – Condensation water test atmospheres
DIN 50902 Protective coatings on metals – Concepts, application methods and surface preparation
DIN 50960-1 Electroplated and chemically applied coatings – Designation and information in technical
documentation
DIN EN 1403 Corrosion protection of metals – Electrodeposited coatings – Method of specifying general
requirements

Continued on pages 2 to 5.

Translation by DIN-Sprachendienst.
In case of doubt, the German-language original should be consulted as the authoritative text.

© No part of this translation may be reproduced without the prior permission of Ref. No. DIN 50938 : 2000-04
DIN Deutsches Institut für Normung e.V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, English price group 06 Sales No. 0106
has the exclusive right of sale for German Standards (DIN-Normen).
12.01
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DIN 50938 : 2000-04

DIN EN ISO 2064 Metallic and other non-organic coatings – Definitions and conventions concerning the meas-
urement of thickness
ISO 4519: 1980 Electrodeposited metallic coatings and related finishes – Sampling procedures for inspec-
tion by attributes

3 Concepts
3.1 Black oxide coating
A thermally produced dark-brown to black oxide conversion coating produced by immersion of a component
in alkaline salt solution (cf. DIN 50902) to which reducing agents or other reagents may have been added. The
saturation of the colour obtained depends on the nature of the base metal (substrate), the heat treatment, the
surface preparation and the composition and type of treatment bath.

3.2 Significant surface


Unless otherwise agreed, significant surface is an area on a product that can be touched with a ball 20 mm in
diameter.*)

4 Designation
4.1 General
The designation shall include the following information:
a) The word ‘coating’;
b) the number of this standard;
c) a hyphen;
d) the chemical symbol of the base metal or the main component of the alloy;
NOTE: It is recommended that the standard designation of the base material follow the symbol of the base
metal.
e) a solidus;
f) any additional symbols to denote further treatments to be carried out shall be separated by solidi and
give the sequence in which the coatings are applied (see subclauses 4.2, 4.3 and 4.4). If a specific treatment
is not required and thus need not be referred to in the designation, this shall be indicated by a double solidus.

4.2 Coating methods


There are three black oxide coating methods, each resulting in a different mean mass of coating per unit area
(see table 1). These shall be designated as follows:
single-bath coating: A;
two-bath coating: B;
three-bath coating: C.
Table 1: Approximate mean mass per unit area of black oxide coatings
Designation of Approximate mean mass per
coating method unit area of coating, in g/m2
A 4,5
B 5,5
C 6,5

4.3 Heat treatment


The heat treatment shall be designated by the following:
a) the letter ‘H’;
b) the minimum heat treatment temperature, expressed in °C, in brackets;
c) the treatment time, in hours.
Designation of heat treatment carried out for three hours at a minimum temperature of 190 °C:
HT(190)3

*) Translator’s note. In DIN EN ISO 2064, ‘significant surface’ is defined as ‘The part of an article covered or
to be covered by the coating and for which the coating is essential for serviceability or appearance’.
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DIN 50938 : 2000-04

4.4 Supplementary treatments


Any supplementary treatments shall be designated as in table 2.
Table 2: Designation of supplementary treatments applied to black oxide coatings
Symbol Type of treatment
T1 Application of paints, varnishes, pow-
der coatings or similar materials
T4 Application of grease, oil or other lubri-
cants
T5 Application of wax
T10 Application of water-displacing anti-
corrosive agents

NOTE: The symbols conform to the standard designations for supplementary treatment for electrodeposited
coatings as in DIN EN 1403, except for T10.
Designation of a black oxide coating on a steel (Fe) component that has not been heat-treated, but has
undergone the single-bath coating process (A) and then waxed (T5):

Coating DIN 50938 – Fe//A/T5

5 Order details
The customer shall provide the following information:
a) the designation of the coating (see clause 4);
b) whether heat treatment is required prior to coating (see subclause 4.3);
c) the significant surface (e.g. by providing a suitably marked specimen);
d) the quality, state and appearance of the base metal if they may affect the serviceability and appearance
of the coating;
e) the location of unavoidable defects (e.g. attachment points);
f) details of sampling, the acceptable quality level or any test requirement differing from those in ISO 4519
(see clause 7).
The customer may provide the following supplementary information:
g) any special requirements or conditions relating to the surface preparation of the components;
h) any special requirements relating to the reprocessing of discarded components;
i) any other special requirements (e.g. regarding roughness).

6 Procedure
6.1 Preparation of surfaces
The surfaces of the components to be coated shall be carefully degreased and any scale, oxide and other
impurities removed. To prevent the temperature of the bath dropping sharply, the components may be
preheated in water at 60 °C to 80 °C.

6.2 Main treatment


One or more coating stages shall be carried out in boiling alkaline oxidizing solution at about 135 °C to 145 °C,
optionally with reducing agents or other substances added to the bath. Depending on the composition, con-
centration and temperature of the solution, the coatings will develop in immersion times of between five and
twenty minutes. The coating time will also depend on the nature and quality of the components.
The suppliers’ operating and safety instructions shall be observed when making up and using the bath. The
condition of the bath shall be continuously checked by monitoring the boiling point, which is dependent on
concentration. If necessary, this point shall be adjusted to the required value by carefully adding water or
coating salt. No other bath checks are generally needed. In some cases, the quality of the coating may be
improved by adding other salts to the bath.
In the case of the multi-bath methods, the second immersion and, where necessary, the third immersion shall
be carried out in separate baths, the boiling point of each bath being about 5 °C higher than that of the preceding
bath, with a rinse in cold water between baths.
After coating, the components shall be rinsed, first in cold, stationary water, then thoroughly in cold, running
water and finally in hot water at 60 °C to 80 °C.
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DIN 50938 : 2000-04

6.3 Drying and supplementary treatment


After rinsing, the components shall be dried immediately in an oven at about 120 °C or in hot air. Drying is
unnecessary if there is to be an aftertreatment with hot saponifiable oil at about 120 °C, in oil emulsions at 80 °C
to 95 °C or with hot, molten wax. If the components are to be aftertreated in water-displacing anti-corrosion
agents, they shall be treated while cold to minimize the loss of solvent by evaporation.
Supplementary treatments serve to increase the degree of protection. To meet special requirements, paints or
similar coatings may be applied.

7 Testing the untreated coating


The test to be used to assess the quality of the coating or of the bath shall be agreed on a case-by-case basis.
Unless otherwise agreed, the samples shall be collected as specified in ISO 4519 (see clause 5, item f)).
For accuracy experiments, the samples taken shall measure at least 50 mm × 50 mm × 1 mm, be of the same
material grade, have a surface texture as similar as possible to that of the component to be coated and have
received the same treatment prior to coating.

7.1 Appearance
The black oxide coating shall cover the surface of the base metal evenly and completely, and its colour shall
be uniform and as black as possible. There shall be no brownish or greenish spots due to an excessive
concentration or contamination of the coating bath. If a coated component that has not been aftertreated is
wiped with a clean white cloth, no colour shall appear on the cloth, except in the case of cast materials and
hardened components.

7.2 Determining the degree of protection by exposure to a standard atmosphere


The anti-corrosive effect of the coating shall be determined by suspending components or specimens that have
not been aftertreated, but dried as described in subclause 6.3, in the DIN 50017 – KK standard atmosphere.
This test may be commenced immediately after the specimens have been dried and cooled to ambient tempera-
ture.
Table 3: Minimum exposure times in DIN 50017 – KK test
Minimum time with no signs
Coating method
of corrosion, in hours
A 24
B 48
C 72

The minimum exposure time shall be as specified in table 3, after which not more than 1 % of the surface of
the component tested shall be covered with rust, unless otherwise agreed. Slight changes in hue shall be
ignored. When components having highly contoured surfaces are tested, the minimum exposure time shall be
agreed on a case-by-case basis. To prevent edge corrosion, sharp edges shall be coated with acid-resistant
paint after coating and prior to being placed in the test chamber. Any corrosion at such points shall be ignored.

7.3 Determining the degree of protection with acetic acid at ambient temperature
7.3.1 Test solution
20 % (m/m) aqueous solution of analytical grade acetic acid, CH3COOH.

7.3.2 Procedure
After coating, the components or specimens shall not be aftertreated, but dried as specified in subclause 6.3
and cooled to ambient temperature. About four drops of the test solution shall then be applied to a flat area
of the coated specimen or component. The time taken for the surface of this area to be exposed shall not be
less than that specified in table 4.
When components having highly contoured surfaces are to be tested, full immersion with amended times may
be agreed.
Table 4: Minimum exposure times in acetic acid test

Minimum exposure time,


Coating method
in minutes
A 10
B 20
C 30
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DIN 50938 : 2000-04

Table 5: Assessment of oxalic acid test


Appearance of exposed
Quality of coating
coating area
Grey with light-grey halo Inadequate
Black to brownish black Good
with exposed halo1)
1) Even good quality coatings may have very
bright halos due to metal being exposed at the
boundary of the area to which the solution was
applied. However, assessment shall be based
solely on the area covered by the drops.

7.4 Determining the degree of protection with oxalic acid at ambient temperature
7.4.1 Test solution
5 % (m/m) aqueous solution of analytical grade oxalic acid, C2H 2O4 . 2 H 2O.

7.4.2 Procedure
After coating, the components or specimens shall not be aftertreated, but only dried as specified in subclause
6.3 and cooled to ambient temperature. About three drops of the test solution shall then be applied to a flat area
of the coated specimen or component.
After eight minutes’ exposure, the test solution shall be rinsed off with water and the affected area evaluated
visually as in table 5.

7.5 Determining the mass per unit area


7.5.1 Test solution
Chemically pure 1 mol/l hydrochloric acid with a commercial inhibitor added, the inhibitor being chosen so that
the loss in mass, m0, determined as specified in subclause 7.5.2, is less than 0,5 g/m2.
An adequate inhibitory action is achieved, for example, if a 4 % (m/m) solution of hexamethylenetetramine,
C 6H 12N 14, in 1 mol/l hydrochloric acid is used.

7.5.2 Procedure
The coated, dried specimen or component shall be weighed (mass m1) after the area of the surface, A, has been
determined.
The specimen or component shall then be immersed in the test solution at ambient temperature until the coating
has been dissolved. It shall then be removed, rinsed, dried and reweighed (mass m2).
To determine the loss in mass of steel due to the action of the test solution containing inhibitor, m0, uncoated
test sheets or components made of the same material shall be weighed (mass m3), treated for the same time
as the coated component with test solution, dried and reweighed (mass m4 ).
The loss in mass, m0, is given by equation (1):

m0 = m 3 – m4 (1)

The value of m0 shall be taken into account when calculating the loss in mass, Dm, of the coated part, using
equation (2):

Dm = m 1 – m 2 + m0 (2)

The mass per unit area, mA, in g/m2 , is given by equation (3):

Dm
mA = × 10 (3)
A

where m is in mg and A is in cm².

8 Test report
The test report shall refer to this standard and include the following details:
a) type and designation of coated component;
b) type and designation of coating;
c) type and results of testing as described in clause 7.

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