Double Etching Method for Steel Roll Surfaces

by Henrik Kaker
 Contents

1 Etching flaw detection 3

2 Preparation of etching solution 3

2a Nitric acid solution 3

2b Hydrochloric acid solution 3

3 Etching procedure 4

3a Removing oil from roll surface 4

3b Etching procedure 4

4 Characteristics and problem on abnormality to be detected by etching 7

4a Crack detection by etching 7

4b Retempered and rehardened portions 8

4c Relation between fatique failure due to crack and abnormality detected

by etchnig 9

4d Examples of abnormality detected by etching 11

5 Conclusion 12
1 Etching flaw detection

Finding cracks on the steel roll surfaces is sometimes very difficult task and this
short paper shows simple and very effective method for finding this cracks by
chemical etching of the roll surface.

2 Preparation of etching solution

For etching we normally used solution described in the text bellow. You may also
used Aqua Regia (1 part HNO3 and 3 parts HCl) or diluted Agua Regia (1 part H2O, 1
part HNO3, 3 parts HCl and 20 g/l CuCl2).

Note: All chemical, including many metals and oxides, pose some degree of danger to the human
organism. This may come about by ingestion through the respiratory or digestive tracts or by external
contact with the skin or eyes. Basically, the same precautions apply to the metallographic laboratory as to
all chemical laboratories, except that certain specific areas are particularly critical. Some significant
precautions are: Clearly label all storage containers. Dilute concentrated chemicals before disposal and
observe all local waste-disposal regulations. Critical substances (flammable, explosive, toxic, or corrosive)
should be stored in approved containers in cool, fireproof, isolated areas. When preparing etchants
containing aggresive chemicals such as sulfuric acid, the chemical should always be added to the solvent
(water, alcohol, etc.) slowly with gentle stirring. External cooling may also be required if haet evolution is
particularly strong. Volatile, flammable and explosive materials, such as benzone, acetone, ether,
perchlorate, nitrate, etc. should not be heated or kept near open flames. Mixtures of alcohol and
hydrochloric acid can react in various ways to produce aldehydes, fatty acids, explosive nitrogen
compounds, etc. The tendency toward explosion increases with increasing molecule size. Hydrochloric acid
content should not exceed 5 % in ethanol or 35 % in methanol. These mixtures should not be stored.
Hydrofluoric acid is a very strong skin and respiratory poison that is hard to control. It should be handled
with extreme care, because sores resulting from its attack on skin do not heal readily. Hydrofluoric acid
also attack glass, and fumes from specimen etched in HF solution could easily damage front element of
microscope lenses. Specimen should be rinsed throughly and some cases placed in a vacuum desiccator
for one or two hours before examination.

2a Nitric acid solution

Mix 50 cm3 water (H2O) and 50 cm3 nitric acid (HNO3) in the glass bottle. Put cap on
the bottle, but do not seal. Mix solution with slight and gentle shake. Completely seal
and store and label the bottle with the name ‘Nictric acid solution’.

2b Hydrochloric acid solution

Mix 50 cm3 water (H2O) and 50 cm3 hydrochloric acid (HCl) in the glass bottle. Put
cap on the bottle, but do not seal. Mix solution with slight and gentle shake.
Completely seal and store and label the bottle with the name ‘Hydrochloric acid
solution’.
3 Etching procedure

3a Removing oil from roll surface

Oil on roll surface hinders the proper effect of etching. To avoid this, oil should be
first removed before performing etching. Wipe off oil on roll surface with waste cloth
as much as possible.

1. Apply a thin coat of cleaning oil (kerosene) over the entire surface of the roll
Then flush the surface with water.

2. Rub the roll surface with a cloth immersed in hydrochloric acid solution to remove
remaining oil. Then flush the surface with water.

3. Wipe off remaining oil with volatile liquid like alcohol or gaseline.

4. Polish the roll surface well with emery paper. Remaining oil is removed almost
completely by the method (1) for etching wide range. The method (3) and (4) are for
etching the narrow area because of time needed.

Adhering oil can be removed completely by slight grinding of the roll surface by
grinding machine. If there is some welding of sheet or roughness on the roll surface
due to previous rolling accidents, grinding of roll surface is required before etching.

3b Etching procedure

1. Apply nitric acid solution.

2. Flush water to run out the acid after the roll is etched in black.

3. Apply nitric acid solution again.

4. When the roll surface become black, flush it with water.

5. Apply hydrochloric acid.

6. When the entire surface become whitish or silver white, rub it with waste cloth
while pouring water.

7. Dry the surface.

Caution

1. When applying nitric acid solution, special attention should be paid so that the roll
surface can be etched uniformly. When the etching is not uniform, rub the roll
surface with waste cloth immersed in nitric acid solution to gradually permit uniform
etching. In this first application of nitric acid solution a slight unevenness of etching
is allowable.

2. Utmost care should be taken to apply hydrochloric acid uniformly. Make sure that
the acid is evenly applied on the entire roll surface.

3. Pour water in the step (6) above when the normal portion becomes whitish or
silver white, in a striking contrast to the area abnormally etched in black.

4. Blow jet air for drying comperatively large area. Drying aperation should be
carried out as quickly as possible. Otherwise the roll surface might be rusted,
causing difficulty in detection cracks.

A blow of breath my be enough, if for drying small area. Refer to Image 1 for detail
of etching procedure.

Oil adheres on the roll surfaces after

rolling.

Sometimes rolled material adheres.

Remove oil.

Remove the sticking material (grinding).

Etching.

By rubbing the surface with a cloth, it

can be etched uniformy.
Washing.

Flush the etching residue with water.

Also rub with a cloth.

Etching.

Pour the etching solution successively

from one end in rotationg the roll. (There
is no need to rub the roll with a cloth this
time.)

Washing.

Flush with water and rub with a cloth to

remove the etching residue.

Contrast normal portion with abnormal

portions.

Pour hydrochloric acid solution

successively from one end, rotating the
roll. This procedure should be carried out
quickly, and the etching solution should
be poured as uniform as possible.
 Washing.

After attaining the suitable contrast

between the normal and retempered
portion, pour water.

In case of no retempered zone, pour

water, when the whole becomes
silverwhite.

When pouring of water is too late the

retempered portion also become whitish.

Drying.

Drying should be carried out as quickly

as possible. Otherwise roll surface is
partially rusted, so that the detection of
the retempered portion and cracks is
somewhat difficult.

Image 1: Etching procedure.

4 Characteristics and problem on abnormality to be detected

by etching

4a Crack detection by etching

Image 2 shows the mechanism how invisible crack is detected by the etching. Crack
occurring on the roll has, in general, a narrow width and is in a compressed status.
Therefore, it is diffucult to identify by naked eye inspection. In the etching process,
etching solution penetrated in the crack emerges on the roll surface as it dries and
magnifies, the with of a crack and thus gives an appearance of a wider of the crack
for easy detection.
Image 2: Schema of the detecting process of crack by etching.

4b Retempered and rehardened portions

Altrough an abnormal portion is found black ordinarily by etching method, sometimes

an abnormal whitish or silverwhite portion edged in black may also be identified.
This abnormal white occours if heating temperature exceeds the transformation
point. The correlation with retempered and regardened portions is shown in Image 3.
Figure 3: The relation between retempered and rehardened part.

4c Relation between fatique failure due to crack and

abnormality detected by etchnig

If a roll is put to subsequent rolling without removing cack by grinding, stress is

concentrated on the cracked portion and the fatique fracture will further develop. If
fatique fracture reaches to a certain degree, spalling will occur.

Spalling is scarely broken out by single rolling, but tends to occur after several rolling
operations. In many cases, the initial abnormality is removed completely and only
the portion deteriorated by fatique is left even after several times of roll surface
grinding after crack occurs.

Image 4 indicates a relationship between the fatique failure due to ordinary crack
and the abnormality detected by etching.
 In this condition crack is followed by the
retempered or rehardened cone.

In the initial step of the fatique fracture

generally the retempered zone is left on
the surface.

In this step, roll surface is often in the

condition that the retempered, or
rehardened zone, and initial crack are
removed completely.

Generally there is nothing except fatique

cracks on the surface, when the spalling
occours.

Image 4: Schema of the relation between the fatique fracture from cracks and the
abnormal etching part.
4d Examples of abnormality detected by etching

Image 5 indicates an example of abnormality detected by etching. There are so

many abnormalities that there is no identical case assumed.

Example of welding. Appearance after etching, removing the

left welding. Black area is the
retempered portion. White part in the
black zone is rehardened. In the black
area there are some cracks.

The retempered portion and crack by The retempered and rehardened portions
slip accident. by the slip accident.

The abnormal part by hitting the
grinding wheel.
Enlarged view of the left photo.
The whitish part edged in black is the
rehardened part.
Black of the edge is the retempered part.
Cracks appear in the outside of black and
rehardened part.

The abnormal part by hitting the
grinding wheel.
An example of the retempered part and
crack which becomes the origin of the
spalling.
The origin of the above spalling is crack
which appears in the retempered zone.

The abnormal part by the hitting. The Conditions of the abnormal part partially
whitish is the rehardened part. The removed. In the interior of the whitish
black is retempered part. part, the black part appears.

Image 5: Examples of abnormalities detected by double etching.

5 Conclusion

This short paper introduced the most suitable method for the easy detection of crack
accurring on the roll surface. This etching method is adopted to your roll
maintenance pratice it will certainly work to prevent spalling of roll and troubles such
as unevennes of luster and so on in rolling.