Measurement of Prep Ene Trant Etch
Measurement of Prep Ene Trant Etch
Measurement of Prep Ene Trant Etch
INTRODUCTION
ost penetrant testing specifications
go into great detail about how to
control the penetrant materials, the
equipment and the process, but some say little about how to control pre-penetrant etching. For example, paragraph 7.1.5 of ASTM
E 1417-05 says Etching processes shall be
developed and controlled to prevent damage to components under test (ASTM,
2005). Statements like this leave the controls and degree of control wide open. Who
agrees to whatever is developed? Nadcap
mandates much of what we do at our business, such as the statistical process control.
This is because we also perform chemical
milling, macro-etching and passivation,
and we are required by most of our customers to have chemical processing approval from Nadcap. Nadcap does not require these same controls for NDT labs or
manufacturers that perform their own
etching in support of their penetrant testing. So how does the NDT industry control
etching when there may be only limited
specification requirements? This paper is
limited to how we measure etch rate at our
particular business: perhaps some of the
questions brought up herein will inspire
others to write about some of their own
etching control methods. Important equations are discussed in the body of the
paper, with their derivations given in the
appendices.
rate, almost none require measuring the resulting stock removal on the etched part.
The removal from the part is usually assumed to be what the etch rate said it
should have been. This is probably the best
approach, as mechanically measured removal values are not trustworthy for reasons discussed later. However, this means
that control of etch rate and visual testing
of the etched surfaces is very important.
Figure 1 Individual control chart for a given tank (no temperature correction).
T0 TF
2te
measured in inches/surface/minute,
with te being etch time.
(a)
(b)
(d)
(c)
Figure 2 Tabs: (a) thin, flat; (b) thick, flat; (c) long cylindrical; (d) short cylindrical.
R=
WO WF
454 ( AS ) ( 2 )( d ) (te )
R=
W
454 ( AS ) ( 2 )( d ) (te )
or
(3)
where
WO = original weight (in grams)
WF = final weight (in grams)
454 = the approximate number of
grams in a pound
d = density (in pounds per cubic inch)
AS = surface area (in square inches [the
2 reflects the fact that there are two
surfaces being etched])
te = etching time (in minutes)
W = the weight differential (original
weight minus final weight)
the resulting etch rate is in inches per surface per minute.
This calculation ignores the area of the
edges of the tab and is probably the second
or third most common method of calculation for measuring etching rate. It works
only for tabs with large surface to thickness
ratios. In SI units, the equation would be
(4)
R=
W
( AS )( 2)( d )(te )
(we actually use 2.350). We use the equations in Table 1 to calculate the time to remove 2.54 mm (0.1 mil) per surface for the
noted alloy families.
To take another example, our titanium
etch tank had a standard UNS R56400 (6-4 Ti)
tab with a starting weight of 26.1389 g, and a
final weight of 25.8003 g, which gave a W of
1.2737 g in 20 min. The etch rate (R) was then
1.3767 mm (0.05420 mil)/surface/min and the
time to remove 2.54 mm (0.1 mil) of stock per
R=
( W )T0
( W0 ) ( 2)( te )
where
W = the weight loss (W0 WF) in grams
W0 = the original weight in grams
T0 = the tab starting thickness
measured to 2.54 mm (0.1 mil) with a
microthickness gage
te = the etching time (20 min in our
case).
This gives the rate in inches/surface
/minute if the thickness is measured in
inches, and in millimeters/surface/minute
if the thickness is measured in millimeters.
Because this method ignores the area of the
edges of the tab, the surface area to thickness
ratio of the tab should be no less than 100 to
1. If the previous calculation was the second
most commonly used calculation, then this
is the third most common. See Appendix 2
for the derivation of this equation.
Thick, Flat, Non-standard Alloy Tabs
If the available tab is not thin (surface
area to thickness ratio < 100 to 1), then the
stock loss from the total surface area of the
tab must be taken into account (including
the edges), and you can no longer use the
percent thickness loss as a substitute for the
percent volume loss (Figure 2b). Given tab
length l, width w and thickness T, the etch
rate formula becomes:
where
AS = surface area (in square
centimeters)
d = density (in grams per cubic
centimeter)
the resulting etch rate is in centimeters
per surface per minute.
1236 Materials Evaluation/December 2008
t = 1.638/DW
t = 2.288/DW
t = 2.350/DW
t = 4.010/DW
t = 4.180/DW
t = 4.350/DW
(8)
R=
( W ) Tlw
W0 ( 2) ( lw + Tw + lT ) te
W ( d )
R=
W0 ( 4 ) te
where
d = the starting tab diameter (in inches) measured with a thickness gage
to 0.1 mil.
If the tab is a hollow tube, substitute the
difference between the outer and inner diameters for d in the above equation. See
Appendix 4 for its derivation.
If you use the percent weight loss equation for a thin flat tab to calculate the etch
rate for a long round tab by substituting the
tab diameter for the thickness T in the flat
tab equation, you will have made an error
of a factor of 2 in the calculated etch rate
and you will remove only one half the
stock you thought you did.
Short Non-standard Cylindrical Tabs
What if the available cylindrical tab
length is not at least 8.3 times greater than
its diameter (Figure 2d)? With diameter d
and length l, the equation for etch rate becomes
(10)
W ( l )( d )
R=
W0 ( 2)( d + 2l ) te
(11)
RS = RD + 0.05 ( S )
where
RS = the corrected etch rate to a
standard temperature
RD = the daily etch rate
tS = the standard temperature
t = the actual temperature
0.05 = the correction factor.
For example, if the etch rate is 2.0 min to
remove 2.54 mm (0.1 mil) per surface at 294 K
(70 F), then the rate corrected to a standard
297 K (75 F) would be 2 + 0.05(70 75) = 2
0.25 = 1.75 min. The actual relationship is
probably a logarithmic function, but for
small temperature changes it was hoped
that a linear relationship would be accurate
enough. Sometimes our etch rate data give
us the feeling that our baths are actually
etching faster with a drop in bath temperature but this cant be. If the bath temperature changes by more than 2.8 K (5 F),
we re-measure the etch rate.
Another consideration is the chemistry
of the tank. How do changes in the bath
chemistry affect the etch rate? Again, we
have not been able to see any reliable
trends. However, our ability to make small
special mixes and to carefully control the
processing parameters in the use of such
mixes is very limited. We are not a research
lab and our equipment and time are very
limited. We are a job shop and the volume
of product going through any specific
etching tank is constantly changing. Another problem with chemistry is that some
customers use the same basic mixes, differing only in the percentages of the constituents. Of course, each thinks his is the
best and the only reliable mix. We do not
have our own lab operation, so chemical
analysis is handled by an outside vendor,
meaning we cant get instantaneous results. Our basic feeling is that chemistry
is, or at least should be, secondary to the
etch rate. We use some etching mixes that
over time develop contaminates (dissolved metal salts and so forth) that affect
both the etch rate and the etched part sur-
REFERENCES
ASTM, ASTM E 1417-05: Standard Practice for Liquid Penetrant Examination, West
Conshohocken, Pennsylvania, ASTM International, 2005.
APPENDICES
1: Thin, Flat Plate Tabs of Known Alloys
The equation in English units is derived
as follows. If the area around the edge of
the tab is small compared to the total surface area of the tab, then the area of the
edge may be ignored. Then, the total stock
removed during etching consists of two
small volumes, one from the top and one
from the bottom surface of the tab. Each
volume is the product of the tabs length
times its width (this product is its surface
area) times the thickness of the removed
stock. The total volume removed is twice
this volume. Then,
(A1)
V = AS ( 2 ) st
where
V = volume
AS = surface area
lst = stock loss per surface.
The weight (W) of this lost stock is the
product of the volume of stock removed
times the density (d) of the metal or,
(A2)
W = Vd
W = AS ( 2)( d ) st
W = W0 WF
(A5)
W = AS ( 2)( d ) st
W
= AS ( 2 )( d ) st
454
st =
W
454 ( AS )( 2)( d )
R=
W
454 ( AS ) ( 2 )( d ) (te )
R is in inches/surface/minute, W is in
grams, d is in pounds/cubic inch, AS is in
square inches (and is the area of one face of
the tab, not the total surface area on both
sides of the tab), and the etching time is in
minutes.
2: Thin, Flat, Non-standard Alloy Tabs
The accuracy of the microthickness
gage measurement does not greatly affect
this calculation, and if the tab is not of uniform thickness an average thickness based
upon thickness gage measurements at several spots on the tab may be used (we normally try to use five spots, the four corners
and the middle). The term W/W0 in the
equation, if multiplied to 100%, is the percent weight loss. The 2 is because the loss is
attributed to two surfaces on the tab. This
equation ignores the stock loss from the
edges of the tab. Consequently, it works
only for tabs with a large surface area to
thickness ratio. It makes no difference what
the shape of the tab is: square, rectangular,
round or any other shape, as long as the
surface area to thickness ratio is large
(greater than 100/1).
3: Thick, Flat, Non-standard Alloy Tabs
This equation comes from the following. For a tab where the thickness is not
small, the total volume lost must be used.
The volume lost in etching is the total surface area of the tab times the per surface
stock loss thickness (lst). If the dimensions of the tab are l for length, w for
width and h for height, then the total tab
volume is simply the product of these
three values or lwh. The surface area is
two times the sum of lw + hw + lh. Then
the ratio of the weight loss to the original
weight is equal to the ratio of the volume
loss to the original volume or,
(A9)
W ( lw + hw + lh )( 2) st
=
W0
hlw
( W ) hlw
( W0 ) ( 2 )( lw + hw + lh )
( W ) hlw
W0 ( 2)( lw + hw + lh)( te )
( ) ( l)
R=
W ( d )
st
=
te
4W0 ( te )
dl
= 0.943
2 d 2
dl +
4
l+
d
2
= 0.943
and
(A18)
l = 0.943l +
0.943d
2
Then
0.943d
2
(A19)
0.057l =
(A20)
l 0.943
=
= 8.3
d 0.114
4 ( st )
d
4
The ratio of the volume loss to original volume is equal to the ratio of the weight loss
to original weight. Then,
(A13)
(A15)
( )
(A21)
d2 l
W 4 st
=
W0
d
4
becoming
(A14)
( OD + ID )( st ) l
W ( d )
st =
4W0
OD 2 ID 2 l
(A22)
which equals
(A23)
4 ( OD + ID ) st
OD
( + ID) ( OD ID)
which equals
(A24)
4 st
( OD ID)
( ) + dl
2 d 2
st
4
W
(A25)
=
W0
d2
( )
4
(A26)
st =
( )
W d 2 l
d2
4W0 + dl
2
(A27)
R=
( W ) dl
2W0 ( d + 2l ) te