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SEMI D10-95 © SEMI 1995, 2003 3 material durable to the test media and condition s. (Wax, varnish, epoxy resins, adhesive tape, etc ., may be used.) 9 Procedure 9.1 Test Specimen Processing 9.1.1 Prepare cylindrical wide…
SEMI D10-95 © SEMI 1995, 2003 2
5.1.2 step measurement using profilometry — a
method to measure depths of etching by comparing the
differences in heights between etched and non-etched
parts of a specimen measured by profilometry or an
equivalent method.
5.1.3 weight loss method — a method to calculate
depths of etching by comparing differences in specimen
weights before and after the etch sequence.
6 Apparatus
6.1 For all chemical reactions, the following apparatus
shall be used.
6.1.1 Reaction Vessel
6.1.1.1 Material — Teflon or other suitably etch-
resistant material.
6.1.1.2 Shape and Capacity — Cylindrical wide-
mouthed sealable vessel, suitable for the size and
quantity of samples to be tested.
6.1.2 Thermostatically Controlled Shaker Bath or
Equipment
6.1.2.1 Shaking Stroke — 10 to 60 mm.
6.1.2.2 Shaking Frequency — 30–90/min., controllable
to ± 10/min.
6.1.2.3 Operating Temperature Range — 20 to 150° C,
controllable to ± 1° C.
6.1.3 Oven — Controllable to ± 10° over an operating
range of 50 to 200° C.
6.1.4 Desiccator — Room temperature, with sufficient
capacity and size for all samples to be tested.
6.1.5 Caliper — Per JIS B7507, or equivalent.
6.2 For the measurements, one of the following shall
be used.
6.2.1 Method A — Balance per JIS B7601, or
equivalent.
6.2.2 Method B — Profilometer per ISO 3274, JIS
B0651, or equivalent.
6.2.3 Method C — Haze measurement equipment with
integrating sphere per JIS K7105, or equivalent.
NOTE 1: It is ideal to use haze measurement equipment
which automatically measures total transmittance, diffuse
transmittance, and haze values.
7 Reagents and Materials
7.1 No specific requirement is defined for the reagents
and materials. As long as the test conditions are
reported with the result, any combination of chemical
reagents with any concentration can be used for the test.
The test conditions should reflect actual process
conditions which are specific for the Flat Panel Display
manufacturers. Some reagents suggested for the test are
provided in Related Information 1 as a reference.
7.2 This standard may involve hazardous materials,
operations, and equipment. This standard does not
purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
standard to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to use.
8 Sample Preparation
8.1 Prepare at least a specimen from a lot of the
substrates to be tested. The specimen is a rectangular
plate about 25 × 50 mm edge length for Methods A and
B, or 40 × 40 mm edge length for Method C.
8.1.1 If they are not already chamfered, specimen
edges and corners should be chamfered slightly to
remove chips and prevent cracking. If repeated tests are
expected, prepare an appropriate quantity of test
specimens.
8.2 Measure edge lengths of the test specimens, and
calculate total surface area, A:
A
=
(
L
×
W
×
2
)
+
{ (
L
+
W
)
×
T
×
2
)}
(
1
)
where
L
=
one edge length of test specimen in cm,
W
=
adjacent edge length of test specimen in cm,
T
=
thickness of test specimen in cm, and
A
=
total surface area of test specimen in cm
2
.
8.3 Clean all test specimens by a method appropriate
for the history of the material. The cleaning method
should not cause any corrosion. Clean the specimens by
an appropriate neutral or alkali detergent for
approximately 10 minutes using an ultrasonic bath.
8.3.1 Rinse them continuously in a stream of deionized
water, having a conductivity of less than 1 µ S/cm, for 1
minute using the ultrasonic bath. Finally, dry them.
8.4 Place all specimens on a clean heat resistant sample
holder. Dry the specimens at 140 ± 10° C for 30
minutes.
8.5 Place all specimens in a desiccator containing silica
gel or calcium sulfate and cool them, for a minimum of
1 hour, to room temperature.
8.6 If Method A will be used, weigh the test specimen
to 0.1 mg or 0.01 mg as required using the balance.
8.7 If Method B will be used, coat about a half portion
of each test specimen by an appropriate coating
SEMI D10-95 © SEMI 1995, 2003 3
material durable to the test media and conditions. (Wax,
varnish, epoxy resins, adhesive tape, etc., may be used.)
9 Procedure
9.1 Test Specimen Processing
9.1.1 Prepare cylindrical wide-mouthed sealable
vessels, sample holders, etc., made of materials which
do not react with the test medium under the test
conditions. Use a reaction vessel in which the test
specimen, while on the sample holder, is sufficiently
immersed in the required volume of test reagent.
9.1.2 Place the test specimen on the sample holder with
spacing of 1 to 2 cm between the test specimen and
bottom of the empty vessel. When a part of the
specimen is coated by protective material, position the
sample so that its coated portion faces down. The test
specimen may be leaned against the vessel wall if the
test is to be done in relatively brief or slightly corrosive
conditions, or in concentrated, extremely corrosive
media.
9.1.3 Pour the test reagents into the reaction vessel.
Volume of the test medium shall be 5 to 10 ml per cm
2
of specimen surface area. Preheat the test medium to
the specified test temperature.
9.1.4 Place the reaction vessel in the preheated shaker
bath with specified shaking stroke and frequency. Close
the reaction vessel loosely, and expose the specimen at
specified temperature for specified time.
9.1.5 At the completion of specified test time,
immediately remove the reaction vessel from the shaker
bath. Remove the test specimens from the reaction
vessel using soft forceps, and rinse the specimens
immediately by deionized water at appropriate
temperature. When the specimen temperature is high
following this process, rinse the specimens completely
with water of gradually decreasing temperature. Finish
it by deionized water at room temperature. Less caution
is required when the reaction temperature is low. A
synthetic rubber or plastic glove may be used instead of
forceps if sufficient care is taken. In all cases, the
surface of the test specimen shall not be scrubbed.
Never dry the test specimen during this operation.
Generation of cracks or chips due to thermal or
mechanical shocks should be avoided.
9.1.6 For Method B samples, remove coating by
appropriate non-corrosive method, and clean samples
again. In this case, residue from the coating material
should not contaminate the overall test specimen.
9.1.7 Place the test specimens on a clean heat-resistant
sample holder, and dry them at 140 ± 10° C for 30
minutes.
9.1.8 Place the specimens in the desiccator and allow
them to cool to room temperature.
9.2 Measurement Method
9.2.1 Method A (Weight Change)
9.2.1.1 Weigh the test specimen to 0.1 mg or 0.01 mg
as required, using the balance.
9.2.1.2 Calculate the areal weight change with the
following equation.
W
A
=
W
2
–
W
1
A
(2)
where
W
1
= the initial weight of the test specimen in mg,
W
2
= weight of the test specimen in mg after the test,
A = is surface area of test specimen in cm
2
,
as calculated in 8.2, and
W
A
= the areal weight change, in mg• cm
-2
.
NOTE 2: A negative result indicates a real weight loss, and a
positive result indicates a real weight gain.
9.2.1.3 Calculate penetration depth of corrosion, P, of
the test sample by the following equation.
P
=
10
W
A
D
(3)
where
W
A
= the areal weight change in mg• cm
-2
D = the density of the substrate material in mg
•
cm
-3
(see 9.2.1.4) and
P =
p
enetration depth in
µ
m
NOTE 3: A negative result indicates loss of material, and a
positive result indicates material gain.
9.2.1.4 When density of the materials is unknown, use
the value measured by the method described in ASTM
C729.
9.2.2 Method B (Profilometry)
9.2.2.1 Measure the height, H, in µ m, of the step
between the unetched (coated) section and the etched
(uncoated) section by a calibrated surface profilometer.
Trace length shall be between 2 and 4 mm, with the
boundary between the two sections located near the
center of the trace.
Repeat this measurement at least 3 times.
9.2.2.2 Calculate the average penetration depth P:
P =
H
1
+
H
2
+
•
•
•
••+
H
N
N
(4)
SEMI D10-95 © SEMI 1995, 2003 4
NOTE 4: A negative result indicates loss of material, and
positive result indicates material gain.
9.2.3 Method C (Surface Haze)
9.2.3.1 Measure total transmittance, Tt, and diffuse
transmittance, Td, and calculate the haze value from the
following expression:
H =
Td
Tt
× 100 (5)
where
Tt = total transmittance,
Td = diffuse transmittance, and
H = haze value in %.
10 Reporting Results
10.1 Report date and time of test, ambient temperature,
test operator, test conditions (reagent and concentration,
volume of the test medium, test temperature, test time,
stroke length, and frequency of shaking), specimen size
and total surface area, specimen cleaning method, and
the following:
10.1.1 Method A — The areal weight change (W
A
), the
initial weight of the specimen (W
1
), the density of the
substrate material (D), and calculated depth of
corrosion (P).
10.1.1.1 Method B — Penetration depth (P).
10.1.1.2 Method C — The average, maximum and
minimum value of total transmittance (Tt), diffuse
transmittance (Td), and haze value (H).
10.2 Remarks — In a typical test, one specimen is
immersed in an unused medium of specified volume in
a reaction vessel during a specified time. However, as
long as various conditions are described in the report,
even irregular methods may be allowed. Repetitive
usage of a medium may not markedly affect the result
when the test is done in relatively brief or slightly
corrosive conditions, or in concentrated, extremely
corrosive media.
11 Precision and Accuracy
11.1 Interlaboratory evaluation of these test methods is
planned to verify their suitability and reliability. Until
the results are established, use of this test method for
commercial transactions is not recommended unless the
parties to the test establish the degree of correlation that
can be obtained.
11.2 No standards exist against which any bias of this
test method can be evaluated.
NOTICE: SEMI makes no warranties or
representations as to the suitability of the standards set
forth herein for any particular application. The
determination of the suitability of the standard is solely
the responsibility of the user. Users are cautioned to
refer to manufacturer' s instructions, product labels,
product data sheets, and other relevant literature,
respecting any materials or equipment mentioned
herein. These standards are subject to change without
notice.
By publication of this standard, Semiconductor
Equipment and Materials International (SEMI) takes no
position respecting the validity of any patent rights or
copyrights asserted in connection with any items
mentioned in this standard. Users of this standard are
expressly advised that determination of any such patent
rights or copyrights, and the risk of infringement of
such rights are entirely their own responsibility.