Detecting Detrimental Intermetallic Phase in Duplex Austenitic/Ferritic Stainless Steels
Detecting Detrimental Intermetallic Phase in Duplex Austenitic/Ferritic Stainless Steels
Detecting Detrimental Intermetallic Phase in Duplex Austenitic/Ferritic Stainless Steels
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3.2 The sodium hydroxide etch test may be used to screen the cutting of the test specimen should be by a technique that
specimens intended for testing in Test Method B, Charpy prevents these effects. Alternatively, after the specimens are
Impact Test for Classification of Structures of Duplex Stainless cut, any material that may have been affected by high tempera-
Steels, and in Test Method C, Ferric Chloride Corrosion Test ture or deformation associated with the cutting should be
for Classification of Structures of Duplex Stainless Steels. removed by machining or wet grinding prior to testing.
3.3 Reference photomicrographs are provided to show clas- 5.2 For mill products, the specimen should allow for a
sifications of etch structures of a particular stainless steel type survey across the full thickness of the section or, in the case of
that are equivalent to acceptable or to possibly unacceptable a heavy section, a survey from one surface through the
performance for each practice. When Test Method A is used as mid-thickness of the section. The specimen shall include the
a screening test for Test Method B or Test Method C, mid-thickness.
specimens having acceptable etch structures need not be 5.3 For cast materials, the specimen shall be taken at
subjected to Test Method B or Test Method C. approximately 1/4T.
3.4 Table 1 indicates the applicability and acceptance crite- 5.4 Polishing—On all materials, cross-sectional surfaces
ria for Test Method A. When Test Method A is specified as an should be polished to a metallographic finish suitable for
acceptance test, specimens having other than acceptable etch examination at 4003 after etching. Specimens containing
structures may, at the option of the producer, be tested by Test welds should include base metal, weld heat–affected zone, and
Method B or Test Method C. weld metal. The area to be etched may be prepared by grinding
3.5 The steel shall be tested in the final solution heat treated to an 80- or 120-grit finish on a grinding belt or wheel without
condition or such other conditions as are agreed upon between excessive heating and then by polishing on successively finer
the producer and the user. emery papers, No. 1, 1⁄2 , 1⁄0 , 2⁄0 , 3⁄0 , and finer. Other methods
of polishing may be acceptable.
4. Apparatus
5.5 Etching Solution—The solution for etching is prepared
4.1 Source of Direct Current—Battery, generator, or recti- by adding 40 g of reagent grade sodium hydroxide (NaOH) to
fier capable of supplying approximately 15 V and 20 A. 100 g of distilled water.
4.2 Ammeter—Range from 0 to 30 A (see Note 1). 5.6 Etching Conditions—The polished specimen should be
4.3 Variable Resistance (see Note 1). etched at approximately 1 to 3 V dc, for 5 to 60 s (see Note 2).
4.4 Cathode—A cylindrical piece of conductive metal.
4.5 Large Electric Clamp, to hold the specimen to be NOTE 2—When etching is performed at 1 to 3 V dc with a platinum
etched. cathode for 5 to 60 s, any intermetallic phase is revealed by yellow, then
brown, staining, followed by staining of the ferrite.
4.6 Metallurgical Microscope, for examination of etched
microstructures to 400 to 500 diameters. 5.7 Rinsing—Following etching, the specimen should be
4.7 Electrodes of the Etching Cell—The specimen to be rinsed thoroughly in hot water and in acetone or alcohol,
etched is made the anode, and a cylindrical piece of metal as followed by air drying.
large as the specimen to be etched is made the cathode.
4.8 Electrolyte, sodium hydroxide (NaOH), reagent grade. 6. Classification of Etch Structures
NOTE 1—The variable resistance and ammeter are placed in the circuit 6.1 The etched surface shall be examined on a metallurgical
to measure and control the current on the specimen to be etched. microscope at 400 to 5003.
5. Preparation of Test Specimens 6.2 The etched cross-sectional areas should be examined
thoroughly by complete traverse of the full sample and across
5.1 For mill products, examination shall be made on a all zones such as weld metal, weld-affected zones, and base
longitudinal or transverse section. For cast products, examina- metal on specimens containing welds.
tion shall be made on a separately cast test coupon which was 6.3 The etch structures are classified into the following
heat treated in the same furnace load as the casting it types:
represents. Unless otherwise specified, selection of the test
6.3.1 Unaffected Structure (Fig. 1, Fig. 2)—The ferrite has
coupon size shall be at the discretion of the producer. Because
been etched without revelation of intermetallic phase. The
high temperature or mechanical deformation associated with
interphase boundaries are smooth.
particular cutting processes may alter the structure of the steel,
6.3.2 Possibly Affected Structure (Fig. 3, Fig. 4)—The
ferrite has been etched with isolated indications of possible
TABLE 1 Applicability and Acceptance Criteria for
Test Method A
intermetallic phase. The interphase boundaries may show a fine
waviness.
Grade Acceptable Nonacceptable 6.3.3 Affected Structure (Fig. 5, Fig. 6)—The indications of
Etch Structure Etch Structure an intermetallic phase are readily revealed before or simulta-
S31803, unaffected possibly affected neously with the staining of the ferrite during etching.
S32205, structure (Fig. 1, structure (Fig. 3,
S32750, J92205 Fig. 2) Fig. 4) 6.3.4 Centerline Structure (Fig. 7)—An intermetallic phase
affected structure is observed as a continuous or semi-continuous phase in the
(Fig. 5, Fig. 6) mid-thickness region of the product, with or without the
centerline structure
(Fig. 7) affected structure outside of the mid-thickness region, indica-
tive of segregation.
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distances as a function of the local thermal cycle. In such cases, 15.1 Before testing by the ferric chloride corrosion test,
the placement of the V-notch may affect the measured result specimens of the steel may be given a rapid screening test in
significantly. accordance with the procedures of Test Method A, Sodium
Hydroxide Etch Test for Classification of Etch Structures of
12. Procedure Duplex Stainless Steels. Preparation, etching, and the classifi-
12.1 Perform the test in accordance with the procedures cation of etch structures are described therein. Specimens
described in Test Methods and Definitions A 370. having an etch structure described as Unaffected Structure in
12.2 Unless otherwise specified, perform the test at −40°F Test Method A will be essentially free of detrimental effects on
(−40°C). pitting corrosion resistance as related to the formation of an
intermetallic phase. Other mechanisms for loss of pitting
13. Acceptance Values and Retests resistance may occur independently but are beyond the scope
of this test method. Specimens showing Unaffected3 Structure
13.1 Unless otherwise specified, the acceptance criteria
in Test Method A are acceptable with respect to the absence of
shall be as given in Table 2.
intermetallic phases and need not be tested by the ferric
13.2 If a test specimen shows a value below the specified
chloride corrosion test as described in Test Method C. All
minimum, one retest of two specimens is permitted. For
specimens having other than Unaffected Structure shall be
acceptance, both retest specimens shall show a value at or
tested by the ferric chloride corrosion test.
above the specified minimum value.
13.3 A product that has failed the Charpy impact test may,
16. Apparatus
at the option of the producer, be given a full anneal and
retested. 16.1 Glass Beakers, 1000-mL, tall-form, or Erlenmeyer
flasks, 1000-mL, wide neck, or 50-mm (2-in.) diameter test
TEST METHOD C—FERRIC CHLORIDE tubes, or other suitable glass containers.
CORROSION TEST FOR CLASSIFICATION OF 16.2 Glass Cradles (Fig. 8)—The dimensions of the cradle
STRUCTURES OF DUPLEX shall be restricted to those that will permit its passage through
STAINLESS STEELS the test container opening, a diameter of approximately 40 mm
(1.6 in.) in the case of the Erlenmeyer flask.
14. Scope 16.3 Water or Oil Bath, constant temperature.
14.1 This test method describes the procedure for conduct-
17. Ferric Chloride Test Solution
ing the ferric chloride corrosion test for detecting the presence
of detrimental intermetallic phases in duplex stainless steels. 17.1 The test solution is prepared by dissolving 100 g of
The presence or absence of corrosion attack in this test is not reagent-grade ferric chloride, FeCl3·6H2O, in 900 mL of
necessarily a measure of the performance of the material in distilled water (approximately 6 % FeCl3 by weight). The
other corrosive environments; in particular, it does not provide solution is filtered through glass wool or filter paper to remove
a basis for predicting resistance to forms of corrosion not insoluble particles.
associated with the precipitation of intermetallic phases (see 17.2 The pH of the test solution shall be adjusted to
Note 4). approximately 1.3 prior to beginning the test by the addition of
14.2 The ferric chloride corrosion test may be used to HCl or NaOH, as required.
evaluate mill products, provided that it is possible to obtain a
specimen of relevant location and geometry. 18. Test Specimen
14.3 Table 3 indicates the applicability and acceptance 18.1 Various shapes and sizes of test specimens may be
criteria for Test Method C. used. For flat products, a specimen should be approximately 25
NOTE 4—Although this test method uses some equipment and proce- by 50 mm (1 by 2 in.) by thickness. The full thickness of the
dures similar to those of Test Method G 48, this test method should not be product should be included. In the case of heavier sections, the
confused with Test Method G 48. This test method does not determine the specimen may be taken in a perpendicular orientation with
critical pitting temperature or test for the suitability for use in a particular dimensions of approximately 6 by 25 mm (1⁄4 by 1 in.) by
environment. This test method is designed solely for detection of the thickness. In very heavy sections, the thickness dimension of
precipitation of detrimental intermetallic phases in duplex stainless steels. the specimen may be cut so that one half to two thirds of the
15. Rapid Screening Test product thickness is tested.
18.2 Other product forms may be cut for test specimens
convenient for testing, provided that the specimen exposes
TABLE 3 Applicability and Acceptance Criteria for surfaces representative of the full thickness of the product.
Test Method C 18.3 After the specimens are cut, any material that may have
Grade Condition Test Maximum Acceptable been affected by high temperature or deformation associated
Temperature Corrosion Rate Calculated with the cutting should be removed by machining or grinding
from Weight Loss
prior to testing.
S31803, S32205 base metal 25°C (77°F) 10 mdd 18.4 For mill products, all surfaces of the specimen should
weld metal 22°C (72°F) 10 mdd
S32750 base metal 40°C (107°F) 10 mdd be polished to a uniform finish at least equal to a 120-grit
finish, or finer. Wet polishing is preferred. If used, dry
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polishing should be performed slowly to prevent overheating. Maintain the test temperature throughout the test. Cover the
Sharp edges of the specimen should be rounded, with care test container with a watchglass during the test period. Unless
taken to remove all burrs. otherwise specified, the test period shall be 24 h.
18.5 The surface of the specimen shall not be chemically 19.6 At the end of the 24-h test period, remove the specimen
passivated by treatments such as nitric, citric, or phosphoric from the solution, rinse with water, scrub with a soft bristle
acid, or pickled by treatments such as nitric hydrofluoric acid, brush under running water to remove corrosion products,
subsequent to grinding the surface. dipped in acetone or alcohol, and dried in air. Ultrasonic
18.6 For other than mill products, testing of a specimen with cleaning is a permitted alternative when there are corrosion
the surface in the as-fabricated condition may be relevant to the products that are difficult to remove.
application. 19.7 Weigh the specimen to 0.001 g or better and reserve for
18.7 The dimensions of the specimen are measured, and the examination.
total exposed surface area is calculated.
18.8 The specimen should be cleaned with magnesiumoxide 20. Acceptance Values
paste or equivalent, rinsed well with water, dipped in alcohol or 20.1 The corrosion rate is calculated in accordance with the
acetone, and air dried. The specimen shall be weighed to the weight loss and total surface area (see Note 5). Unless
nearest 0.001 g or better. It should be stored in a desiccator otherwise specified, the calculated corrosion rate shall not
until ready for testing. exceed 10 mdd (see Note 6).
19. Procedure NOTE 5—The corrosion rate is calculated in accordance with the
following: corrosion rate (mdd)
19.1 Perform the test using ferric-chloride solution with a = weight loss (mg)/[specimen area (dm2) 3 time (days)]
volume at least the larger of 150 mL or 20 mL/cm2(125 NOTE 6—It is probable that corrosion will occur by pitting when it does
mL/in.2) of the specimen surface area. Fill the test container occur. The calculation of a uniform corrosion rate would be an inappro-
with the required volume, transfer to the constant temperature priate method of expressing the pitting corrosion. However, in this case,
bath, and allow to come to equilibrium at the desired test the calculation of a corrosion rate is used primarily to normalize the
temperature. weight loss for the variety of specimen sizes and shapes permitted.
19.2 Unless otherwise specified, the test temperature for 20.2 If the specimen shows a corrosion rate in excess of 10
wrought products of S31803 and S32205 shall be 25°C (77°F), mdd, one retest on two new specimens from the same product
maintained within an accuracy of 61°C (2°F) during the test. is permitted. No retest specimen shall exhibit a corrosion rate
19.3 Unless otherwise specified, the test temperature for in excess of 10 mdd.
S31803 and S32205 products containing weldments shall be 20.3 At the option of the producer, a product that has failed
22°C (72°F), maintained within an accuracy of 61°C (2°F) the ferric-chloride corrosion test may be given a full anneal and
during the test. retested.
19.4 Unless otherwise specified, the test temperature for
S32750 products shall be 40°C (104°F), maintained within an 21. Precision and Bias
accuracy of 61°C (2°F) during the test. 21.1 No statement is made concerning either the precision
19.5 Place the specimen in the glass cradle and immerse in or bias of Test Methods A, B, or C for detecting the presence
the test solution once the temperature has been established. or absence of detrimental intermetallic phases in wrought
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duplex stainless steels because the results state merely whether 22. Keywords
there is conformance to the criteria for success specified in the
22.1 duplex; intermetallic; stainless steels
procedure.
APPENDIXES
(Nonmandatory Information)
C Mn P S Si Cr Ni Mo N
0.023 1.44 0.022 0.001 0.49 22.3 5.60 3.13 0.182
Heat Treatment Condition CVN Impact Energy (ft-lb at −40°F (J at −40°C))B Critical Pitting Temperature (°C)C
Longitudinal Transverse
Mill annealed 185 (251) 127 (172) 35
1950°F (1066°C) + WQ 196 (266) 123 (167) not tested
1950°F (1066°C) + WQ + 5 min, 1550°F 42 (60) 25 (34) 20
1950°F (1066°C) + WQ + 10 min, 32 (43) 16 (22) 15
1550°F
1950°F (1066°C) + WQ + 15 min, 26 (35) 12 (16) not tested
1550°F
1950°F (1066°C) + WQ + 20 min, 21 (28) 9 (12) 15
1550°F
1950°F (1066°C) + air cool 198 (268) 133 (180) not tested
1950°F (1066°C) + slow cool 80 (108) 88 (119) 30
A
Davison, R. M., and Redmond, J. D., Paper No. 302, NACE Corrosion 91, 1991.
B 3
⁄8-in.
(9.5-mm) plate, three-quarter size Charpy specimen.
C
CPT per Test Method G 48, Test Method A.
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SUMMARY OF CHANGES
Committee A01 had identified the location of selected changes made to this standard since the last issue,
A 923–01e1, that may impact the use of this standard. (Approved Oct. 1, 2003).
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