Exfoliation

Donald O. Sprowls; 1revised by Kevin R. Coope/

E V A L U A T I O N OF E X F O L I A T I O N CORROSION
HISTORICALLY,exfoliation corrosion problems have been associated principally with high-strength aluminum alloys used in aircraft construction and by the U.S. Department of Defense. This chapter, therefore, will deal mainly with test procedures developed for alloys of aluminum.

Basic Principles
Exfoliation is defined in ASTM G 15, Terminology Relating to Corrosion and Corrosion Testing, as a form of "corrosion that proceeds laterally from the sites of initiation along planes parallel to the surface, generally at grain boundaries, forming corrosion products that force metal away from the body of the material, giving rise to a layered appearance." An example is shown in Fig. 1. For a metal to exfoliate, a highly directional grain structure is necessary along with electrochemically active corrosion paths parallel to the metal surface. The severity of exfoliation in susceptible materials is influenced to a m a r k e d degree by environmental conditions []. Figure 2 shows the broad range of behavior of a particular material in different types of atmospheres [2]. Taking an example from service, it is recognized that forged m o t o r truck wheels made of an a l u m i n u m copper alloy (AA2024-T4) give corrosion-free performance for many years in the w a r m dry climates of the southern and western United States, but they exfoliate severely in only one or two years in the northern states where deicing salts are used on the highways during the winter months [3].

FIG. 1--Three degrees of resistance to exfoliation produced by variations in heat treatment of a AA2024 alloy extruded 13-mm thick bar. 1"/10 and 1"/2 are designations for the interior machined test surfaces (refer to the subsection, Test Specimens, in this chapter). The stepped specimens were exposed for 55-61 months in an industrial environment at Brookfield, IL [3]. (Reprinted with permission from EMAS, Ltd., U.K.)

Susceptible Metal Alloy Systems

Aluminum
Exfoliation corrosion of a l u m i n u m is an industrial problem chiefly with the higher strength AA2XXX, AA5XXX, and AA7XXX alloy wrought products in which the grains of metal are elongated during manufacture. The alloy typically is in a t e m p e r that is susceptible to d o m i n a n t intergranular corrosion. The severity of the exfoliation will depend not 1Consultant; retired, Alcoa Technical Center, Alcoa Center, PA 15069. ZResearch Scientist, Luna Innovations, Inc., 705-A Dale Ave, Charlottesville, VA 22903.

only on the extent to which the grains have been elongated, but also to the continuity of the anodically active paths and to the environmental conditions. These materials also have a low resistance to environment-assisted cracking when stressed in the short transverse direction, and the two phen o m e n a may be mutually accelerating when short transverse tension stresses are involved [3,4]. A more detailed discussion of the importance of the macrostructure of the exfoliation test specimens is given in Refs 3-4 and in the ASTM G 112, Standard Guide for Conducting Exfoliation Corrosion Tests in Aluminum Alloys. Exfoliation also can occur in the directional fragmented grain structure of severely cold-rolled products of certain lower strength strain-hardening alloys of the AA3XXX and

266

CHAPTER 22--EXFOLIATION 2 6 7
i
1

1RY$1VIR! (IO) I SIi II[i (IC)

!

PL

NDffH

8ROOKFtiLD

! AIRCRAFI6RRIIIf

POINT DAITONA E.iACH

An experimental magnesium-base alloy sheet containing 14 % lithium and 2 % a l u m i n u m was reported to have experienced intergranular layer attack similar to the exfoliation of aluminum-copper alloys [8].
Test Procedures for Aluminum Alloys

MODEIATI ( i l l

i
I SLIGHT(llll I PttlLADILPHII MONTREAl

Relation to Service Conditions

Laboratory corrosion tests for exfoliation corrosion susceptibility are a necessary tool for research and quality control engineers; however, the validity of such accelerated tests depends on their relationship to realistic service conditions and their sensitivity to various degrees of susceptibility. The tests must be discriminating and yet not so severe as to be unrealistic. For the majority of engineered structures, exposure to outdoor atmospheres provides a baseline that is representative of m a n y service conditions, except for structures that are subjected to unusual chemical environments. Experience has shown that seacoast conditions are more corrosive to a l u m i n u m alloys than inland urban and industrial conditions (see Fig. 2), and seacoast atmospheric exposure tests have been particularly useful for the validation of accelerated exfoliation tests [9]. Accelerated tests do not precisely predict long-term corrosion behavior; however, answers are needed quickly in the development of new materials. For this reason, accelerated tests are used to screen candidate alloys before conducting atmospheric exposures or other field tests. They also are used for production control of exfoliation-resistant heat treatments for the AA2XXX, AA5XXX, and AA7XXX aluminum alloys. ASTM has standardized several laboratory tests for susceptibility to exfoliation corrosion in recent years.

PI~IHG (I) I 14 1 II I 60

II

41

i XllOilJit ItMI Ill MOHTI~$

FIG. 2--Influence of environmental conditions on the exfoliation corrosion of a material with a low resistance to exfoliation. AA2124-T351 rolled 51-mm thick plate rated ED in the standard EXCO test, ASTM G 34 [2].

AA5XXX families. The anodic corrosion path in these materials is not in the grain boundaries, but rather it is in deformation bands of aluminum or Al-Mg solid solutions interspersed between relatively cathodic strata of Al-Mn and/or Al-Cr phases depending on the composition of the alloy and the thermal history during processing. Although this form of intragranular exfoliation corrosion rarely presents industrial problems, it is possible, however, as a result of inappropriate ingot homogenizing thermal treatments, to encounter exfoliation susceptibility of severely cold-rolled products in aggressive environments [3]. Severe exfoliation has been reported with graphite/alum i n u m metal matrix composites in marine environments [5]. Localized corrosion along wire-wire and wire-foil diffusion bonds resulted in disbondment of the precursor wires and a l u m i n u m foils. See also the discussion by Hihara on corrosion of metal-matrix composites in Section VI of this manual.

Selection of Appropriate Test Procedures

Selection of the most appropriate test procedure(s) depends on the type of alloy to be tested, the anticipated service environment, and the purpose of the test. W h e n testing an experimental alloy or product form, one would normally select a procedure known to be applicable to a similar commercial alloy. The investigator is cautioned, however, that even a small difference in alloy chemistry or changes in processing method can markedly affect the resistance to exfoliation of the new material and the appropriateness of a specific test method. Therefore, when investigating a new type of material, it is advisable to initially use more than one laboratory test procedure and compare the test results. If they do not agree, determine which procedure is the most applicable by conducting a seacoast atmospheric exposure. It is unrealistic to expect a single laboratory test to be applicable to all materials and purposes [2]. The known applicability of each of the standardized test procedures is discussed below. These several tests, developed by the producers of alumin u m alloys and U.S. Government laboratories, have been used mainly for research and alloy development. Certain test procedures are also used for production control of exfoliation-resistant materials. If they are considered for quality assurance purposes, however, limits of acceptable performance should be the subject of an agreement between concerned parties.

Other Metals
Although exfoliation corrosion has been reported in a few other metal systems, incidents of this form of corrosion are few and presumably not of practical importance. Therefore, no attempts have been made to develop and standardize specific tests for detecting susceptibility to exfoliation for these other metals. The following notes from published literature m a y be of interest to some readers. "A peculiar form of attack (exfoliation) has been reported with 80/20 or 70/30 cupro-nickel tubes in high-pressure feedwater heaters. A severe form of general corrosion on the steam side consists of an exfoliating scale mainly of a mixture of metal oxides in the same proportions as the metals present in the alloy. The attack has only been observed on tubes heated intermittently and the mechanism is o b s c u r e . . , materials which are immune are copper or 90/10 cupro-nickel" [6], Wrought iron, produced by piling several plates on top of one another, subjected to heat, and passed through a rolling mill, develops zones that behave differently from one another when subjected to corrosive conditions. Evans considers this zonal corrosion of wrought iron to have much in common with the layer corrosion (exfoliation) of light alloys [7].

268

C O R R O S I O N TESTS AND STANDARDS MANUAL

ASTM G 66, Method for Visual Assessment of Exfoliation Corrosion Susceptibility of AA5XXX Series Aluminum Alloys (ASSET Test), describes a procedure for the continuous immersion exfoliation testing of AA5XXX alloys containing 2.0 % or more magnesium. Specimens are i m m e r s e d for 24 h at 65C (150F) in a solution containing 1.0 M a m m o n i u m chloride, 0.25 M a m m o n i u m nitrate, 0.01 M a m m o n i u m tartrate, and 0.09 M hydrogen peroxide. This method provides a reliable prediction of the exfoliation corrosion behavior of AA5XXX alloys in marine environments including seawater [17,18]. This test is useful for alloy development studies and quality control of mill products such as sheet and plate. ASTM G 34, Method for Exfoliation Corrosion Susceptibility in 2XXX and 7XXX Series Aluminum Alloys (EXCO Test), provides an accelerated test for AA2XXX and AA7XXX a l u m i n u m alloys by continuous immersion of test materials in an aqueous solution containing 4 M sodium chloride, 0.5 M potassium nitrate, and 0.1 M nitric acid at 25C (77F) (with a starting pH of 0.4 rising to 3.2 during the first 7-20 h of exposure) for periods of 24-48 h. "This test method is primarily used for research and development and should not be construed as a method for quality acceptance." Seacoast atmospheric exposures of six to twelve years have proven the EXCO test to be a reliable indicator of service performance for the following alloys used in an interlaboratory testing program: AA2024 and AA2124 in T351 and T851 tempers; AA7075 in T651, T7351, and T7651 tempers; and AA7178 in T651 and T7651 tempers [14,15,19]. The EXCO test has been reported as being too aggressive and not representative of outdoor atmospheres for more recently developed alloys, such as AA2219, AA2419, and AA2519 in the T851 tempers [20], for aluminum-lithium alloys AA2020, AA2090, AA2091, and AA8090 in both asquenched and artificially aged tempers [10,11,15, 21 ] and for AA7050 and AA7150 in the T7XX type tempers [21]. The problem is that EXCO test specimens of these materials quickly become covered with corrosion products from general attack making it difficult to visually distinguish the general attack from genuine exfoliation. The result is that test specimens frequently have been rated as being overly susceptible to exfoliation (EA or EB) whereas little or no exfoliation occurred in extended seacoast exposures. Metallographic examination is often required to establish a true rating for these relatively resistant materials. Similar problems related to the severity of the EXCO test have also been experienced with copper-free AA7XXX alloys and wrought products of powder metallurgy AA7XXX alloys. This sort of difficulty contributes to variability in the assessment of the exfoliation. Modified EXCO test solutions not yet standardized that cause less general corrosion have been investigated with promising results in that the reduced general attack favored positive identification of the exfoliation and more accurate estimation of the intensity of it without the necessity of metallographic examination. One approach was to reduce the acidity to pH 3.2 and to add a small amount of a l u m i n u m ion while keeping the molarities of chloride and nitrate the same. A 96 h exposure to this modified EXCO solution appears more capable of reliably predicting exfoliation performance in seacoast environments and of distinguishing

Salt Spray (Fog) Tests--Three different cyclic acidified salt spray tests have been widely used for exfoliation testing in the a l u m i n u m and aircraft industries. These are described in Annexes A2, A3, and A4 in ASTM G 85, Practice for Modified Salt Spray (Fog) Testing. The three practices are not equivalent, and the user should determine which one is best suited for the alloy and application under investigation. The following notes were taken from the ASTM G 112, which contains additional details regarding their usage:
Annex A2 describes a cyclic salt spray test (MASTMAASIS) that uses a 5 % sodium chloride solution acidified to pH 3 with acetic acid in a spray c h a m b e r at a temperature of 49C (120F). This test is applicable for exfoliation testing of AA2XXX (dry-bottom operation) and AA7XXX (wet-bottom operation, that is, with approximately 25 m m (1 in.) of solution present in the bottom of the test chamber) a l u m i n u m alloys with test duration of 1-2 weeks. Results with AA7075 and AA7178 alloys in various metallurgical conditions have been shown to correlate well with results obtained in a seacoast atmosphere (four-year exposure at Point Judith, RI) [9]. The exfoliation behavior of lithium-containing a l u m i n u m alloys AA2090-T8, AA2091-T3 and T8 and AA8090-T8 obtained with dry bottom MASTMAASIS agree with marine environments [10-12]. There is no record of this test being unrealistically aggressive, that is, causing exfoliation of a material that did not exfoliate at the seacoast. Annex A3 describes a cyclic salt spray test (SWAAT) that uses a different exposure cycle and a 5 % synthetic sea salt solution acidified to pH 3 with acetic acid in a spray c h a m b e r at a temperature of 49C (120F). This test is applicable to the production control of exfoliation-resistant tempers of the AA2XXX, AA5XXX, and AA7XXX alumin u m alloys. Wet-bottom operating conditions are recomm e n d e d with test durations of 1-2 weeks [13,14]. Annex A4 describes a salt-sulfur dioxide (SO2) spray test that uses either 5 % sodium chloride or 5 % synthetic sea salt solution in a spray c h a m b e r at a temperature of 35C (95F). The spray may be either cyclic or continuous, which, along with the type of salt solution and test duration, is subject to agreement between the purchaser and the seller. This test, which was developed to simulate the hostile environment on the deck of an aircraft carrier, reproduces in two weeks the exfoliation attack on susceptible AA2XXX and AA7XXX a l u m i n u m alloys that occurs on a c a r d e r in about eight months [2]. However, the sulfur dioxide salt spray does not well reproduce the exfoliation behavior of a l u m i n u m lithium alloys AA2020, AA2090 and AA8090 observed when exposed to the environment encountered on aircraft carriers [15,16].

Immersion Tests--Continuous total immersion tests were developed more recently to provide simpler, rapid, and more reproducible test methods than the salt spray tests. Although plain sodium chloride solutions do not cause exfoliation during the desirable short periods of immersion, formulations of chloride-nitrate solutions were found that produced severe exfoliation of highly susceptible alloys of various types in only one to four days. Optimum test conditions differed for separate alloy families [1].

CHAPTER 2 2 - - E X F O L I A T I O N
between various commercial tempers of AA7075, AA7050, and AA7150 alloys. With a 48 h exposure at a slightly elevated temperature of 52C (125F) this modified solution also reflected accurately the performance in a seacoast atmosphere of alloys AA2024 and aluminum-lithium AA2090, in both the T3 and T8 type tempers [21]. Another approach involved the addition of a corrosion inhibitor. Sinyavsky et al. [4], using an addition of 10 g/L potassium dichromate to the standard EXCO solution, reported that the exfoliation trends were the same as in the standard solution for all of the alloys examined (AA2124-T3, T8; AA2618-T6; and AA7175-T6, T76, T73), and because of less general corrosion the exfoliation was easier to identify and to assess in the inhibited solution. Additional testing of these and other possible modifications, including interlaboratory comparisons, is needed to verify the promising results noted. An ideal modification would hopefully work well with a variety of alloys and be shown to have good reproducibility before it is proposed as a new standard test method. Historically, various investigators in Europe have used hydrochloric acid-potassium dichromate solutions for testing the exfoliation susceptibility of all types of aluminum alloys. An example is the Russian Standard GOST 9.904-82, Aluminium Alloys: Methods of Accelerated Exfoliation Corrosion Testing [22]. It should be noted, however, that hexavalent chromium (Cr 6) solutions are considered undesirable for health and environmental considerations and have been prohibited in some countries.

269

The test surface is either the as-fabricated surface or some other specified plane(s). Interior planes typically used are: (a) T/10 = 10 % of the thickness removed (this is representative of a minimal cut to obtain a flat surface free of traffic marks), (b) T/4 -- quarter plane, 25 % of the thickness removed, or (c) T/2 = midplane, 50 % of the thickness removed. These interior planes are representative of many of the exposed surfaces of parts machined for aircraft components and they also may expose regions in the grain structure with the highest likelihood of exfoliation susceptibility. When removing test specimens from extrusions and die forgings, locations where the grain structure is variable, such as underneath flanges and ribs, should be avoided. The roughness parameter of machined test surfaces, R a, should not exceed 2.5 gm, unless it is required to simulate an as-manufactured surface condition. Edges of the test specimens should preferably be sawed or machined. If specimens are obtained by shearing, the plastically deformed edges should be dressed by machining, sanding, or filing to a depth equal to the specimen thickness to remove residual short transverse tensile stresses. With very susceptible materials stress-corrosion cracks parallel to the surface m a y initiate in the edges.

Test Duration
The length of time to develop exfoliation in a susceptible material can vary appreciably depending on the degree of directionality of the grain structure and the heat treatment of the test specimen. Therefore, it can be helpful when the purpose is to compare various items in a series to examine and assign exfoliation ratings after increasing periods of exposure during the test.

Electrochemical and Conductivity Tests--These are useful techniques that indicate expected exfoliation corrosion performance but do not actually produce corrosion. Both the electrochemical corrosion potentials and the electrical conductivity are secondary characteristics that relate to the metallurgical condition of the metal and must be correlated to actual exfoliation corrosion tests. Several researchers experimented with electrochemically driven techniques. Budd and Booth used a potentiostatic approach [23]. Others have tried impressed current tests. Although both appeared promising, these procedures did not lend themselves to the multiple testing required for production control of heat treatment. Neither type of test has been standardized to date. A useful measure of the degree of improvement in exfoliation resistance of the overaged T7X tempers for AA7075 and similar copper-containing AA7XXX alloys is available from a correlation of the decrease in yield strength combined with the increase in electrical conductivity as the alloy is overaged [3]. Such lot acceptance criteria are included in certain specifications for the T7X t e m p e r products of these alloys. Test Specimens
Specimens m a y be of any practical size or shape. However, it is advisable not to use too small a specimen since visual examination is the key evaluation method. It is reco m m e n d e d that flat specimens at least 50 m m by 75 m m in size and full section thickness be used with the specimen length oriented in the direction of principal deformation of the mill product. Larger sized panel specimens are desirable for salt spray testing or outdoor exposures.

Accelerated Tests--Standard tests generally are conducted for the r e c o m m e n d e d exposure period. However, if no appreciable exfoliation is observed on a new alloy or temper, the period may be doubled. If this still does not produce significant exfoliation it generally can be concluded that the material is not susceptible to exfoliation in that test medium. Outdoor Tests--Past experience has shown that materials that are very prone to exfoliation in service conditions will show marked exfoliation within four years of exposure at severe outdoor sites, such as seacoast and certain highly industrialized urban areas. If test space is limited, specimens surviving this length of exposure at outdoor sites known to cause exfoliation can be terminated and considered "not highly susceptible." However, some investigators now have programs of 20 or m o r e years duration showing that exposures exceeding four years still may discriminate between materials with the "better and best" resistance. Evaluation o f Test Results
One of the problems with evaluating exfoliation corrosion is the lack of a generally accepted numerical measure of the corrosion damage. Mass loss is a poor indicator of exfoliation behavior because the degree of attack can be spatially nonuniform. Delaminated layers that are not completely detached from the specimen also complicate accurate mass loss determination. Cross-sectional metallographic examination can add valuable information on the degree and mode of attack, but is time consuming and no relative ranking system has been devised.

270

CORROSION TESTS AND STANDARDS MANUAL

Therefore, the usual practice is to inspect the specimens and to assign visual ratings with reference to standard photographs illustrating four degrees of severity as in ASTM G 34 and G 66. To choose a rating, the inspector must make a judgment, and herein lies the main source of variability in the test results from the relatively uncomplicated immersion tests. It is often desired for the record to make photographs of the exposed test specimens as well as to rate t h e m using the standard photographs.

Classification of Exfoliation--The following classifications (Table 1) are recommended when reporting the visual ratings of corroded test specimens by comparison with standard photographs in Figs. 3-8 (after ASTM G 34, G 66, and G 112):
TABLE 1--Classifications for corroded test specimens.
Classification Rating

No appreciable attack Pitting General Exfoliation

N p G EA, EB, EC, ED

FIG. 4--Examples of exfoliation rating EA (superficial): tiny blisters, thin slivers, flakes, or powder, with only slight penetration into the metal (reprinted from ASTM G 34).

(a) N - - N o appreciable attack: surface m a y be discolored or superficially etched.

(b) P--Pitting: discrete pits, sometimes with a tendency for undercutting and slight lifting of metal at the pit edges (Fig. 3a). (c) G--General: fairly uniform corrosion with accumulation of powdery corrosion products; the basic type of attack may be either pitting or intergranular. (d) EA to ED--Exfoliation: visible separation of the metal into layers manifested in various forms such as blisters, slivers, flakes, fairly continuous sheets, and sometimes granular particles resulting from disintegration of thin layers of metal; attack m a y be wide-spread or localized. Various degrees of exfoliation with increasing area, penetration, and loss of metal are shown in Figs. 4-8.

FIG. 3--Metallographic sections illustrating two different types of attack (reprinted from ASTM G 34): (a) undermining pitting that may from the surface give the appearance of the beginning of exfoliation (Keller's Etch: 100x); (b) exfoliation resulting from rapid lateral attack of selective grain boundaries or strata forming wedges of corrosion product that force layers of metal upward giving rise to a layered appearance (Keller's Etch: 100x).

Inspection of Specimens--After discontinuation of the exposure, performance should be rated while the specimens are still moist, taking into account all corrosion products adhering to the metal surface or lying on the bottom of the test container. Photographs m a y be advisable at this stage. If in some cases it is impossible to positively distinguish mild forms of exfoliation from general corrosion it m a y be helpful to chemically clean the specimens by soaking them in concentrated nitric acid (70 % HNO 3, specific gravity 1.19) at room temperature for only a few minutes, just long enough to dissolve corrosion products without dislodging layers or flakes of true exfoliation, followed by gently rinsing again with tap water. When the presence of exfoliation is still questionable because of remaining powdery deposits or if real exfoliation actually was removed, metallographic examination of a cross section of the corrosion will be required to determine the correct rating (Fig. 3). The purpose is to avoid giving a specimen an unrealistic visual rating of EA or EB when there is no microscopic evidence of actual delamination or conversely giving an erroneous visual rating of P or G when the evidence of real exfoliation was destroyed. Experience has shown that material that is roughened and exhibiting a loosely adherent powdery deposit in the standard EXCO test does not exfoliate during exposure of five years in the seacoast atmosphere at Point Judith, RI [24].

CHAPTER 22

EXFOLIATION 271

FIG. 5~Examples of exfoliation rating EB (moderate): notable layering and penetration into the metal (reprinted from ASTM G 34).

FIG. 7--Examples of exfoliation rating ED (very severe): similar to EC except for much greater penetration and loss of metal (reprinted from ASTM G 34).

FIG. 6~Examples of exfoliation rating EC (severe): penetration to a considerable depth into the metal (reprinted from ASTM G 34).

FIG. 8~Examples of four degrees of exfoliation corrosion, EA-ED of several AA5XXX alloys (reprinted from ASTM G 66).

When a test specimen appears to be borderline, choose the rating indicating higher susceptibility. And when exfoliation occurs at isolated sites, rate the worse condition observed. Care must be taken not to over interpret the inherently subjective ratings. As an example, the difference in the a m o u n t of attack between samples rated on the severe end of the EA range and mild end of the EB range is small such that samples receiving those designations may not in fact have different exfoliation susceptibilities. In addition, material with exfoliation resistance between highly susceptible and highly resistant can be difficult to rate visually, as highlighted in an interlaboratory test program that used two non-commercial heat treatments of AA7075 with different levels of resistance (see ASTM G 34-01 section 14). Results from this round-robin test p r o g r a m indicate that the visual rating system gives consistent classification designation for highly susceptible samples but may produce a large a m o u n t of variation for moderately resistant tempers. Experience also suggests that the visual rating system produces more consistent results for highly resistant material than it does for aging conditions of moderate to low resistance.

Another approach based on visual examination has been used in the former Soviet Union [4,22]. Three rating criteria are used to express the degree of damage on a scale of 1-10: (a) Percent area of swelling and exfoliation of test surface, (b) Maximum diameter in m m of swellings (blisters) on test surface, and (c) Percent length of cracking in specimen perimeter (edges). The material is evaluated by calculating the arithmetic mean of these three criteria. Although a numerical result is generated, it is calculated from subjective visual estimates and is more complicated. A classification system for exfoliation attack based on an objective and quantitative rating method and criteria would be a beneficial alternative to the existing subjective visual rating method.

Test Procedures for Other Metals

Exploratory investigations of the possible susceptibility to exfoliation corrosion of alloys of other metals would be advisable if wrought mill products have highly directional grain structures and if it is known that they may be susceptible to intergranular

272 CORROSION TESTS AND STANDARDS MANUAL

or lameHar corrosion. It is r e c o m m e n d e d that, if practicable, exposure tests be conducted under environmental conditions of anticipated service applications. Otherwise, consider a severe seacoast atmosphere, one of the cyclic salt spray tests described in ASTM G 85, or one of the immersion type tests. [10] Colvin, E. L. and Lifka, B. W., "Accelerated and Atmospheric Exfoliation Corrosion Performance of A1-Li Alloys," Advances in Localized Corrosion: Proceedings of the Second International Conference on Localized Corrosion, NACE-IO, H. S. Isaacs, U. Bertocci, J. Kruger, and S. Smialowska, Eds., National Association of Corrosion Engineers, Houston, TX, 1989, pp. 215-220. [11] Colvin, E. L. and Murtha, S. J., "Exfoliation Corrosion Testing of A1-Li Alloys 2090 and 2091," Proceedings of the Fifth International Aluminum-Lithium Conference, T. H. Sanders Jr. and E. A. Starke Jr., Eds., Materials and Component Engineering Publications Ltd., Birmingham, U.K., 1989, pp. 1251-1260. [12] Braun, R., "Exfoliation Corrosion Testing of Aluminium Alloys," British Corrosion Journal, Vol. 30, No. 3, 1995, pp. 203-208. [13] Romans, H. B., "An Accelerated Laboratory Test to Determine the Exfoliation Corrosion Resistance of Aluminum Alloys," Materials Research Standards, Vol. 9, No. 11, 1969, pp. 31-34. [14] Ketcham, S. J. and Jeffrey, P. W., "Exfoliation Corrosion Testing of 7178 and 7075 Aluminum Alloys," Localized Corrosion-Cause of Metal Failure, ASTM STP 516, ASTM International, West Conshohocken, PA, 1972, pp. 273-302. [15] Thompson, J. J., "Exfoliation Corrosion Testing of AluminumLithium Alloys," New Methods for Corrosion Testing of Aluminum Alloys, ASTM STP 1134, V. S. Agarwala and G. M. Ugiansky, Eds., ASTM International, West Conshohocken, PA, 1992, pp. 70-81. [16] Tankins, E., Kozol, J., and Lee, E. W., "The Shipboard Exposure Testing of Aircraft Materials," Journal of Metals, Vol. 47, No. 9, 1995, pp. 40-44. [17] "Technical Report: Exfoliation Corrosion Testimony of Aluminum Alloys 5086 and 5456," The Aluminum Association. [18] Summerson, T. J., "Interim Report, Aluminum Association Task Group on Exfoliation and Stress-Corrosion Cracking of Aluminum Alloys for Boat Stock," Proceedings of the TriService Corrosion Military Equipment Conference, Technical Report AFML-TR-75-42, Vol. H, Air Force Materials Laboratory, 1975, pp. 193-221. [19] Sprowls, D. O., Summerson, T. J., and Loftin, F. E., "Exfoliation Corrosion Testing of 7075 and 7178 Aluminum AlloysInterim Report on Atmospheric Exposure Tests," Corrosion in Natural Environments, ASTM STP 558, ASTM International, West Conshohocken, PA, 1974, pp. 99-113. [20] Lifka, B. W. and Lee, S., "Exfoliation Test Results on 2519T87 Plate: Disparity of Results in EXCO Versus Other Environments," Presentation of ASTM Subcommittee GOl.05 Workshop on Exfoliation Corrosion, 1988. [21] Lee, S. and Lifka, B. W., "Modification of the EXCO Test Method for Exfoliation Corrosion Susceptibility in 7XXX, 2XXX and Aluminum-Lithium Alloys," New Methods for Corrosion Testing of Aluminum Alloys, ASTM STP 1134, V. S. Agarwala and G. M. Ugiansky, Eds., ASTM International, West Conshohocken, PA, 1992, pp. 1-19. [22] Formin, G. S., "Corrosion and Corrosion Protection," Encyclopedia of International Standards, Moscow Standards Publishing House, 1994, pp. 193-194. [23] Budd, M. K. and Booth, F. F., "An Accelerated Test For Indicating Susceptibility Of Aluminum Alloys To Layer Corrosion," Corrosion, Vol. 18, 1962, pp. 197t-203t. [24] Li~a, B. W., "Corrosion Resistance of Aluminum Alloy Plate in Rural, Industrial, and Seacoast Atmospheres--Paper #420," Corrosion~87, National Association of Corrosion Engineers, Houston, TX, 1987.

Test Controls
It is always advisable to include control specimens from known materials representing both high and low resistance to exfollation. This is r e c o m m e n d e d for both accelerated and outdoor tests. Such controls verify the validity of a particular test environment and permit the investigator to make some assessm e n t of the normalcy of a particular test run. For example, one cannot conclude that a n e w material is resistant to exfoliation if the susceptible control specimen did not exfoliate to the usual degree. In outdoor tests, the condition of the susceptible control serves as an indicator of w h e n a meaningful length of exposure has been reached. Control specimens are especially advisable in outdoor environments that encounter variable conditions of temperature, precipitation, airborne pollutants, and the like.

REFERENCES
[1] Sprowls, D. O., Walsh, J. D., and Shumaker, M. B., "Simplified Exfoliation Testing of Aluminum Alloys," Localized Corrosion-Cause of Metal Failure, ASTM STP 516, ASTM International, West Conshohocken, PA, 1972, pp. 38-65. [2] Ketcham, S. J. and Jankowsky, E. J., "Developing an Accelerated Test: Problems and Pitfalls," Laborato~ Corrosion Tests and Standards, ASTM STP 866, G. S. Haynes and R. Baboian, Eds., ASTM International, West Conshohocken, PA, 1985, pp. 14-23. [3] Summerson, T. J. and Sprowls, D. O., "Corrosion Behavior of Aluminum Alloys," Conference Proceedings Volume III, Aluminum Alloys: Their Physical and Mechanical Properties, E. A. Starke, Jr. and T. H. Sanders, Jr., Eds., Engineering Materials Advisory Services Ltd., West Midlands, U.K., 1986, pp. 1576-1662. [4] Sinyavski, V. S., Kalinin, V. D., and Dorokhina, V. E., "Study of Correlations Between Structural, Electrochemical and Physical Characteristics and Resistance to Exfoliation Corrosion of Aluminum Alloys," Proceedings of the Second International Conference on Aluminum Alloys-Their Physical and Mechanical Properties, International Academic Publishers, A PergamonCNPIEC Joint Venture, 1990, pp. 692-697. [5] Aylor, D. M., "Corrosion of Metal Matrix Composites," Metals Handbook, 9th ed., Vol. 13 Corrosion, ASM International, Metals Park, OH, 1987, pp. 859-863. [6] Butler, G. and Ison, H. C. K., "Corrosion and Its Prevention in Waters," Reinhold Publishing Corp., New York, NY, 1966, p. 48. [7] Evans, U. R., The Corrosion and Oxidation of Metals, Edward Arnold Ltd., London, U.K., 1961. [8] Loose, W. S., "Magnesium and Magnesium Alloys," The Corrosion Handbook, 1st ed., John Wiley and Sons, Ltd., New York, NY, 1976, pp. 218-252. [9] Lifka, B. W. and Sprowls, D. O., "Relationship of Accelerated Test Methods for Exfoliation Resistance in 7XXX Series Aluminum Alloys with Exposure to a Seacoast Atmosphere," Corrosion in Natural Environments, ASTM STP 558, ASTM International, West Conshohocken, PA, 1974, pp. 306-333.