ASTM-B-571-yr-97-R-13.pdf

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Designation: B571 − 97 (Reapproved 2013)

Standard Practice for

Qualitative Adhesion Testing of Metallic Coatings 1 This standard is issued under the fixed designation B571; the number immediately following the designation indicates the year of  original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense.

of either. Such adhesion is usually obtained if good electroplating practices are followed.

1. Sco Scope pe 1.1 This practice covers covers simple, qualitative qualitative tests for evaluating the adhesion of metallic coatings on various substances.

2.5 For many purposes, purposes, the adhesion test has the objecti objective ve of detecting any adhesion less than “perfect.” For such a test, one uses any means available available to attempt to separate the coating from the substrate. This may be prying, hammering, bending, beating, heating, sawing, grinding, pulling, scribing, chiseling, or a com combin binatio ation n of suc such h tre treatme atments nts.. If the coa coatin ting g pee peels, ls, flakes, flak es, or lift liftss fro from m the substrat substrate, e, the adhesion adhesion is less than perfect.

1.2 Th 1.2 Thee va valu lues es sta stated ted in SI un units its are to be re rega gard rded ed as standard. No other units of measurement are included in this standard. standard d doe doess not purport purport to add addre ress ss all of the 1.3   This standar safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciate ted d wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use.

2.6 If evaluation evaluation of adhesion is required, required, it may be desirable to use one or more of the following tests. These tests have varying degrees of severity; and one might serve to distinguish between satisfactory and unsatisfactory adhesion in a specific application. The choice for each situation must be determined.

2. Sign Significan ificance ce and Use 2.1 The These se tes tests ts are useful useful for product production ion control control and for acceptance testing of products.

2.7 When this guideline guideline is used for acceptance acceptance inspection, inspection, the method or methods to be used must be specified. Because the results of tests in cases of marginal adhesion are subject to interpretation, agreement shall be reached on what is acceptable.

2.2 Inter Interpretin preting g the results of qualitative qualitative methods for determining the adhesion of metallic coatings is often a controversial subject. If more than one test is used, failure to pass any one test is considered unsatisfactory. In many instances, the end use of the coated article or its method of fabrication will suggest the technique that best represents functional requirements. men ts. Fo Forr ex exam ampl ple, e, an ar artic ticle le th that at is to be su subs bseq eque uent ntly ly formed would suggest a draw or a bend test; an article that is to be soldered or otherwise exposed to heat would suggest a heat-quench test. If a part requires baking or heat treating after plating, adhesion tests should be carried out after such posttreatment as well.

2.8 If the size and shape of the item to be test tested ed preclude precludess use of th use thee de desi sign gnate ated d tes test, t, eq equi uiva valen lentt te test st pa pane nels ls may be approp app ropria riate. te. If per permitt mitted, ed, test pan panels els shall be of the same material and have the same surface finish as the item to be tested test ed and shall be pro proces cessed sed thr throug ough h the   same   preplating, electroplating, and postplating cycle with the parts they represent.

2.3 2. 3 Se Seve vera rall of th thee te tests sts ar aree li limit mited ed to sp speci ecific fic ty type pess of  coatings, thickness ranges, ductilities, or compositions of the substr sub strate ate.. The These se limi limitati tations ons are not noted ed gen genera erally lly in the test descriptions and are summarized in Table in  Table 1 for 1  for certain metallic coatings.

3. Bend Tests Tests 3.1 3. 1 Ben Bend d th thee pa part rt wi with th th thee co coate ated d su surf rface ace aw away ay ov over er a mandrel until its two legs are parallel. The mandrel diameter should be four times the thickness of the sample. Examine the deformed area visually under low magnification, for example, 4×, for peeling or flaking of the coating from the substrate, which is evidence of poor adhesion. If the coating fractures or blisters, a sharp blade may be used to attempt to lift off the coating. With hard or brittle coatings, cracking usually occurs in the bend area. Such cracks may or may not propagate into the substrate. In either case, cracks are not indicative of poor adhesion unless the coating can be peeled back with a sharp instrument.

2.4 “Pe “Perfe rfect” ct” adh adhesi esion on exi exists sts if the bon bondin ding g bet betwee ween n the coating and the substrate is greater than the cohesive strength

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This practice is under the jurisdiction of ASTM Committee B08 Committee  B08  on Metallic and Inorganic Coatings and is the direct responsibility of Subcommittee B08.10 Subcommittee B08.10 on  on Test Methods. Current edition approved Dec. 1, 2013. Published December 2013. Originally approved in 1979. Last previous edition approved in 2008 as B571 – 97 (2008) 1. DOI: 10.1520/B0571-97R13. ε

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B571 − 97 (2013) TABLE 1 Adhesion Tests Appropriate for Various Coatings Coating MaterialA Adhesion Test

Cadm Ca dmiu ium m

Chro Ch romi mium um

Copp Co pper er

Lead and Lead/Tin Alloy

Nickel

+ − + − − +

− + + − + +

+ + + + + −

+ − + − + −

+ + + + + +

+ + − + + +

− + − − −

+ − + − −

+ + + − +

+ − − − −

+ + + + +

+ + − + −

B e nd Burnish Chisel/knife Draw File Grind and saw Heat/quench Im p a c t P e el Pus h Scribe A

Rhod Rh odiu ium m

Silv Si lver er

Tin and Tin/Lead Alloy

Zinc

Gold

+ − + − − +

+ − − − + −

+ + + − + −

+ − + − + +

+ + − + − +

+ − + − + −

− − − − −

− − − − −

+ − + − −

+ − + − −

− + − + −

+ − + − −

Nickel and Pall Pa llad adiu ium m Chromium

+ Appropriate; Appropriate; − not appropriate. appropriate.

TABLE 2 Temperature Test Guide Coating Material Substrate

Chromium, Nickel,, Nickel + Nickel Chromium, Copper, Temperature, °C

Tin, Temperature, °C

Lead, Tin/Lead, Temperature, °C

Zinc, Temperature, °C

Gold and Silver, Temperature, °C

Palladium, Temperature, °C

Rhodium, Temperature, °C

250 15 0 2 50

1 50 150 15 0

15 0 150 15 0

15 0 1 50 15 0

25 0 1 50 250

3 50 1 50 3 50

18 5 1 50 18 5

2 20

15 0

15 0

15 0

220

2 20

18 5

S te e l Zinc alloys Copper and copper alloys Aluminum and aluminum alloys

ordinary punc ordinary punch h press.2 Pe Pene netr trati ation on of th thee ma male le di diee ma may y be continued until the cap fractures. The adhesion of the coating may be observed directly or evaluated further by techniques described in Section 5   for detachment from the substrate. If  ther th eree is pe peel elin ing g or fla flaki king ng of th thee co coat atin ing g or if it ca can n be detached, the adhesion is not satisfactory.

3.2 Ben Bend d the part rep repeate eatedly dly,, bac back k and forth, forth, thr throug ough h an angle of 180° until failure of the basis metal occurs. Examine the region at low magnification, for example, 10×, for separation or peeling of the coating. Prying with a sharp blade will indicate unsatisfactory adhesion by lift off of the coating. 4. Burnishing Test Test

6.2 Resul Results ts fro from m thi thiss tec techn hniqu iquee must must be int interp erpret reted ed cautio cau tiousl usly y, bec becaus ausee the duc ductili tilities ties of bot both h the coa coatin ting g and substrate subst rate are involv involved. ed.

4.1 Rub a coa coated ted area of about 5 cm with a smo smooth oth-en -ended ded tool for approximately 15 s. A suitable tool is a steel rod 6 mm in dia diamete meterr with a smo smooth oth hem hemisp ispher herical ical end end.. The pre pressu ssure re shall be sufficient to burnish the coating at each stroke but not so great as to dig into it. Blisters, lifting, or peeling should not develop. Generally, thick deposits cannot be evaluated satisfactorily.

7. File Test Test 7.1 Saw off off a piece of the coated specimen specimen and inspect it for detachment at the deposit/substrate interface. Apply coarse mill filee acr fil acros osss th thee saw sawed ed ed edge ge fr from om th thee su subs bstr trate ate to towa ward rd th thee coating so as to raise it, using an approach angle of approximately 45° to the coating surface. Lifting or peeling is evidence of unsatisfactory adhesion.

5. Chisel-Knife Test Test 5.1 Use a sha sharp rp cold chisel chisel to pen penetr etrate ate the coating coating on the article being evaluated. Alternativel Alternatively y the chisel may be placed in back of an overhang area of the coating or at a coatingsubstrate interface exposed by sectioning the article with a saw. A kn knif ifee ma may y be su subs bstit titut uted ed fo forr th thee ch chis isel el wi with th or wi with thou outt hammer ham mering ing or ligh lightt tap tappin ping. g. If it is pos possib sible le to rem remove ove the deposit, the adhesion is not satisfactory. Soft or thin coatings cannot be evaluated for adhesion by this method.

7.2 This technique technique is not suitab suitable le for thin or soft coatings. coatings. 8. Grind-Saw Test Test 8.1 Hold the coated article article against a rough emery wheel wheel so that the wheel cuts from substrate toward toward the depos deposit it in a jerky or bu bump mpy y fa fash shio ion. n. A ha hack ck saw may be su subs bstit titut uted ed fo forr th thee wheel wh eel,, ma maki king ng su sure re to saw in th thee di dire recti ction on th that at ten tends ds to

6. Draw Test Test 6.1 Form a suitable suitable sample about 60 mm in diameter into into a flanged cap approximately 38 mm in diameter, to a depth up to 18 mm, th thro roug ugh h th thee us usee of a se sett of adjusta adjustabl blee di dies es in an

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Romanoff, F. P.,   Transactions, Ele Electr ctroch ochem. em. Soc., Vol Vol 65, 1934, p. 385 385;; Proceedings, Amer. Electroplate Review w, Electroplaters rs Soc. Vol Vol 22, 1934, p. 155;   Monthly Revie Amer. Electroplaters Soc., Vol 22, April 1935, p. 8.

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B571 − 97 (2013) separate the coating from the substrate. Lifting or peeling is evidence of unsatisfactory adhesion.

11. 1.2 2 The te tens nsile ile an and d sh shea earr st stre reng ngth thss of ad adhe hesiv sives es an and d sold so lder erss lim limit it th thee ra rang ngee of ad adhe hesio sion n str stren engt gths hs th that at ca can n be evaluated. A quantitative analysis of the factors involved has been published.3

8.2 This technique technique is especia especially lly effective effective on hard or brittle coatings but is not suitable for thin or soft coatings.

12. Push Test Test

9. Heat-Quenc Heat-Quench h Test Test

12.1 12 .1 Dril Drilll a bl blin ind d ho hole le 0. 0.75 75 cm in di diam amet eter er fr from om th thee underside until the point of the drill tip comes within approximatel ma tely y 1. 1.5 5 mm of th thee de depo posi sit/s t/sub ubstr strate ate in inter terfa face ce on th thee opposite side. Supporting the material on a ring about 2.5 cm in diameter, apply steady pressure over the blind hole using a hardened steel punch 0.6 cm in diameter until a button sample is pus pushed hed out out..3 Exf Exfolia oliatio tion n or pee peelin ling g of the coating coating in the button or crater areas is evidence of inadequate adhesion.

9.1 Hea Heatt the coated coated arti article cle in an oven for a suf suffficie icient nt time for it to reach the temperature shown in  Table 2. 2.  Maintain the temperature of the oven within 10°C of the nominal. Coatings and substrates that are sensitive to oxidation should be heated in an inert or reducing atmosphere or a suitable liquid. Then quen qu ench ch th thee pa part rt in wa wate terr or ot othe herr su suita itabl blee liq liqui uid d at ro room om temperature.

12.2 Soft, very ductile, ductile, and thin deposits deposits are gener generally ally not suited for this technique.

9.2 Flakin Flaking g or peeling of the depos deposit it is eviden evidence ce of unsatisfacto isfa ctory ry adh adhesio esion. n. Blis Blisters ters may eru erupt pt dur during ing the hea heatt and quench que nch tes testt whe when n plat plating ing sol solutio ution n is ent entrap rapped ped in sub substra strate te surface pits or pores which are bridged by the deposit. If the deposited coating cannot be peeled or lifted from the substrate in an area adjacent to the blister(s), the appearance of blisters should not be interpreted as evidence of inferior adhesion.

13. Scribe-Gri Scribe-Grid d Test Test 13.1 Scrib Scribee three or more parallel lines or a rectangular rectangular grid pattern on the article using a hardened steel tool ground to a sharp (30°) point with a distance between the scribed lines of  approximately ten times the nominal coating thickness, with a mini mi nimu mum m di dist stan ance ce of 0. 0.4 4 mm mm.. In sc scri ribi bing ng th thee lin lines, es, us usee sufficient pressure to cut through the coating to the substrate in a single stroke. If any portion of coating between the lines breaks away from the substrate, the adhesion is inadequate.

9.3 Dif Diffus fusion ion and sub subseq sequen uentt allo alloyin ying g of met metals als may improve the bond strength of electrodeposits. In some cases, a brittle layer may be created by the materials involved causing peeling as a result of fracture rather than poor adhesion. This woul wo uld d no nott gi give ve a co corr rrec ectt in indi dica catio tion n of th thee as as-p -plat lated ed bo bond nd strength.

13.2 Whe 13.2 When n app appare arentl ntly y sat satisf isfacto actory ry adh adhesio esion n is ind indicat icated, ed, apply app ly a pre pressu ssurere-sen sensiti sitive ve tap tape, e, hav having ing an adh adhesio esion n bon bond d strength of at least 45 g/mm, using firm finger pressure onto a clean grid area. Make sure that any loose coating particles from scribing do not remain. Shortly thereafter, remove the tape by seizing a free end and pulling it off rapidly (not jerked) back  upon up on its itsel elff as clo close se to an an angl glee of 18 180° 0° as po poss ssib ible le.. Th Thee adhesion is not adequate if the tape has deposit adhering to it that comes from the area between the scribed lines. Deposit continuous to the scribed lines is not considered. 13.2.1 13.2. 1 The tape supplier supplier4 shall specify that their tape has a suffficie suf icient nt adh adhesi esion on bon bond d str streng ength. th. The tap tapee sha shall ll be wid widee enough to cover three or more parallel lines of the scribed area.

9.4 Thi Thiss tes testt is non nondes destru tructiv ctivee if the procedure procedure does not create unwanted effects on parts. 10. Impac Impactt Test Test 10.1 Use a hammer or impact device coupled coupled with a suitable backing block to support the article to be tested to deform the sample. Reproducible results are more easily obtained by the use of a sui suitab tably ly mod modifie ified d imp impact act tester where where the force force is reproducible and the impact head contour is in the form of a 5-mm 5mm di diam amete eterr ba ball, ll, sh shoc ock k lo load aded ed by a fa falli lling ng we weig ight ht or swinging pendulum weight. The severity of the test may be altered by changing the load and diameter of the ball. Exfoliation or blis blister terss in and around around ind indent entatio ations ns are evi eviden dence ce of  inadequate adhesion. `  `    ,   ,   ,   ,   , `  `  `    ,   , `    ,   ,   , `  `    ,   ,   , `    , `  `    , `  `  `    , `  `    ,   , `    ,   , `    , `    ,   , `  -

13.3 Generally, thick deposits are not not suitable for evaluation unless a chisel or other sharp instrument is used to pry the exposed coating/substrate interface, in which case this technique becomes a variant of Section 5.

10.2 This test is sometimes difficult difficult to interp interpret. ret. Soft and ductile coatings are generally not suited for evaluation.

14. Test-Coating Systems 14.1 Recomm Recommended ended adhesion adhesion tests for a variety of coatin coating g systems are given in Table in  Table 1. 1.

11. Peel Test Test 11.1 Bon Bond d a str strip ip of stee steell or brass brass abo about ut 1.5 mm thic thick k and 20 mm wide by solder or suitable adhesive to a properly flat area of the coated surface of the article. Adhesive-backed tape may be considered as a possible alternative. Heat curing of the adhesive may be used, keeping in mind considerations noted in 9.3..   The 9.3 The an angl glee of pu pull ll sh shal alll be 90 90°° to th thee su surf rfac ace. e. Fo Forr reproducible results, the rate of pull, the thickness and width of  the strip, and deposit thickness must be standardized. Failure in the coatin coating/sub g/substrate strate interface is eviden evidence ce of inadequate adhesion. Provided by IHS under license with ASTM

15. Pre Precisi cision on and Bias 15.1 No statement statement is made about the precision and bias of  these tests because of their qualitative nature.

3

Saubestre, E. B., Durney, L. J., Hajdu, J., and Bastenbeck, E.,  Plating, Vol 52, October 1965, pp. 982–1000. 4 Permacel 99, a product of and manufactured by Permacel, New Brunswick, NJ 08903, is reported to be a suitable product for this purpose.

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B571 − 97 (2013) 16. Keyw Keywords ords 16.1 adhesi adhesion; on; metallic coatings ASTM International International takes no positi position on respecting the validi validity ty of any patent rights assert asserted ed in connec connection tion with any item mentio mentioned  ned  in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk  of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and  if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards  and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the  responsible respon sible technical technical committee, which you may attend. If you feel that your comments have not receiv received ed a fair hearing you should  make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above  address addr ess or at 610610-832832-9585 9585 (pho (phone), ne), 610610-832832-9555 9555 (fax (fax), ), or serv service@ ice@astm astm.org .org (e-m (e-mail) ail);; or thro through ugh the ASTM webs website  ite  (www.astm. (www .astm.org). org). Permission Permission rights to photocopy the standa standard rd may also be secure secured d from the ASTM website (www.astm.or (www.astm.org/  g/  COPYRIGHT/).

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