1、Designation: B 877 96 (Reapproved 2003)Standard Test Method forGross Defects and Mechanical Damage in Metallic Coatingsby the Phosphomolybdic Acid (PMA) Method1This standard is issued under the fixed designation B 877; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test standard covers equipment and methods forusing phosphomolyb
3、dic acid (PMA) to detect gross defects andmechanical damage including wear through in metallic coat-ings of gold, silver, or palladium. These metals comprise thetopmost metallic layers over substrates of nickel, copper, orcopper alloys.1.2 Recent reviews of porosity testing, which include thosefor g
4、ross defects, and testing methods can be found in theliterature.2,3An ASTM guide to the selection of porosity andgross defect tests for electrodeposits and related metalliccoatings is available as Guide B 765. Other related porosityand gross defects test standards are Test Methods B 735,B 741, B 798
5、, B 799, B 809, and B 866.1.3 The values stated in SI units are the preferred units.Those in parentheses are for information only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establis
6、h appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:B 374 Terminology Relating to Electroplating4B 488 Specification for Electrodeposited Coatings of Goldfor Engineering Uses4B 542 Terminology Re
7、lating to Electrical Contacts andTheir Use5B 679 Specification for Electrodeposited Coatings of Palla-dium for Engineering Use4B 689 Specification for Electroplated Engineering NickelCoatings4B 735 Test Method for Porosity in Gold Coatings on MetalSubstrates by Nitric Acid Vapor5B 741 Test Method fo
8、r Porosity in Gold Coatings on MetalSubstrates by Paper Electrography5B 765 Guide for Selection of Porosity Tests for Electrode-posits and Related Metallic Coatings4B 798 Test Method for Porosity in Gold or PalladiumCoatings on Metal Substrates by Gel-Bulk Electrography5B 799 Test Method for Porosit
9、y in Gold and PalladiumCoatings by Sulfurous Acid/Sulfur-Dioxide Vapor5B 809 Test Method for Porosity in Metallic Coatings byHumid Sulfur Vapor (“Flowers-of-Sulfur”)4B 866 Test Method for Gross Defects and MechanicalDamage in Metallic Coatings by Polysulfide Immersion43. Terminology3.1 DefinitionsMa
10、ny terms in this test method are definedin Terminology B 374 or B 542.3.2 Definitions of Terms Specific to This Standard:3.2.1 base metal, nany metal other than gold, silver,platinum, palladium, iridium, or rhodium. Typical base metalsused as underplates or substrates are copper, nickel, tin, lead,a
11、nd their alloys.3.2.2 defect indications, ncolored droplets resulting fromthe reaction between the PMA reagent and the underlyingmetal.3.2.3 gross defects, nthose breaks in the coating thatexpose relatively large areas of underlying metal to theenvironment. Gross defects include those produced by me
12、-chanical damage and wear, as well as as-plated large pores withdiameters an order of magnitude greater than intrinsic porosityand networks of microcracks.NOTE 1Large pores and microcrack networks indicate serious devia-tions from acceptable coating practice (dirty substrates and contaminatedor out-
13、of-balance plating baths).3.2.4 intrinsic porosity, nthe normal porosity that ispresent, to some degree, in all commercial thin electrodeposits(precious metal coatings for engineering purposes) that willgenerally follow an inverse relationship with thickness.1This test method is under the jurisdicti
14、on of ASTM Committee B08 on Metallicand Inorganic Coatings and is the direct responsibility of Subcommittee B08.10 onTest Methods.Current edition approved Feb. 10, 2003. Published May 2003. Originallyapproved in 1996. Last previous edition approved in 1996 as B 877 96.2Clarke, M., “Porosity and Poro
15、sity Tests,” Properties of Electrodeposits, ed. bySand, Leidheiser, and Ogburn, The Electrochemical Society, 1975, p. 122.3Krumbein, S. J., “Porosity Testing of Contact Platings,” Trans. Connectors andInterconnection Technology Symposium, Philadelphia, PA, October 1987, p. 47.4Annual Book of ASTM St
16、andards, Vol 02.05.5Annual Book of ASTM Standards, Vol 02.04.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 2Intrinsic porosity is due to small deviations from ideal platingand surface preparation conditions. Scanning electron
17、microscope (SEM)studies have shown the diameter of such pores at the plating surface is 1to 2 m so only small areas of underlying metal are exposed to theenvironment.3.2.5 measurement area, nthat portion or portions of thesurface that is examined for the presence of gross defects ormechanical damage
18、 and wear through. The measurement areashall be indicated on the drawings of the parts or by theprovision of suitably marked samples.3.2.6 metallic coatings, ninclude electrodeposits, clad-dings, or other metallic layers applied to the substrate. Thecoating can comprise a single metallic layer or a
19、combinationof metallic layers (gold over palladium).3.2.7 porosity (general), nthe presence of any hole, crack,or other defect that exposes the underlying metal to theenvironment.3.2.8 underplate, na metallic coating layer between thesubstrate and the topmost metallic coating. The thickness of anund
20、erplate is usually greater than 1 m, in contrast to a strikeor flash, which is usually thinner.3.2.9 wear through, nthe exposure of underplate or sub-strate as a direct result of wear. Wear through is an observablephenomenon.3.2.10 wear track, na mark that indicates the path alongwhich physical cont
21、act has been made during a sliding process(the mating and unmating of an electrical contact).4. Summary of Test Method4.1 This test method involves the use of a solution ofphosphomolybdic acid (PMA), which is a solid complex ofmolybdenum trioxide, Mo2O3, and phosphoric acid, H3PO4.Inthis state, moly
22、bdenum is very reactive with many free metalsand may be used to detect exposed underplates and substratemetals. The part is exposed briefly to fumes of hydrochloricacid to remove oxides in the defect region. A small drop of theaqueous PMA solution is applied to the spot in question usingan applicato
23、r. If it contacts base metals from exposed under-plate or substrate, the Mo2O3will immediately be reduced tolower oxides, forming the intensely colored, molybdenum bluecomplex (heteropoly blue).64.2 This test may not be suitable for some precious metalalloy coatings that contain significant concentr
24、ations of non-precious metals (base metals) like nickel or copper. (See .)4.3 The reagents in this test also react with tin, lead, andtin-lead solder.5. Significance and Use5.1 The primary purpose of the PMA test is to determine thepresence of mechanical damage, wear through, and other grossdefects
25、in the coating. Most metallic coatings are intended tobe protective, and the presence of gross defects indicates aserious reduction of such protection.5.2 The protection afforded by well applied coatings may bediminished by improper handling following plating or as aresult of wear or mechanical dama
26、ge during testing or while inservice. The PMA test can serve to indicate the existence ofsuch damage.5.3 This test is used to detect underplate and substrate metalexposed through normal wear during relative motions (matingof electrical contacts) or through mechanical damage. As such,it is a sensitiv
27、e pass/fail test and, if properly performed, willrapidly detect wear through to base metals or scratches thatenter the base metal layers.5.4 This test is relatively insensitive to small pores. It is notdesigned to be a general porosity test and shall not be used assuch. The detection of pores will d
28、epend upon their sizes andthe length of time that the reagent remains a liquid.5.5 This test cannot distinguish degrees of wear through orwhether the wear through is to nickel or copper. Once basemetal is exposed, the colored molybdenum complex is formed.While relatively small area defects (compared
29、 to the area of thedroplet) may be seen at the bottom of the drop as tiny coloredregions immediately after applying the PMA, any larger areasof exposed base metal will cause the entire droplet to turn darkinstantly.5.6 The PMA test also detects mechanical damage thatexposes underplate and substrate
30、metal. Such damage mayoccur in any postplating operation or even at the end of theplating operation. It can often occur in assembly operationswhere plated parts are assembled into larger units by mechani-cal equipment.5.7 The PMA test identifies the locations of exposed basemetal. The extent and loc
31、ation of these exposed areas may ormay not be detrimental to performance. The PMA test is notrecommended for predictions of product performance, nor is itintended to simulate field failure mechanisms. For such contactperformance evaluations, an environmental test known tosimulate actual failure mech
32、anisms should be used.5.8 The PMA test is primarily intended for the evaluation ofindividual samples rather than large sample lots, since evalu-ations are normally carried out one at a time under themicroscope (see Section 10).5.9 This test is destructive. Any parts exposed to the PMAtest shall not
33、be placed in service.6. Apparatus6.1 In addition to the normal equipment (beakers, weighingbalances, funnels, etc.) that are a part of every chemicallaboratory.6.2 Microscope, Optical, Stereo, 10 to 303It is preferredthat one eyepiece contain a graduated reticle for measuring thedefect location. The
34、 reticle shall be calibrated for the magni-fication at which the microscope is to be used, preferably103.76.3 Light source (illuminator) for microscope, incandescent.6.4 Glass volumetric flask, 10 mL.6Van Wazer, J. P., Phosphorous and Its Compounds, Interscience Publishers,New York, 1961.7Magnificat
35、ion standards suitable for calibrating optical microscopes may bepurchased from U.S. National Institute of Standards and Technology, Office ofStandard Reference Materials.B 877 96 (2003)26.5 Glass bottle of a stable shape and with glass stopper. Thebottle opening shall be 2.5 cm (1 in) minimum. An e
36、xample isa 50-mL low-form weighing bottle or a flask-shaped weighingbottle.6.6 Applicators (see 9.2)Platinum wire, 32 AWG, ordisposable glass micropipets, 1 or 0.5 L size.7. Reagents and Materials7.1 Phosphomolybdic Acid (PMA)Crystalline, ACS certi-fied grade.7.2 Concentrated Hydrochloric Acid ACS a
37、nalytical re-agent (AR) grade or better.8. Specific Safety and Health Precautions8.1 All the normal precautions shall be observed in handlingthe materials required for this test. This shall include, but is notlimited to, procuring and reviewing Material Safety DataSheets that meet the minimum requir
38、ements of the OSHAHazard Communication Standard for all chemicals used incleaning and testing and observing the recommendationsgiven.9. Preparations9.1 Preparation of solutions:9.1.1 Two types of PMA solutions can be used with thismethod.9.1.1.1 Method A, the preferred method, uses a dilute 8 %solut
39、ion of PMA in water.9.1.1.2 Method B, uses a saturated solution of PMA inwater.NOTE 3The dilute solution is preferred because it works well withsilver, gold, and palladium coatings, while the saturated solution reactswith silver to give false indications. In addition, the saturated solution hasa ten
40、dency to dry up quickly on the test surface before proper evaluationscan be made.9.1.2 Dilute (8 %) PMA solution (for Method A):9.1.2.1 Place a small, clean, and dry glass funnel in the neckof a clean, dry 10 mL volumetric flask.9.1.2.2 Tare out the weight of the funnel and flask on abalance.9.1.2.3
41、 Weigh 0.8 (60.1) g PMA into the flask, using aplastic or glass spatula.9.1.2.4 Rinse the funnel with distilled or deionized water todrain any adhering PMA into the flask.9.1.2.5 Dilute to mark with deionized water.9.1.2.6 Place stopper in flask and mix thoroughly. Cloudysolution will clear after st
42、anding 10 to 15 min.9.1.2.7 Pour clear solution into a clean glass bottle and sealwith glass stopper. Label bottle with PMA concentration anddate of preparation.9.1.2.8 Store bottle in refrigerator. Solution may be used forone week.9.1.3 Saturated PMA solution (for Method B):9.1.3.1 Prepare solution
43、 in accordance with 9.1.2.1-9.1.2.6,except use approximately5gofPMAinstead of 0.8 g. (Filterout sediment, if necessary.)9.1.3.2 Mix thoroughly for at least 10 min.NOTE 4There shall be a small excess of PMA, seen as a sediment inthe bottom of the flask. This indicates saturation.9.1.3.3 Pour into a c
44、lean bottle and label bottle withcontents and preparation date.9.1.3.4 Solution may be used for one week. Store inrefrigerator when not in use.9.1.4 Hydrochloric acid (for both methods):9.1.4.1 Fill the special glass bottle (see 6.4) to approxi-mately halfway from the top.9.1.4.2 Label glass bottle
45、with contents.9.1.4.3 Keep stoppered and under a fume hood when not inuse.9.2 Preparation of applicators:9.2.1 The applicator shall not react with the PMA solution.Examples are as follows:9.2.1.1 PlatinumMake a small loop using a 32 AWGplatinum wire and an appropriate size mandrel (such as aneedle).
46、 Leave a small gap to facilitate release of the PMAdroplet (see Fig. 1). Attach loop to a wooden or plastic handle.9.2.1.2 Platinum inoculating loops with handles may bepurchased. Cut the loop with a knife to create a small gap (Fig.1), which will facilitate the release of the PMA droplet.9.2.1.3 Gl
47、ass capillary micropipets in the 1-L size orsmaller.9.2.2 If a platinum loop is used as the applicator, the loopdiameter shall preferably be 1 mm and shall not exceed 2 mm.The loop diameter is kept small for the following reasons:9.2.2.1 The small dimensions of many examination areas.9.2.2.2 The abi
48、lity of the loop to release a rounded dropletinstead of a thin sheet of solution, which dries too fast.9.2.2.3 Difficulty in controlling flow and observing reac-tions in large drops.9.3 Preparation of test samples:9.3.1 Handle samples as little as possible even prior tocleaning and only with tweezer
49、s, microscope-lens tissue, orclean, soft cotton gloves.9.3.2 Prior to being cleaned, the samples shall be preparedso the measurement area is accessible and can be placed in abasically horizontal plane. This allows for easy viewingthrough the microscope and prevents the PMA solution fromrunning off during application.9.3.3 Masking:9.3.3.1 The PMA solution will react with any exposed basemetal such as nickel, copper, tin, lead, or solder. If theexamination area is within a millimetre of exposed or thinlyplated substrate metal, masking may be necessary.9.3.3.2 If m
